AXIS UltraDLD

AXIS UltraDLD
Operators Manual
39-306
supplied by:
Kratos Analytical
Wharfside, Trafford Wharf Road,
Manchester, M17 1GP, UK

AXIS Ultra DLD Operating Manual
Kratos Analytical Ltd. 2009
Ref: 39-306
Latest Revision: rev. 4
All rights reserved.
No part of this publication may be copied, reproduced, stored in a retrieval system, or transmit-
ted, in any form or by any means, electronic, mechanical, photo-reproduction, recording or oth-
erwise without the prior written permission of Kratos Analytical.
Kratos Analytical assumes no responsibility for the use of equipment other than as described.
Several aspects of the instrument described are subject to patent regulation. No licenses or
other rights are assumed or granted.
Kratos Analytical has a policy of continuous product improvement and therefore reserves the
right to make alterations to specifications without notice. The product delivered may differ from
that described. Information described in this manual is subject to change without notice. While
Kratos Analytical believes that this document is true and accurate, Kratos Analytical cannot be
held responsible for any errors and omissions contained herein.
This manual is written for use with Kratos Vision software version 2.2.7 running on MS Win-
dows XP. A full description of new features and improvements is listed in the Vision 2.2.7
release notes.
KRATOS ANALYTICAL Ltd., Surface Analysis Product Group, Wharfside,
Trafford Wharf Road, MANCHESTER, M17 1GP, England.
Tel. +44 (0)161 888 4400, Fax. +44 (0)161 888 4402
www.kratos.com
Contents
Chapter 1 Safety Warnings .................................................. 9

1.1 European Union Directives Compliance ..... 9
1.1.1 FCC Compliance ................................................ 9
1.1.2 Electrical Supplies ............................................. 10
1.1.3 Maintaining compliance with the electromagnetic compat-
ibility and low voltage directives10
1.1.4 Sample records ................................................. 10
1.1.5 Safety labels...................................................... 11
1.1.6 Warning: Ionising Radiation Generator ............. 13
1.1.7 Laser Light......................................................... 13
1.1.8 Handling Liquid Nitrogen ................................... 14
1.1.9Taking the Vacuum System to Atmospheric Pressure14
1.1.10 Rotary Pump Exhaust...................................... 14
1.1.11 Radiation Hazard ............................................. 14
1.1.12 Thoriated Filaments......................................... 15
1.2 Equipment Return Declaration ................. 15
Chapter 2 AXIS Technology as Applied to the AXIS Ultra DLD 21

2.1 Introduction. ................................................ 21
2.2 X-ray photoelectron spectroscopy .............. 21
2.2.1XPS instrumentation........................................... 22
2.2.1.1The X-ray source ................................................... 23
2.2.1.2Transfer lens ......................................................... 25
2.2.2The AXIS Spectrometer Lens Geometry ............ 26
2.2.2.1The Magnetic lens ................................................. 26
2.2.2.2The Charge Neutraliser ......................................... 27
2.2.2.3Lens Modes and the Solid Angle of Collection ...... 29
2.2.2.4The Scan Deflection Plates ................................... 30
2.2.3Electron Energy Analysers ................................. 32
2.2.3.1XPS imaging. ........................................................ 32
2.2.3.2Parallel XPS imaging. ........................................... 32
2.2.4Applications of small spot and imaging XPS. ..... 34
2.2.5Summary. ........................................................... 36
Chapter 3 Overview of the AXIS Ultra DLD ............................. 37

3.1. The Hardware ............................................. 37
3.1.1Services Required .............................................. 37
3.1.1.1Water ..................................................................... 37
3.1.1.2Electricity ............................................................... 38
3.1.1.3Air Conditioning and Ventilation ............................ 38
3.1.1.4Gas Supplies ......................................................... 38
3.1.1.5Vibration ................................................................ 38
3.1.1.6Magnetic Fields ..................................................... 38
3.1.2Electronic Units................................................... 39
1
3.1.2.1DLD Pre-amplifier ..................................................39
3.1.2.2Analyser Control Unit ............................................39
3.1.2.3Vacuum Control Unit .............................................39
3.1.2.4Stage Control Unit .................................................39
3.1.2.5NICPU Control Unit ...............................................39
3.1.2.6X-ray Source Control Unit .....................................40
3.1.2.7Deflector Control Unit ............................................40
3.1.2.8Magnetic Lens Control Unit ...................................40
3.1.2.9X-ray High Voltage Controller ................................40
3.1.2.10Ion Pump and TSP Controller .............................40
3.1.3Vacuum Chamber............................................... 41
3.1.4The Vacuum System .......................................... 42
3.1.5Pressure Measurement ...................................... 44
3.1.6Automatic Vacuum Sequences in Vision Software44
3.1.6.1Vent STC ...............................................................45
3.1.6.2Pump STC .............................................................45
3.1.6.3Ion Gun Gas On ....................................................46
3.1.6.4Ion Gun Gas Off ....................................................46
3.1.6.5Open STC-SAC Valve ...........................................46
3.1.6.6Close STC-SAC Valve ...........................................46
3.1.6.7Pump SAC ............................................................47
3.2. Vacuum Control Unit ...................................47

3.2.1Understanding the Vacuum Control Unit ............ 48
3.3. Pumping the AXIS Ultra DLD from Atmosphere 49
3.4. Baking the AXIS Ultra DLD .........................49
3.4.1Preparation for Baking the AXIS Ultra DLD........ 50
3.4.2Baking the AXIS Ultra using Vision Software ..... 56
3.4.3Baking the AXIS Ultra DLD using the VCU ........ 57
3.4.4Failure to start baking ......................................... 60
3.4.5Degassing Filaments and Sources After Baking 60
3.5. Venting the AXIS Ultra DLD to Atmosphere 61
Chapter 4 Basic Operation ..................63

4.1. Introduction .................................................63
4.2. The Mouse ..................................................63
4.3. Opening the Manager Software and Vision Zones
64
4.4. The Manual Window ...................................68
4.4.1Entering values in boxes .................................... 70
4.4.2Modes of Operation ............................................ 70
4.4.3Manual Window Selection .................................. 71
4.4.4Optical Images.................................................... 71
4.4.5Analyser Control and Parallel XPS Imaging ....... 74
2
Contents
4.4.5.1Analyser Mode ...................................................... 74

4.4.5.2Lens Mode ............................................................ 75
4.4.5.3Resolution ............................................................. 76
4.4.5.4Area of Analysis .................................................... 76
4.4.5.5Analyser State ....................................................... 78
4.4.5.6XPS Parallel Imaging On and Off .......................... 78
4.4.5.7Integration Mode ................................................... 78
4.4.5.8Energy ................................................................... 79
4.4.5.9Grab Image ........................................................... 79
4.4.6Acquisition Control ............................................. 79
4.4.6.1Spectrum ............................................................... 80
4.4.6.2Map ....................................................................... 82
4.4.6.3Line Scan .............................................................. 82
4.4.6.4Snapshot ............................................................... 82
4.4.7X-ray PSU .......................................................... 83
4.4.7.1Selecting X-ray Source ......................................... 83
4.4.7.2Switching the X-rays to stand-by ........................... 85
4.4.7.3Switching the X-ray Source On ............................. 85
4.4.7.4Switching the X-ray Source Off ............................. 85
4.4.7.5X-ray Parameters .................................................. 85
4.4.7.6Leakage Current ................................................... 86
4.4.8The Charge Neutraliser ...................................... 88
4.5. Sample Mounting Techniques ..................... 89
4.5.1General Requirements ....................................... 89
4.5.2Sample Handling and Storage............................ 89
4.5.3Sample Stubs ..................................................... 90
4.5.4Mounting on Sample Bars .................................. 92
4.6. Sample Insertion ......................................... 93
4.6.1Standard or Long STC........................................ 93
4.6.1.1Loading a Sample Stub ......................................... 94
4.6.1.2Loading a Sample Bar ........................................... 96
4.6.2Loading Samples on to the Sample Magazine WX-48997
4.7. Sample Insertion With Fast Entry Lock WX-523 99
4.7.0.1Loading a sample stub into the fast entry lock ...... 99
4.7.0.2Loading a sample bar into the fast entry lock ....... 103
4.8. Operation of the Autostage ........................ 104

4.8.1Calibrating the Autostage .................................. 105
4.8.2Manual Stage Control ........................................ 106
4.8.3Automatic Stage Control.................................... 108
4.8.3.1Inserting a stage position in the general position table 111
4.8.3.2Driving the Autostage to a Position Defined in the General Posi-
tion Table ................................................................ 112
4.8.3.3Saving and Retrieving a Position Table ................ 112
4.8.4Automatically Finding the Correct Analysis Height113
4.8.5Transferring a Sample Stub to the SAC ............ 117
4.8.6Removing a Sample Stub from the SAC ........... 120
4.8.7Transferring a Sample Bar to the SAC .............. 120
4.8.8Removing a Sample Bar from the SAC............. 122
3
4.9. Aperture and Iris Drives .............................124
Chapter 5 Mini Beam I and III Ion sources .....................127

5.1. The Ionisation Chamber .............................127
5.2. Overview of Mini Beam I (WX-414) ............129
5.2.1Mini Beam I Ion Optics ...................................... 130
5.3. Overview of the Mini Beam III (WX-422) ....131
5.3.1Mini Beam III Ion Optics .................................... 131
5.3.2Ion Beam Stabilisation ....................................... 133
5.4. Depth Profiling ...........................................133
5.5. Manual Software Interface .........................135
5.5.1Ion source Controls ........................................... 135
5.5.1.1Source High Tension (HT) ....................................136
5.5.1.2Extractor / Emission Toggle and Extractor or Emission
Current ...................................................................137
5.5.1.3Float Voltage ........................................................137
5.5.1.4Beam Energy ........................................................137
5.5.1.5Etch Rate ..............................................................137
5.5.1.6Sample Current ....................................................137
5.5.1.7Raster Size ...........................................................137
5.5.2Ion source Table ................................................ 137
5.5.2.1Update Row ..........................................................138
5.5.2.2Restore Row .........................................................138
5.5.2.3Preset Row ...........................................................138
5.5.3Tuning................................................................ 138
5.5.3.1Filament selector ..................................................139
5.5.3.2Filament Current Limit ..........................................139
5.5.3.3Grid Voltage ..........................................................139
5.5.3.4Extractor Voltage ..................................................139
5.5.3.5Condenser ............................................................139
5.5.3.6Focus ....................................................................140
5.5.3.7Align X and Align Y. ..............................................140
5.5.3.8Scale X and Y .......................................................140
5.5.3.9Offset X and Y ......................................................140
5.5.3.10Max FSD ............................................................140
5.5.4Status................................................................. 140
5.5.4.1Source HT ............................................................141
5.5.4.2Filament ................................................................141
5.5.4.4Extractor Current ..................................................141
5.5.4.5Float Voltage ........................................................142
5.5.4.6Grid Voltage ..........................................................142
5.5.4.7Condenser ............................................................142
5.5.4.8Focus ....................................................................142
5.5.4.9Alignment X1 and X2 ............................................142
5.5.4.10Emission Current ................................................142
5.5.5Bias Current....................................................... 142
4
Contents
5.5.6Degas ................................................................ 143

5.6. Standard Manual Operation ....................... 145
5.6.1Starting the flow of Argon .................................. 145
5.6.2Switching the ion source on .............................. 146
5.6.3Switching the ion source off............................... 148
5.7. Ion source Tuning ...................................... 149
5.7.1Imaging the ion spot .......................................... 149
5.7.2Positioning the Ion Spot..................................... 151
5.7.3Fine Adjustment of the Ion Beam Position and Crater Size
153
5.7.4Tuning the beam................................................ 156
5.8. Determining the Etch Rate ......................... 158
Chapter 6 Floating Ion Gun ............................................. 159

6.1. Overview of Floating Ion Gun .................... 160
6.1.1The Ionisation Chamber .................................... 160
6.1.2Ion Beam Stabilisation....................................... 162
6.1.3Ion Optics .......................................................... 163
6.1.4Configuration of the Ion Optics for Different Applications
164
6.1.4.1Rapid Depth Profiling ........................................... 165
6.1.4.2Low Energy Depth Profiling and the floating mode 167
6.2. Manual Software Interface ......................... 168

6.2.1Ion Gun Controls ............................................... 169
6.2.1.1Source High Tension (HT) .................................... 169
6.2.1.2Extractor / Emission Toggle and Extractor or Emission
Current ................................................................... 170
6.2.1.3Float Voltage ........................................................ 170
6.2.1.4Beam Energy ....................................................... 170
6.2.1.5Etch Rate ............................................................. 170
6.2.1.6Sample Current .................................................... 170
6.2.1.7Raster Size ........................................................... 170
6.2.1.8Compucentric Rotation on/off ............................... 170
6.2.2Ion Gun Table .................................................... 171
6.2.2.1Update Row ......................................................... 171
6.2.2.2Restore Row ........................................................ 172
6.2.2.3Preset Row ........................................................... 172
6.2.3Tuning................................................................ 172
6.2.3.1Filament selector .................................................. 172
6.2.3.2Filament Current Limit .......................................... 173
6.2.3.3Grid Voltage .......................................................... 173
6.2.3.4Extractor Voltage .................................................. 173
6.2.3.5Condenser ............................................................ 173
6.2.3.6Focus ................................................................... 173
6.2.3.7Align X. ................................................................. 173
6.2.3.8Scale X and Y ...................................................... 173
5
6.2.3.9Offset X and Y ......................................................174
6.2.3.10Max FSD ............................................................174
6.2.4Status................................................................. 174
6.2.4.1Source HT ............................................................175
6.2.4.2Filament ................................................................175
6.2.4.4Extractor Current ..................................................175
6.2.4.5Float Voltage ........................................................175
6.2.4.6Grid Voltage ..........................................................175
6.2.4.7Condenser ............................................................175
6.2.4.8Focus ....................................................................176
6.2.4.9Alignment X1 and X2 ............................................176
6.2.4.10Emission Current ................................................176
6.2.5Bias Current....................................................... 176
6.2.6Degas ................................................................ 177
6.2.7Pneumatic Sputter Shield (optional) .................. 179
6.3. Standard Manual Operation .......................180
6.3.1Starting the flow of Argon .................................. 180
6.3.2Switching the ion gun on ................................... 181
6.3.3Using Rotation .................................................. 182
6.3.4Switching the ion gun off ................................... 183
6.4. Ion Gun Tuning ..........................................184
6.4.1Imaging the ion spot .......................................... 185
6.4.2Positioning the Ion Spot..................................... 187
6.4.3Fine Adjustment of the Ion Beam Position and Crater Size
189
6.4.4Tuning the beam................................................ 193
6.5. Determining the Etch Rate .........................194
Chapter 7 Data Acquisition using the Instrument Manager 197

7.1 Introduction ................................................197
7.2 The Instrument Manager Window - An Overview
197
7.2.1The Menu Bar.................................................... 198
7.2.1.1File ........................................................................199
7.2.1.2Edit .......................................................................200
7.2.1.3Mode ....................................................................201
7.2.1.4Window .................................................................201
7.3 Defining an Experiment in the Manager Window 205

7.3.1Large Area Survey Spectrum ............................ 205
7.3.2Large Area High Resolution Spectra ................. 209
7.3.2.1Spectra from Insulators ........................................ 211
7.3.3Parallel Imaging - Field of View 2 ...................... 215
7.3.4Parallel Imaging - FOV 1 and FOV 3................. 218
6
Contents
7.3.5Small Spot - Selected Area Spectra .................. 219

7.3.6Automated Spectral Acquisition From Several Samples
224
7.3.6.1Acquiring Spectra From Similar Samples. ............ 224
7.3.6.2Acquiring Spectra from Dissimilar Samples ......... 229
7.3.6.3Adding a Delay to Automated Acquisition ............ 232
7.3.7Automatically Finding the Sample Analysis Height (AutoZ)
233
7.3.8Angle Resolved XPS ......................................... 241
7.3.8.1Defining the Sample Positions for ARXPS in Manual Mode
241
7.3.8.2Using the rotation about a point routine to define the sample
positions ................................................................. 243
7.3.8.3Defining the ARXPS Experiment in Manager ....... 246
7.3.9Automated Depth Profiling ................................ 248
7.4 Acquisition Conditions Reference Sheet ... 254
Chapter 8 Vision Processing Software ............................. 257

8.1 Examples of data processing. .................... 258
8.1.1Quantifying a large area survey spectra............ 258
8.1.2Survey spectra quantification report generation.261
8.1.3Propagation of defined regions to other spectra.262
8.1.4Peak synthesis and curve fitting........................ 263
8.1.5Components quantification report generation.... 269
8.1.6Components and regions quantification report generation.
270
8.2 Reference section. ..................................... 273
8.2.1Vision Processing. ............................................. 273
8.2.1.1File. ...................................................................... 274
8.2.1.2Options. ................................................................ 275
8.2.1.3View. ..................................................................... 275
8.2.1.4Data object view modes. ...................................... 275
8.2.1.5Current Dataset. ................................................... 276
8.2.1.6Dataset comment area. ........................................ 276
8.2.1.7The Scratch section. ........................................... 276
8.2.1.8Data object selection mechanisms. ...................... 277
8.2.1.9Background menu pop-up. ................................... 278
8.2.2Display window.................................................. 279
8.2.2.1Display window selection mechanisms. ............... 279
8.2.2.2Background menu pop-up. ................................... 280
8.2.3Overlaying Objects in the Display Window........ 281
8.2.4Processing......................................................... 283
8.2.4.1Smooth. ................................................................ 285
8.2.4.2Differentiate. ......................................................... 285
8.2.4.3Integrate. .............................................................. 286
8.2.4.4Deconvolute. ........................................................ 286
8.2.4.5Calibrate. .............................................................. 286
7
8.2.4.6Quantify. ...............................................................287
8.2.4.7Annotate. ..............................................................297
8.2.4.8Normalise. ............................................................299
8.2.4.9Data Editing. .........................................................299
8.2.4.10History. ...............................................................300
8.2.4.11Background menu pop-up. .................................301
8.2.5Browser Actions................................................. 302
8.2.5.1Periodic table. .......................................................302
8.2.5.2Calculator. ............................................................303
8.2.5.3Profile spectra. .....................................................305
8.2.5.4Profile images. ......................................................308
8.2.5.5Describe. ..............................................................309
8.2.6Element List....................................................... 310
8.2.7Display Parameters. .......................................... 312
8.2.8Page Display...................................................... 315
8.2.9Browser filter...................................................... 316
8.2.10Colour editors. ................................................. 317
8.2.11Printing............................................................. 318
Appendix ........................................................................................319
9.1. Points of Contact at Kratos ........................319
9.1.1USA, Canada and South America ..................... 319
9.1.2Europe and Far East ......................................... 319
9.1.3Japan................................................................. 320
9.2. Configuration File .......................................320
9.3. Instrument Checks and First Line Maintenance 322
9.3.1Chiller Servicing................................................. 322
9.3.2Instrument Performance Checks ....................... 322
9.3.3Weekly Functional Checks. ............................... 323
8
13 July 2009
Chapter 1
Safety Warnings
Please read this section of the manual carefully as it sets out the safety issues
relating to the operation of the AXIS Ultra DLD. All users must have read this
section and be aware of the safety aspects and safe operating procedures of
the spectrometer.
After acceptance of the instrument it is strongly recommended that the checks

outlined in Instrument Checks and First Line Maintenance are carried out at
the intervals recommended.
1.1 European Union Directives Compliance
The AXIS Ultra DLD is compliant with the electromagnetic compatibility direc-
tive and the low voltage directive. Compliance is signified by labelling the
spectrometer with the CE label.
1.1.1 FCC Compliance
This equipment has been tested and found to comply with the limits for a
Class A digital device, pursuant to part 15 of the FCC rules. These limits are
designed to provide reasonable protection against harmful interference when
the equipment is operated in a commercial environment. This equipment
generates, uses and can radiate radio frequency energy, and if not installed
and used in accordance with the instruction manual, may cause harmful inter-
ference to radio communications. Operation of this equipment in a residential
area is likely to cause harmful interference in which the user will be required
to correct the interference at his own expense.
This instrument complies with Canadian ICES - 003 Class A EMC require-
ments.
9
European Union Directives Compliance
1.1.2 Electrical Supplies
Europe U.S.A and Japan

Live: Brown Live: Black
Neutral: Blue Neutral: White
Earth: Green/yellow Earth: Green
Mains supply voltage warning
Although the instrument has covers fitted to protect against electrical shock it
is strongly recommended that the instrument is switched off and isolated from
the mains supply before removing any of the mains protection covers or
attempting to replace any of the mains fuses.
HIGH VOLTAGE WARNING
High voltages (kV) are present within the circuitry of the instruments and
extreme caution should be taken when making any adjustments within the
instrument.
1.1.3 Maintaining compliance with the electromagnetic compatibility and

low voltage directives
The following is a list of precautions which must be observed to maintain

conformance with the European directives above:
1.Operate the instrument within the limits set out in either the technical
specification or the site conditions sheet.
2.Do not modify the instrument in any way, electrically or mechanically.
3.Ensure that all covers, fan guards, EMC gaskets and screws are fitted.
4.Ensure that all cable screens are connected.
5.Do not change component values.
6.Do not remove any labels.
7.Purchase spare parts from a recommended spare parts list.
8.Always replace parts like for like.
9.Keep a concise record of all the work carried out on the instrument and any
parts changed with serial numbers where appropriate.
Warning
Service work must be carried out by Kratos trained engineers. Kratos

Analytical cannot be held responsible for the action of un-trained, non-Kratos
service engineers who render the instrument non compliant with the above
European directives. The figures below show the safety labels which are
fitted to the instruments and their meanings.
1.1.4 Sample records
A record should be kept of all substances analysed with the instrument and
their concentration level/amounts. This record will be needed by the Kratos
Analytical Service Centre should any part of the instrument need servicing/
10 Chapter 1 Safety Warnings

replacing. Any item returned for repair/replacement must be accompanied by

this sample report and a completed Returned Equipment Declaration (found
at the end of this manual section).
1.1.5 Safety labels
The figures in Section 2.1.5 show the safety labels which are fitted to the
instruments and their meanings:
FIGURE 1.Mains voltage warning labels
FIGURE 2.High Voltage warning labels
Chapter 1 Safety Warnings 11

FIGURE 3.Earthing Labels
FIGURE 4.Mechanical safety warning labels
FIGURE 5.Ionising radiation warning label

KRATOS ANALYTICAL LTD

WHARFSIDE, TRAFFORD WHARF ROAD,
MANCHESTER, U.K., M17 1GP SERIAL No.
PART No. REV DATE
VOLTS Hz FUSE/TYPE
PHASE VA WEIGHT kg
FIGURE 6.Rating plate
These labels are fitted to the AXIS Ultra DLD Photoelectron Spectrometer in a
number of positions. Please observe the warnings given.
1.1.6 Warning: Ionising Radiation Generator

This instrument is covered by Ionising Radiation Regulations 1999 (IRR99).
Any company, institution and individual using the AXIS Nova must comply with
IRR99 and be familiar with its contents. Note that it is the responsibility of the
AXIS Nova users employer to ensure compliance with IRR99 and consult with
a radiation protection advisor. In particular the following regulations defined in
IRR99 might be relevant:
regulation 7 - Prior risk assessment.
regulation 8 -Restriction of exposure.
regulation 10 -Maintenance and examination of engineering controls etc.
regulation 12 - Contingency plans.
regulation 13 - Radiation protection advisor.
regulation 14 - Information, Instruction and training.
regulation 17 - Local rules and radiation protection supervisors.
regulation 31 - Duties of manufacturers etc. of articles for use in work with

ionising radiation.
regulation 33 - Misuse or interference with sources of ionising radiation.
regulation 34 - Duties of employees.
The IRR99 and associated ACoP (L121) are available on-line at

www.hmso.gov.uk.
1.1.7 Laser Light

The AXIS Ultra DLD makes provision for the use of a laser as an alignment
tool. When fitted to the spectrometer, the device operates as a Class I laser. It
must not be operated independently of the spectrometer, and the warnings and
precautions set out in the device manual must be followed. Avoid staring at the
reflected laser light for long periods. Do not continue to stare at the reflected
light if it appears uncomfortably bright. Staring directly into the beam may

cause damage to the eye.
1.1.8 Handling Liquid Nitrogen

Liquid nitrogen boils at a temperature of -195oC. Surfaces cooled to this
temperature, including pipes used for filling cold-traps, must never come into
contact with skin which would immediately become frozen to the surface.
Similarly, when pouring liquid nitrogen, care must be taken to avoid splashing
the liquid onto any unprotected areas of skin or eyes.
Liquid nitrogen should only be used in a well ventilated area to avoid any
possibility of the evolved nitrogen gas displacing the oxygen in the room and
thereby causing suffocation.
Oxygen boils at a higher temperature (-183oC) than nitrogen; any large surface
area cooled to liquid nitrogen temperature and open to atmosphere can act as
a condenser, producing a high concentration of oxygen locally which could be
a fire hazard.
The change in volume as nitrogen changes from liquid to gas is in the
approximate ratio 1:700, thus liquid nitrogen must never be introduced into a
closed volume or explosive pressures could be generated.
1.1.9Taking the Vacuum System to Atmospheric Pressure

The various chambers of the vacuum system are designed to operate at low
pressure, hence care is needed when backfilling from compressed gas
cylinders otherwise the system could be damaged. Do not pressures the
system above atmospheric pressure. It is always advisable to backfill the
system with a dry, inert gas, thereby avoiding the production of an explosive
mixture if, for example, an inflammable gas has been used in a preparation
chamber.
1.1.10 Rotary Pump Exhaust

Rotary pumps can produce a harmful oil mist exhaust, particularly when
pumping large volumes of gas; it is advisable to pipe the exhaust gases out of
the room.
Similarly, the operator should be aware of any possible hazardous reaction,
e.g. the emission of toxic vapour, which could take place in the specimen when
subjected to the environment of the high vacuum chamber or preparation
chamber. If this is a possibility then any pump exhaust gas, including that from
absorption pumps, should be vented externally.
1.1.11 Radiation Hazard

An intense flux of X-radiation can be generated within the instrument. Shielding
is more than adequate to limit the dose rate outside the instrument to safe
levels.
However, if any modifications are undertaken by the user, the need to maintain
an adequate level of shielding must be borne in mind. This is particularly
important if the large viewport at the front of the analysis chamber is removed.
The viewport is equipped with a thick lead glass shield. This MUST NOT BE
REMOVED under any circumstances and MUST ALWAYS be in place to
maintain adequate shielding for the operator when X-Rays are being
generated. If this viewport is changed for an alternative version, then

Equipment Return Declaration
ADEQUATE CHECKS MUST BE CARRIED OUT FOR LEAKAGE OF X-

RADIATION before using the instrument. No lead glass X-Ray protection
windows should be removed. Other viewports also give unsafe levels of
radiation.
1.1.12 Thoriated Filaments

Thoriated filaments are used in several components and optional extras in
AXIS Ultra DLD. They are fitted to the Monochromator X-Ray gun and to
MiniBeam ion guns.
Thorium is a naturally occurring low level alpha-emitter. Although the micro-

scopic amount of thorium present on each filament presents no significant
hazard, it is good practice to reduce any potential exposure to the minimum
possible. It is suggested, therefore, that these filaments be handled only with
a gloved hand and that both old filaments and gloves be sealed in a plastic
bag and disposed of in accordance with local regulations.
Warning:
Thorium is toxic and may cause cancer. It is harmful by inhalation, contact

with skin and if swallowed.
In case of accident, or if you feel unwell, seek medical advice immediately.
Wear suitable protective clothing, gloves and eye / face protection.
Do not breath dust.
If swallowed, wash out mouth with water provided person is conscious. Call a
physician.
In case of skin contact, flush with copious amounts of water for at least 15
minutes. Remove contaminated clothing and shoes. Call a physician.
If inhaled, remove to fresh air. If breathing becomes difficult, call a physician.
In case of contact with eyes, flush with copious amounts of water for at least
15 minutes. Assure adequate flushing by separating the eyelids with the fin-
gers. Call a physician.
1.2 Equipment Return Declaration
INTRODUCTION
Before you can return your equipment you must warn your supplier/service centre if
the substances you used and/or
produced in the equipment can be dangerous. You must do this to comply with
health and safety at work laws.
You must complete the declaration (DOC.075) and send it to your supplier before you
dispatch the equipment. If you do not, your supplier/service centre will assume that the
equipment is dangerous and they will refuse to accept it. If the declaration is not com-

pleted correctly, there may be a delay in processing your equipment.
GUIDELINES
Take note of the following guidelines:
Your equipment is 'uncontaminated' if it has not been used or if it has only
been used with substances that are not dangerous. Your equipment is 'con-
taminated' if it has been used with any dangerous substances.
If your equipment has been used with radioactive, micro-biological sub-
stances or biologically active bio-chemical substances, it must be decontami-
nated using an approved decontamination process before an engineer at any
Kratos service centre can proceed with any repair or service. You must supply
independent proof of decontamination (for example a certificate of analysis to
your supplier with the declaration DOC.075). Phone your service centre for
advice.
We recommend that contaminated equipment be transported in vehicles
where the driver does not share the same air space as the equipment.
PROCEDURE
Use the following procedure.
1. Contact your service centre and obtain a return authorisation number for your equip-
ment.
2. Complete the declaration (DOC.075) and fax or post a copy to your service centre.
The declaration must arrive at the service centre and permission to ship obtained
before the equipment is despatched.
3. Remove all traces of dangerous gases. Pass an inert gas through the equipment
and any accessories that will be returned to your service centre. Drain all fluids and
lubricants from the equipment and its accessories.
4. Disconnect accessories from the equipment. Safely dispose of the filter elements
from any oil mist filters.
5. Seal up all of the equipment's inlets and outlets (including those where accessories
were attached). You may seal the inlets and outlets with blanking flanges or heavy
gauge tape.
6. Seal contaminated equipment in a thick polyethylene bag. If you do not have a poly-
ethylene bag large enough to contain the equipment, you can use thick polyethylene
sheet.
7. If your equipment is a large pump (or other large piece of equipment), strap the
equipment and its accessories to a wooden pallet. Contact your service centre if you
cannot meet this requirement.
8. If your equipment is too small to be strapped to a pallet, pack it in a suitable strong

box.
9. If the equipment is contaminated, label the pallet (or box) in accordance with laws
covering the transport of dangerous substances.
10. Give a copy of the declaration to the carrier. You must tell the carrier if the equip-

ment is contaminated.
11. Seal the original declaration in a suitable envelope and attach the envelope
securely to the outside of the equipment package. WRITE YOUR RETURN AUTHORI-
SATION NUMBER CLEARLY ON THE OUTSIDE OF THE ENVELOPE OR ON THE
OUTSIDE OF THE EQUIPMENT PACKAGE
(DOC.102 Issue2 January 2001)

EQUIPMENT RETURN / REPAIR DECLARATION faxback +44 (0)161 8884402

You are required to: Return Authorisation Number:
Know and Declare all the substances that have been used in this equipment
Read the procedure (DOC.102) before you complete this form
When parts are being returned, obtain a returns authorisation number and send or fax this form completed to your
local Service Centre before the parts are sent.
SECTION 1 . EQUIPMENT
Equipment model and type number:
Serial Number:
Has the equipment been used, tested or operated? yes: ___ - Go to Section 2, no: ___ - Go to section 4
SECTION 2 - SUBSTANCES USED IN THE EQUIPMENT
Are any of the substances which have been used in this equipment:
Radioactive yes: ____ no: ____
Micro-biological (living cells) yes: ____ no: ____
Biochemical (proteins/peptides) yes: ____ no: ____
Polymers yes: ____ no: ____
Dangerous to human health yes: ____ no: ____
If you have answered no to all these questions, go to section 4, otherwise go to section 3 and section
3a on the following pages. Your Service Engineer / Centre will not be able to carry out any work on
your equipment if it is contaminated with any substance which is radioactive or biologically active and
dangerous unless you:
Decontaminate the equipment and
Provide proof of decontamination
YOU MUST CONTACT YOUR SERVICE CENTRE BEFORE YOU RETURN EQUIPMENT
SECTION 3 - LIST OF SUBSTANCES USED IN THE EQUIPMENT

Substance name Chemical Special precautions required Special action required
symbol after spillage or human contact
Are the hazards restricted to the vacuum envelope? yes: ____ no: ____
If no please give precise details of other parts of the equipment that may be contaminated:
___________________________________________________________________________________________

Please add any further information on a separate sheet and send with this form # now complete section 3a over
SECTION 4 - RETURN INFORMATION
Please state reason for return:
Are you making a warranty claim against this return: yes: ____ / no: ____
SECTION 5 . DECLARATION
Name (Print): _________________________________________ Job Title:______________________________
Organisation: ____________________________________ Phone number: ______________________________
Address: __________________________________________________________________________________
_________________________________________________________________________________________
I declare that the above details are accurate and that I have not withheld any relevant information. I have followed
the requirements of the returns procedure DOC.102.
Signed: _______________________________________________ Date: __________________________
copy of DOC.075 Page 1/2 Issue 5 July 2002
SECTION 3a - EQUIPMENT STATUS DECLARATION

SECTION 3a . EQUIPMENT STATUS DECLARATION
i) Micro-biological Substances:
If the instrument has had micro-biological substances (bacteria/viruses etc.) inserted then:
1. Were any of the substances living or active? yes: ____ no: ____
2. If yes, what class of active micro-organism
has been processed? Class 1: yes: ____ no: ____ , Class 3: yes: ____ no: ____
Class 2: yes: ____ no: ____ , Class 4: yes: ____ no: ____
Note:
If the instrument has had living micro-biological substances of class 2 inserted, then the instrument must be
de-contaminated before it is either returned to Kratos or before a Kratos engineer is asked to work on any
contaminated part of the equipment.
There must be a signed declaration that the decontamination has been carried out to approved procedures (these
must be referenced and copies supplied to Kratos on request).
If the instrument has had living class 3 or 4 micro-biological substances inserted, then the instrument must be
serviced by trained engineers of the institute or organisation to which the instrument belongs.
If you have any doubts about the classification of the substances that have been processed through the instrument
then please contact Kratos. Where there are any doubts, then the action taken must be commensurate with the
highest classification that may have been in contact with or processed through the instrument.
ii) Bio-chemical Samples
Please categories the samples as follows: Soluble in aqueous Soluble in organic

detergent solutions: solvents such as
acetonitrile
a) biologically active proteins/peptidesyes: ____ no: ____yes: ____ no: ____ yes: ____ no: ___
b) synthetic proteins/peptidesyes: ____ no: ____ yes: ____ no: ____ yes: ____ no: ___
c) nucleic proteins/peptides yes: ____ no: ____ yes: ____ no: ____ yes: ____ no: ___
d) synthetic compounds yes: ____ no: ____ yes: ____ no: ____ yes: ____ no: ___

iii) All Bio-chemical, Polymer or other Samples Dangerous to Human Health
You must declare the nature of the hazard to health taking account of the maximum amount and variety of sample
processed and all their associated risks.
Comments
a) Toxic yes: ____ no: ____
b) Immunogenic yes: ____ no: ____
c) Corrosive yes: ____ no: ____
d) Reactive yes: ____ no: ____
iv) Radio-Active Contamination
If the instrument has had radio-active substances inserted or has been in a radioactive environment then the
following questions must be answered:
1. Has the instrument been decontaminated to an approved procedure? yes: ____ no: ____
(Please quote procedure reference): _________________
2. Has the instrument been tested (after any decontamination) for residual radio-active levels?
yes: ____ no: ____
If yes, what maximum radiation level was recorded? _________________
Note: An Instrument that has been radio-actively contaminated must NOT be returned to Kratos unless it has been
fully de-contaminated and is in a safe condition.
Now, please complete sections 4 and 5 on page 1
copy of DOC.075 page 2/2 Issue 5 July 2002

13 July 2009
Chapter 2
AXIS Technology as
Applied to the AXIS
Ultra DLD
Chris Blomfield, Simon Hutton & Adam Roberts
2.1 Introduction.
X-ray photoelectron spectroscopy (XPS), often referred to as electron spec-
troscopy for chemical analysis (ESCA), is a surface analytical technique that
has matured into an essential tool for many materials characterisation labo-
ratory's since the introduction of the first commercial instruments in the late
1960's.
This Chapter reviews the instrumental developments that have lead to

improved spatial resolution and in turn microscopic performance in XPS.
Specific reference is made to the microprobe approach developed by Kratos
using a combination of a magnetic immersion lens in combination with an
aperture in the electrostatic lens. The use of the spherical mirror analyser
(SMA) for fast parallel imaging is also introduced.
2.2 X-ray photoelectron spectroscopy

The are many excellent texts available which review the basic principals of
XPS for example Vickerman [1], Briggs and Seah [2] and Briggs and Grant
[3] and therefore only a very brief overview is presented here. The popular-
ity of the technique when compared with other surface analytical techniques
can be attributed to a unique combination of surface and chemical sensitiv-
ity as well as relatively straightforward means of quantification.
FIGURE 1 shows a sample surface illuminated with X-rays of energy h.
Photoelectrons of kinetic energy (KE) are emitted from the sample surface
via the photoemission process. In the photoelectron spectrometer the
21
X-ray photoelectron spectroscopy
kinetic energy of the photoelectron is measured to give the binding energy

(BE) with which the electron was bound to the nucleus via the relationship
given by Equation 1. represents the combined electron spectrometer and
sample work functions and is an instrument dependent factor normally
derived for each instrument as part of a calibration procedure
Eqn (1) BE (eV) = h - KE -
FIGURE 1. The photoemission process.
The technique derives its chemical sensitivity from the fact that nearest
neighbour atoms will have a direct effect upon the binding energy of the
core level electrons. Therefore any change in the chemical environment
such as oxidation state will lead to a modification of the KE. The surface
sensitivity of the technique can be explained by the fact the relatively low
energy photoelectrons can travel only a short distance though the solid with-
out undergoing inelastic scattering. The average distance the photoelectron
can travel without energy loss is defined as the inelastic mean free path
(IMFP) [3]. The sampling depth, d from which 95% of all photoelectrons are
detected is given by the relationship:
Eqn (2) d = 3
2.2.1 XPS instrumentation

Instrument design has evolved significantly since the very early experiments
of Siegbahn et al. [4] but all modern instruments are based upon the same
key components: X-ray source; electron transfer lens; electron energy ana-
lyser; and detection system. All of these components are contained within
an ultra high vacuum (UHV) envelope. This is usually manufactured from
stainless steel with a high degree of electromagnetic shielding using typi-
cally mu-metal.
22 Chapter 2 AXIS Technology as Applied to the AXIS Ultra DLD

2.2.1.1 The X-ray source

Modern XPS instruments rely mostly upon Al monochromatic X-rays as the
primary photon source, however, most manufacturers offer achromatic
sources of usually Mg and Al as optional items. The dominance of the mon-
ochromatic source in itself shows the advances in the technique, a decade
earlier the achromatic source would have been the standard.
The purpose of the X-ray monochromator is to produce a narrow X-ray line
by Bragg diffraction in a crystal lattice. The single Al anode which is often at
high potential (15 kV) is bombarded by thermonically emitted electrons from
a filament at, or close to earth potential These two components together
constitute the "X-ray gun". The electron beam current can be as high as
tens of mA so at 15 keV electron beam energy several hundred watts of X-
ray power must be dissipated mostly in the form of heat. This heat dissipa-
tion is achieved by water cooling behind the Al anode, which consists of a
thin layer of Al on a typically Cu based substrate. Heat dissipation can be a
limiting factor in sources which utilise a microscopic electron beam to form a
microscopic X-ray spot.
The "X-ray gun" is used in combination with a focusing monochromator con-
sisting of a single or combination of quartz crystals. The crystal backplane
is set on a Rowland circle with radius R and the crystal bent to a radius 2R
the so called Johann geometry. The larger the radius of the Rowland circle
the smaller the energy spread in the X-ray spot per mm. Commercial instru-
ments use either a toroidal or ellipsoidal crystal geometry depending upon
whether they utilise a macroscopic or microscopic monochromator geome-
try. The AXIS Ultra DLD uses a 500 mm Rowland circle monochromator, as
shown in FIGURE 2.
FIGURE 2. The AXIS X-ray source and monochromator.
The advantage of the monochromatic source over the achromatic source is

many fold. Only the major Al K component is diffracted from the quartz
crystal therefore the photon line width is inherently narrower. The natural Al
K1,2 line has a width of < 0.9 eV whereas the monochromated line is < 0.26
eV. The broad energy range, low intensity or so-called Bremsstrahlung radi-
ation and the X-ray satellites due to K radiation are also removed from the
X-ray beam when using a monochromatic source producing a simpler

spectrum. The removal of x-ray satellites and Bremsstrahlung radiation

leads to lower background levels and better signal to noise ratios from mon-
ochromatic sources. Furthermore, removal of the Bremsstrahlung radiation
also reduces sample X-ray damage, however, some microfocused mono-
chromatic X-ray sources can deliver high X-ray flux per unit area causing
increased damage rates relative to those that might be seen with an achro-
matic source on X-ray sensitive samples.
a) b)
FIGURE 3. a) micro-focused x-ray source b) macro-focused x-ray source with lens defined
virtual probe.
Commercial instruments fall into two categories, those which use the X-ray
source to define the area of analysis, and those which use the electron
transfer lens. The source defining system utilises an electron beam on the
Al anode of variable size. X-rays from which are focused to give a variable
size X-ray spot on the sample surface (FIGURE 3). The magnification factor
of the monochromator is normally set to unity so a fine electron emitter of
typically LaB6 type can produce spot diameters as small as 10 m. Such
systems are known as microscopic monochromators Larson et al. [5]. The
electron transfer lens defining instruments such as the Kratos AXIS series of
photoelectron spectrometers normally rely upon a fixed macroscopic X-ray
spot to illuminate approximately 1 mm diameter of the sample. The electron
transfer lens then acts as a virtual probe to select small areas for analysis as
shown in FIGURE 3b.
XPS analysis of insulating materials is complicated by the tendency of such

samples to acquire a surface charge during photoemission leading to detri-
mental spectral artefacts. This effect is compounded by the use of mono-
chromatic X-rays as there are fewer sources of low energy electrons in the
vicinity of the sample. Advances in charge compensation techniques have
been the primary reason for the wider application of monochromatic sources

in routine analysis. All modern XPS instruments use a secondary source of

neutralising electrons see for example the patent of Walker and Page [7]
and the further discussion in Section 3.0.4.2 or a combination of electrons
and ions Kelly [8]. X-ray microprobe systems with a higher X-ray flux gener-
ate a greater localised charge at the sample surface which can place
greater demands on the charge neutraliser system.
2.2.1.2 Transfer lens
The role and design of the transfer lens depends on the type of instrument.
The X-ray microprobe based systems utilise an inherently simpler lens sys-
tem which works in a similar high transmission mode independent of the
type of analysis which is being carried out. The virtual probe approach used
for the AXIS series requires a much more sophisticated design as it is
essentially defining the analysis area in small spot spectroscopy. These
lenses are largely multi-component electrostatic lenses. More recently
magnetic immersion lenses have been introduced to increase the collection
efficiency of photoelectrons of the transfer lens column. The magnetic
immersion lens has a low spherical aberration coefficient and so enables a
large angle of acceptance which is particularly useful in increasing the count
rates in virtual probe instruments at small analysis areas.
FIGURE 4. Electron optical elements of the AXIS virtual probe photoelectron spectrometers.

FIGURE 4 shows the arrangement of the AXIS virtual probe type of instru-
ment. For simplification the first part of the lens, the "objective," is assumed
to have no over all retardation. It simply collects and transfers electrons from
the sample to an area defining aperture. There are a number of variations of
objective lens but all now use either a magnetic immersion lens to increase
the collection angle of the bottom half of the transfer lens or a large solid
angle electrostatic lens. A variable iris can also be used to control the angle
of acceptance of the objective lens prior to the aperture. The upper part of
the lens after the aperture acts as a projector lens to transfer electrons from
the aperture plane into the entrance of the analyser, the last stage of this
lens is the retarding lens. Clearly by varying the diameter of the aperture a
different area on the sample can be analysed and thus small areas of analy-
sis < 10 m diameter can be achieved.
2.2.2 The AXIS Spectrometer Lens Geometry
The AXIS photoelectron spectrometers are built around the established

AXIS lens technology, with co-axial magnetic immersion lens, charge neu-
tralisation source and electrostatic lenses. The AXIS lens geometry is
shown in the schematic FIGURE 5.
FIGURE 5. AXIS lens geometry
2.2.2.1 The Magnetic lens

The magnetic immersion lens of the snorkel type is positioned below the
sample and used to focus the photoelectrons ejected from the surface to the
spot size aperture. Compared with other (electrostatic) lens systems in use
the magnetic lens spherical aberration is at least two orders of magnitude
smaller. The schematic diagram shown in FIGURE 6 shows the lens oper-
ating in standard mode, projecting its imaging field clear from its mechani-
cal structure.

To provide limited detail, the lens comprises an iron circuit with a gap
through which extends an iron pole piece. A water cooled solenoid energies
the iron circuit to produce an intense magnetic field between the pole piece
and the outer body of the lens. The modelled magnetic flux lines are shown
in FIGURE 6. For optimum performance the flux density at the pole must be
a maximum, usually limited by the iron saturation value.
FIGURE 6. A schematic diagram of the magnetic immersion lens.
The focal distance of the magnetic lens must be kept constant as a function
of the KE of the photoelectrons collected by the spectrometer. As a result a
lens function defining the current through the magnetic coil as a function of
KE is defined and stored as part of the configuration of the spectrometer.
The magnetic lens can be used in combination with the electrostatic lens
elements below the selected area aperture to define the size of the selected
area, or virtual probe at the surface of the sample.
The advantages in the use of the magnetic lens include:

High collection efficiency
large solid angle of collection - discussed further in Section 2.2.2.3
low spherical aberration and therefore high magnification (ca x10) in both
imaging and spectroscopy modes.
high small spot spectroscopy sensitivity.
The magnetic lens is discussed further in the European Patent EP 0 243

060 B1.
2.2.2.2 The Charge Neutraliser
The charge neutralisation system used in the AXIS Ultra DLD spectrometer
consists of a filament and electrode plate mounted at the bottom of the elec-
trostatic input lens system. The magnetic field generated by the magnetic
immersion lens is used to confine low energy thermionically emitted elec-

trons from the filament and transport them to the sample surface. The
charge balance electrode acts to direct the neutralisation electrons from the
filament into the magnetic field. This is shown in the schematic diagram in
FIGURE 7.
FIGURE 7. Co-axial charge neutralisation - thermionic electrons from the filament.
As the electrons are a charged particle moving through a magnetic field,

they experience a force perpendicular to the plane defined by the movement
and the magnetic field. This causes the neutralisation electrons to follow a
spiral path towards the sample.
The thermionically emitted electrons from the filament are not the only
source low energy electrons for neutralisation. Models of the neutraliser
suggest that low kinetic energy photoelectrons that are over focused by the
magnetic lens are repelled back towards the surface of the sample by the
potential on the charge balance electrode. These low energy electrons then
combine with the thermionically emitted electrons to form the cloud of oscil-
lating charge neutralisation electrons. The final source of electrons is the
high KE photoelectrons that are under-focused and impact with the charge
balance electrode. These high energy photoelectrons are of sufficient
energy to generate secondary electrons from the charge balance electrode.
The secondary electrons then interact with the magnetic field and combine

with the other charge neutralisation electrons. These two processes are
shown in the schematic diagram, FIGURE 8.
FIGURE 8. Other sources of charge neutralisation electrons.
The charge neutralisation system is simple to operate during data acquisi-

tion. The parameters that may be controlled are the filament current, fila-
ment bias and the charge balance. Once these parameters have been
optimised the charge neutraliser will work with most classes of insulating
samples under the same conditions. There may be specific samples that
will require the neutraliser parameters to be modified to effectively neutralise
a surface charge. Similarly, as the neutraliser ages the parameters may
need to be modified to maintain efficient neutralisation during data acqusi-
tion.
The use of the charge neutraliser and the optimisation of the neutraliser
parameters is discussed in the Acquisition Chapter.
2.2.2.3 Lens Modes and the Solid Angle of Collection
The solid angle of collection is dependent on two parameters - the lens

mode used and the iris setting. The AXIS Ultra DLD is tested and supplied
to the user with four defined lens modes which may be selected independ-
ently of the analyser pass energy that is to be used. The lens modes are
defined by particular combinations of magnetic lens current and electrostatic
lens voltages as a function of the kinetic energy of the photoelectrons ana-
lysed.
The properties of the lens modes are as follows:
Electrostatic Lens Mode
In this lens mode the magnetic lens is switched off and focusing is achieved
via the electrostatic lenses only. The lens system in this mode generates
approximately a x1 magnification of the selected area aperture. Using elec-
trostatic lens mode with the slot aperture will give an approximate analysis

area on the sample of 2 x 1mm which is essentially the area illuminated by

the monochromatic x-ray source.
The maximum acceptance angle in this mode is about +/- 6 degrees with the
iris set open, reducing to +/- 1.5 degrees with the iris closed.
Spectroscopy FOV 1 (Field of View 1)
This lens mode is used to give the highest sensitivity in spectroscopy mode.
Both the magnetic and electrostatic lenses below the selected area aperture
are in use resulting in higher magnification than that of electrostatic mode.
With the slot aperture selected the analysis area in spectroscopy mode is
approximately 700 m in the x-axis and 300 m in the y-axis. This lens
mode is suitable for large area analysis at both high and low energy resolu-
tion with the monochromatic x-ray source.
The solid acceptance angle of this lens magnification in spectroscopy mode

is about +/- 15 degrees.
FOV 2 and FOV 3
As with FOV 1, FOV 2 and FOV 3 can be used in either spectroscopy or

imaging mode with both the magnetic and electrostatic lenses used. The
magnetic lens creates a much higher magnification than the electrostatic
mode of operation with a maximum magnification of about x10 to the
selected area aperture. Spherical aberrations are reduced aiding good ulti-
mate spatial resolution with a very tightly defined focus. In addition a large
acceptance angle of about +/- 15o can be achieved giving high sensitivity
but with a small depth of field. This means that the sample height (z-axis)
must be kept within +/- 20m of the optimum focal height to remain in focus.
For selected area spectroscopy the spatial resolution (spot size) quoted
when using the selected area apertures are only calibrated for FOV 2. The
spot size is determined by a combination of the lens mode, aperture and iris
setting. The user should further note that the sample must be at the correct
focal height for these analysis areas to be as defined.
When used with the imaging analyser the three different lens modes provide
three different fields of view, with FOV 1 being approximately 900m2, FOV
2 being approximately 400m2 and FOV 3 being 200m2. The exact area
of the surface imaged with each lens mode is calibrated during the testing of
the spectrometer and is dependent on the tuning of each individual instru-
ment.
2.2.2.4 The Scan Deflection Plates
The electrostatic lens column contains a set of octopole deflection plates

below the selected area aperture. The position of the scan plates in the

electrostatic lens column are shown schematically to the left hand side of
Figure 9.
FIGURE 9. Schematic diagram of the AXIS Ultra DLD electrostatic lens column and the octopole
scan plates.
By applying a fixed voltage to the scan plates the selected area analysis
position can be deflected from the central axis of the spectrometer. The
deflected analysis area is shown in the upper right hand part of FIGURE 9.
This mode of spectral acquisition allows the user to acquire mulitpoint spec-
tra from a sample without translating the stage.
If the voltages on the scan plates are varied in a raster pattern across the
surface and spectral intensity acquired at each position, a scanned image of
the surface may be acquired. This is shown schematically in the bottom
right hand side of FIGURE 9. The scanned image has the advantage over
parallel imaging that the area imaged can be larger than the largest area
defined in FOV 1. However, the spatial resolution is limited to size of the
aperture used to generate the scanned image.

2.2.3 Electron Energy Analysers
Almost all commercial instruments operate a hemispherical sector analyser

(HSA) also referred to as a concentric hemispherical analyser (CHA). The
analyser consists of two concentric hemispherical electrodes between which
the electrons pass.
2.2.3.1 XPS imaging.
It is clear to see from the above discussion that small spot XPS instruments
with a microscopic capability can be made to form XPS maps. This is
achieved in one of two ways. The X-ray spot defining systems with micro-
scopic monochromator sources can either form a small probe on the sample
and then scan the sample with respect to the probe or scan the X-ray gener-
ating electron beam across the Al anode target producing a scanning beam
across the sample. Alternatively, the virtual probe instruments may have an
electrostatic deflection system placed before the area defining aperture
which can be made to effectively scan the point of analysis across the sam-
ple. In all cases the analyser is set to detect photoelectrons at a particular
kinetic energy while the X-ray probe (virtual or real) rests for a pre-deter-
mined time at each point on the sample. With a multi-channel detector sig-
nal may be recorded simultaneously within a narrow energy window. In all
cases the map must be constructed from a post-acquisition processing
exercise. One limitation of the XPS mapping approach is that as each map
is built up pixel by pixel it can be time consuming. Additionally the spatial
resolution of each map is determined by the minimum size of the X-ray or
virtual probe.
2.2.3.2 Parallel XPS imaging.
Parallel XPS imaging has now become the most widely used form of XPS
imaging. Images can be detected directly normally with a 2-D detector, this
method of acquisition needs a macroscopic X-ray source and a modification
to the standard analyser. Two methods are commercially available, one
where a Fourier Transform lens is used after the retardation lens and then a
further Fourier Transform lens following the analyser, Coxon [9]. The second
employs a spherical mirror analyser designed by Page [10] and used in the
AXIS Ultra DLD and AXIS Nova instruments.

FIGURE 10. Au grid parallel images integrated for different times
The parallel imaging technique has two major advantages over traditional
scanning probe methods. Spatial resolution is limited only by the aberra-
tions in the lens system allowing a spatial resolution at the sample of a few
microns. Also the speed of data collection is greatly enhanced by the simul-
taneous detection of photoelectrons from a large number of adjacent posi-
tions. For example FIGURE 10 shows a series of parallel photoelectron
images acquired at the Au 4f photoelectron energy. Each image contains
64,000 pixels recorded simultaneously for acquisition times from 1 to 20
seconds. To acquire a similar amount of data using the probe mapping
method acquisition times would be significantly greater.
By acquiring images at small energy increments over a narrow energy

range spectroscopic information can be efficiently collected for each pixel of
the image. Fast parallel imaging can be used to find areas of surface inho-
mogeneity or features of specific interest. Normally parallel imaging instru-
ments are arranged so that the lens systems produce pre-determined
magnifications or fields of view.

FIGURE 11. Image magnifications.
FIGURE 11 shows a series of images acquired for the same Au grid at dif-
ferent magnifications. In effect the magnification supplied by the objective
lens of FIGURE 4 is varied to produce a magnified photoelectron image at
the analyser entrance. FIGURE 11 shows an image of a 25 m pitch Au grid
with 5 m bar width acquired at the Au 4f photoelectron binding energy.
Spatial resolution in imaging, as is common with other microscopy tech-
niques, is normally determined via a retrospective line scan across a fea-
ture. The lateral resolution being defined as the distance between the two
points at which the intensity of the line scan is 80% and 20% of the maxi-
mum.
2.2.4 Applications of small spot and imaging XPS.
Now that we have seen the various aspects of instrumental design and how
they interact in each type of instrument it may be useful to see how these
components come together in the modern instrument to perform imaging
and small spot analysis.
The surface chemical analysis of various oxides of TiAlN compounds has

played an important role in the understanding of the oxidation resistance of
these materials in certain high temperature cutting applications, McIntyre

[11]. A TiAlN film deposited on stainless steel and annealed in air for 1 hour
at 950C was analysed by XPS. Large area spectroscopy showed the pres-
ence of both Fe and Cr from the stainless steel substrate at the surface.
XPS imaging was performed on the sample surface revealing a distribution
of Fe across the surface in an island-like formation.
FIGURE 12. Ti, Fe and O parallel images.
Using XPS imaging we have the ability to distinguish between two different
chemical states of an element on the surface of the sample. In this case
large area spectroscopy indicated the presence of more than one oxygen
chemical state. These were attributed to the oxides of Fe (531.8 eV) and Ti
(529.7 eV) and the lateral distributions of these oxygen states were imaged,
FIGURE 12. Chemical state imaging highlights the ability of XPS to show
the surface distribution of different chemical species. Small spot XPS spec-
tra were then acquired from an area of high Ti and a second area of high Fe
concentrations confirming the imaging results, FIGURE 13.

FIGURE 13. Small spot XPS.
Such elemental analysis would have been possible by several surface anal-
ysis techniques but the chemical state distribution would be difficult to
observe by other surface sensitive techniques. The relative independence
of XPS to matrix effects means that reliable quantification may be obtained
from such small areas. The surface analysis points to the fact that both Fe
and Cr have segregated through the TiAlN film from the stainless steel sub-
strate to contribute to the surface oxide layer form after air annealing.
2.2.5 Summary.
XPS maps can be acquired in a serial scanned manner with a spatial resolu-
tion of approximately 15 m. XPS imaging systems are now available that
can acquire images directly from the sample surface using 2-D parallel
detection systems typically with a spatial resolution of < 3 m. Commercial
instruments now combine both imaging and small spot spectral acquisition
capabilities to enable surface chemical analysis of small features on the
micron scale. The future direction of the technique is to achieve higher count
rates at smaller areas and to push forward XPS imaging to be a genuine
sub-micron chemical characterisation technique.

13 July 2009
Chapter 3
Overview of the AXIS
Ultra DLD
Adam Roberts
3.1. The Hardware

The AXIS Ultra DLD incorporates market leading AXIS technology including
co-axial charge neutralisation, magnetic immersion lens and real parallel
imaging. Sample manipulation in the sample analysis chamber (SAC) is
fully automated. Each component of the spectrometer will be covered in the
following sections with details description for operation of the spectrometer
in spectroscopic and imaging modes.
The vacuum chamber and control electronics are linked but articulated. The
total weight is approximately 1200 kg. The standard instrument is 2.09 m
high, 0.95 m wide and over 3 m long (including the transfer probe) with an
approximate floor loading of 500 kgm-2 on eight heavy duty castors. The
site requirements are presented in detail in the AXIS Ultra DLD site require-
ment document which is available by contacting Kratos Analytical.
3.1.1 Services Required
The services required for operation of the AXIS Ultra DLD are as listed in
Section 3.1.1.1 to Section 3.1.1.6. These details are summarised from the
full site requirement document.
3.1.1.1 Water
The instrument is supplied with a closed circuit water chiller which is capa-
ble of dissipating approximately 2.0 kW and supply water at the required
flow rates to the instrument. It should be filled with deionised water with
conductivity < 1Scm-1 which will be maintained by the use of the in circuit
deioniser cartridge. The standard pipe length between the chiller and spec-
trometer is 6m.
37
The Hardware
3.1.1.2 Electricity
A reliable and clean 230 V +10 % -6% AC 50/60 Hz single phase electricity
supply with a 50 A capacity routed via a fused isolation box is required for
operation of the spectrometer. A good earth is essential and the neutral
voltage must be nominally zero. The electrical supply should be continuous
and any damage caused to the instrument through power failures is the
responsibility of the user.
3.1.1.3 Air Conditioning and Ventilation

Permissible ambient temperature range is 22 +/- 5 0C with a maximum vari-
ation of 2 0C per day and stability of better than 1 0C per hour.
Relative humidity should be less than 65% non condensing meaning that
the combination of ambient temperature, relative humidity and inlet water
temperature must not result in condensation on any of the water cooled
components.
The heat dissipation during normal operation can be up to 5 kW (including

the chiller) however, during baking this can rise to 8 kW. It should be
ensured that this quantity of heat can be dissipated in the laboratory without
the ambient temperature rising above the maximum level.
3.1.1.4 Gas Supplies
Liquid Nitrogen - a pressurised supply of liquid nitrogen is required as a

cold trap refrigerant when the TSP cryoshield is in use. Note that the cry-
oshield is not commonly used during sample analysis.
Nitrogen gas (N2) - 1 kgcm-3 (15 psi) for venting the vacuum chamber. The
purity should be 99.99% (dry).
Compressed air - 5.6 kgcm-3 (80 psi) for operating the pneumatic valves.
Argon (Ar) - 0.5 kgcm-3 ( ~7.5 psi) with purity >99.99% used for Ar+ ion
etching samples.
3.1.1.5 Vibration
The requirement is for vibration velocity less than 12.5 mms-1 rms within the
band 1 to 100 Hz. Intermittent floor vibrations such as nearby cranes, ele-
vators, folding doors, mechanical hammers and other heavy plant should be
checked also.
3.1.1.6 Magnetic Fields

The requirement is for less than 20 mG peak to peak AC fields in the range
5 - 200 Hz in any direction.
Less than 1 Gauss DC static field is required.
38 Chapter 3 Overview of the AXIS Ultra DLD

The Hardware
3.1.2 Electronic Units

All the control electronic power supply units (PSU) for the AXIS Ultra DLD
are housed in a separate console linked to the vacuum system. There are
no manual controls on any of these units with the exception of the vacuum
control unit (VCU). The units are not user serviceable any faults must be
reported to Kratos Analytical or their representative as soon as possible.
A brief description of each of the electronic units is given in Section 3.1.2.1

to Section 3.1.2.10. Each unit has a power switch that will isolate that single
unit from the mains power supply when switched off. The unit is shown to
be off when the green power LED is not illuminated.
3.1.2.1 DLD Pre-amplifier

This unit acts as the pre-amplifier and receives the raw signal from the
delay-line detector. The green LED on this panel, which is visible through
the smoked panel, of the controller should be continuously illuminated to
indicate that the there is power to the unit. There are no user defined soft-
ware controlled parameters associated with this unit.
3.1.2.2 Analyser Control Unit

The analyser control unit supplies the voltages to the various electrostatic
lenses including the hemispherical analyser and spherical mirror analyser.
The maximum voltage output by this unit is 10 kV. The green LED on the
front panel indicates that there is power to the control unit and the red lamp
indicates that the high voltage supplies within the unit are powered. Note
that the power is removed from this unit when the HV interlock is activated
by the baking routine or high-pressure interlock.
3.1.2.3 Vacuum Control Unit

The vacuum control unit (VCU) is the only unit that is intended for user inter-
action and has an LCD display with push buttons to select various proce-
dures. The operation of the VCU is described further in Section 3.2.
Also present on the front of the VCU is the red high voltage switch. This
switch is protected by a flip cover that should be lifted up if it is necessary to
switch the high voltage off. Switching off the high voltage using this switch
provides a quick way of removing all high voltages from the control units, the
instrument cables and internal lens elements.
3.1.2.4 Stage Control Unit

This unit provides an interface between the sample stage and the control
software. There are no user controls on the unit itself and as all stage
movements are initiated through the Vision software or via the remote con-
trol box.
The stage control unit also provides power and control of the aperture and
iris drive motors. Note that the aperture and iris drives will fail to calibrate if
the Vision software is started when this unit it switched off. Note that the
power remains on to this unit when the HV interlock is activated.
3.1.2.5 NICPU Control Unit

The Ultra DLD Interface Control Processor Unit (NICPU) acts as the inte-
face between the Vision Control software and the AXIS Ultra DLD spectrom-
Chapter 3 Overview of the AXIS Ultra DLD 39

The Hardware
eter. The LED display shows the status of the down loaded code in the
NICPU unit and should show [d.number] where the d and number are con-
tinuously illuminated and the . (dot) is flashing. If the LED displays a flash-
ing [E.number] this indicates that the down load code has become corrupted
and it is necessary to restart the Vision software to re-establish the correct
down loaded code.
3.1.2.6 X-ray Source Control Unit

The X-ray control unit provides the interface between the X-ray source and
the Vision software. The emission current is stabilised by this unit, therefore
providing a constant X-ray flux at the sample. This unit also supplies a read
back for the conductivity of the X-ray anode cooling water which should be
kept below the minimum defined value to prevent a leakage current being
measured.
The X-ray source controller will also ensure that the correct source is
selected in dual X-ray source systems. Control of this unit and therefore the
X-ray source is entirely through the Vision software.
The high voltage required by the X-ray source is generated by the x-ray high
voltage controller (Section 3.1.2.9).
The X-ray source control unit power is turned off when the HV interlock is
activated during either baking or when the high-pressure limit is reached.
3.1.2.7 Deflector Control Unit

This unit supplies the voltages to the octopole scanning unit in the electro-
static lens column. As with the X-ray source control unit, the power is turned
off when the HV interlock is activated during baking or when the high-pres-
sure limit it reached.
3.1.2.8 Magnetic Lens Control Unit

The magnetic lens control unit provides the correct current for the electro-
magnetic lens. The magnetic lens functions for the different operation
modes are defined by the Vision software. There are no user defined con-
trols for this unit. The correction coil to eliminate stray magnetic fields due
to the local operating environment of the instrument is driven by this unit.
This unit is interlocked with the HV and power will be removed from the unit
during baking or when the HV pressure limit is exceeded.
3.1.2.9 X-ray High Voltage Controller

This unit supplies the high voltage to the X-ray source. The maximum high
voltage output by this unit is 15 kV.
This unit is interlocked with the HV and power will be removed from the unit
during baking or when the HV pressure limit is exceeded.
3.1.2.10 Ion Pump and TSP Controller

The ion pump and titanium sublimation pump controller are located behind
the left hand door and are third party units supplied by the manufacturer to
control their pumps. A manual supplied by the manufacturer is included in
the documentation of the AXIS Ultra DLD. Only a brief operating procedure

The Hardware
for the ion pump and TSP are given here and for a more detailed operating
description the third party manual for the pumps should be consulted.
Running the Ion Pump

The ion pump must not be operated at pressures greater than 1E-5 torr and
the instructions here assume that the vacuum in the SAC is below this
value.
During the normal operating condition the only available operations of the
ion pump using the ion pump controller are:
switching on / off the high voltage
selection of the value (voltage or current) that is displayed
selection of the maximum output voltage value
To switch the high voltage on and start the ion pump the rocker switch
should be set to the ON position and the ion pump should be switched on by
clicking on it in the vacuum mimic diagram. When the high voltage is
switched on the front panel LEDs show the preset 3, 5 or 7 kV voltages. By
pressing the V push-button on the front of the controller the voltage is dis-
played in the LED display. To increase the operating voltage press the
upward pointing arrow, once. This will increase the maximum operating
voltage of the ion pump relative to the current operating voltage. pressing
the downward facing arrow will decrease the operating voltage relative to
the current operating voltage.
For general use of the AXIS Ultra DLD spectrometer it is recommended that
the ion pump is operated at 5 kV. This should be increased to 7 kV if the
spectrometer is to be used for continual sputter depth profiling. However,
after the depth profiling it is recommended that the pump is returned to 5 kV
operation.
The current generated in the ion pump elements can be displayed by press-
ing the push-button labelled I.
To switch off the high voltage and therefore turn off the ion pump the HV on
/ off rocker switch should be set to the off position.
Note that the ion pump is interlocked to the pressure reading in the SAC and
will be switched off if the pressure rises above the preset value defined in
the vacuum control unit.
Running the TSP

Full instructions for operating the titanium sublimation pump are included
with the system manuals delivered on instrument installation.
3.1.3 Vacuum Chamber
The vacuum chamber is manufactured from 316 non magnetic stainless

steel with all flanges (except the STC door) sealed with CF copper gaskets.
All materials used in vacuum are UHV compatible materials allowing a base
pressure of 5E-10 torr to be achieved after system bakeout.

The Hardware
Magnetic shielding is provided by mu-metal.
The vacuum system has integrated direct heating bands placed at specific
points around the UHV chamber and a heater mounted on the decking
directly beneath the SAC. The baking bands and heater are thermostati-
cally controlled and are placed such that the chamber and internal compo-
nents will reach an elevated temperature greater than 100 0C. Note that a
baking cover is also provided and must be used during bakout, see
Figure 3.4, Baking the AXIS Ultra DLD, on page 49.
3.1.4 The Vacuum System

The standard AXIS Ultra DLD comprises a sample treatment chamber
(STC) and sample analysis chamber (SAC) with UHV pumping and gaug-
ing. The STC is pumped using a turbomolecular pump backed by an oil
filled rotary pump. The pressure in the STC is measured using a wide range
cold cathode gauge. The sample analysis chamber is pumped by a means
of a getter (ion) pump equipped with an additional titanium sublimation
pump (TSP). The ion pump is fitted with a cryobaffle which may be filled with
liquid nitrogen to increase the pump efficiency of the pump. The pressure in
the SAC is also measured by a wide range cold cathode gauge. The STC is
isolated from the SAC by an electrically operated flap valve allowing the
STC to be vented to dry gas in order to introduce sample bars to the vac-
uum system. A schematic layout of the vacuum system is shown in FIG-
URE 1.

The Hardware
FIGURE 1. A schematic diagram of the AXIS Ultra DLD vacuum chamber
The AXIS Ultra DLD vacuum system is controlled from the Vision Manual
window and is fully safety interlocked. A real-time vacuum mimic diagram is
displayed in the Manual window which may be used to monitor the vacuum
within the two chambers. This mimic diagram and the associated automatic
sequences keys may also be used to operate valves and turn gauges and
pumps on or off. The vacuum mimic diagram is colour coded to give quick
visual information relating to the vacuum level in various parts of the vac-
uum system. FIGURE 2. shows the vacuum mimic diagram for the spec-
trometer in standard operating condition.
FV1
FIGURE 2. Vacuum mimic diagram from the Vision Instrument Manager window.
The valves are labelled in the vacuum mimic diagram and have the following
functions:
V2 Ion source differential pumping valve - this valve is between the ion
source region and the STC to provide differential pumping of the ion source
during sputtering.
V3 Baking valve between turbo pump and rotary pump - used to isolate
the rotary pump from the turbo pump.
V5 Vent valve - low pressure dry nitrogen vent to turbo - this valve operates
between the low pressure nitrogen gas line and the turbo pump. When
opened this will let nitrogen into to turbo pump and backfill the STC with dry
nitrogen.

The Hardware
V8 Ion source Ar gas inlet valve - this valve introduces Ar gas into the ion
source gas line.
V9 Ar gas line roughing valve - this valve links the Ar gas line between V8
and the rotary backing pump and is opened to pump out the Ar gas line.
FV1 Flap valve between SAC and STC - the wide valve between the sam-
ple analysis chamber and the sample entry chamber.
The valves detailed above may be operated by clicking on the icon in the
mimic diagram. The software will ask for confirmation before open or clos-
ing the valve by showing a green lamp which must be clicked again for the
operation to proceed. For commonly used operations which would involve
opening / closing a number of valves in a specific order, the Vacuum Control
section of the Manual window has a number of automatic vacuum
sequences. Using these predefined sequences is strongly recommended
during routine operation of the spectrometer. The automatic vacuum
sequences are discussed in further detail in Section 3.1.6.
3.1.5 Pressure Measurement
The pressure in the analysis (SAC) and sample entry chamber (STC) are
measured using independent wide range cold cathode gauges. The pres-
sure in each chamber is displayed in the vacuum mimic diagram in the
Vision Manual control window and also on the vacuum control unit in the
electronic rack. The pressure readings are updated every second.
The pressure in the backing line between the rotary and turbo pumps is
measured using a pirani gauge located on the turbo side of valve V3. Both
the STC cold cathode gauge and the pirani gauge are switched off during
venting of the STC for sample introduction.
It should be noted that some of the automatic stage sequences are inter-
locked with the pressure measurements. Therefore it is important that the
user ensures that the three gauges are switched on during normal operation
of the spectrometer.
3.1.6 Automatic Vacuum Sequences in Vision Software

Within the Vacuum Control section at the bottom of the Instrument Manual
Control window there are a number of buttons that define a sequence of
valve, gauge and pump operations. Ticking the automatic sequences box
will display the seven defined vacuum sequences, as shown in FIGURE 3.

The Hardware
FIGURE 3. Automatic vacuum sequences in the Instrument Manual Control window of the Vision
software.
3.1.6.1 Vent STC

Pressing this button will vent the STC to dry nitrogen gas. It is suggested
that the retaining screws on the STC door should be released during the
vent cycle to prevent the STC from over pressurising. The Vision software
will initiate the following sequence:
confirm the status of the interlocks, valves, pumps and gauges
turn the STC gauge off
close the backing valve V3
turn the turbo pump off
open the vent valve V5 for 1 second and close again
wait for 60 seconds for the turbo pump to slow down
turn off the pirani gauge on the backing line
open the vent valve V5.
The vacuum controller will leave the vent valve open for 10 minutes during
which time the STC will be purged by dry nitrogen. After this time the
sequence will end by closing the vent valve.
3.1.6.2 Pump STC

Pressing this button will start the pump down sequence of the STC. Note
that this sequence will not start if the vent STC sequence discussed in
Section 3.1.6.1 has not finished. If vent STC sequence has not finished,
simply press the large abort button which will force the vent STC
sequence to abort. The Vision software will initiate the following sequence:
confirm the status of the vacuum system
close the vent valve
open the backing valve
turn on the pirani gauge & confirm pressure > 1E-01 torr
turn on the turbo pump
turn on the STC cold cathode gauge
confirm status of vacuum system

The Hardware
With samples that are not out gassing the STC should pump down to the
low E-06 torr pressure range in approximately 10 minutes. If the STC fails
to pump down to the expected vacuum it is possible that the insertion door
has not formed a good seal on the viton o-ring. In this case it is suggested
that the STC is vented using the vent STC sequence and the viton o-ring
and sealing surface are checked for any debris.
3.1.6.3 Ion Gun Gas On

This vacuum sequence is used to leak Ar gas into the system in preparation
for Ar ion sputtering using the ion source. Ar gas is leaked directly into the
Ar ion source region of the Ar ion gun, with differential pumping provided to
maintain a high vacuum in the analysis chamber. The differential pumping
is provided through the STC and therefore the ion gun gas on sequence
should only be used if the STC is under good vacuum. The system is safety
interlocked so that this sequence will not be executed if the STC is vented or
at poor vacuum. The ion gun gas on sequence is defined as follows:
confirm the status of the vacuum system (pressure in SAC & STC < 1E-
05 torr).
open ion source differential pumping valve, V2
open the Ar gas inlet valve, V8
confirm status of the vacuum system
The Ar gas will leak into the SAC through the Ar ion source, with an increase
in the SAC pressure observed. The total pressure in the SAC will be deter-
mined by the amount of Ar allowed into the SAC which is controlled by the
manual all metal fine leak valve. The operating pressure of the ion source in
the SAC is typically in the 5E-08 to 1E-07 torr range. The operation of the
ion source is discussed further in the relevant chapter.
3.1.6.4 Ion Gun Gas Off

The ion gun gas off sequence is used to stop the flow of Ar gas into the ion
source and then to pump the gas line. The sequence is defined as follows:
close Ar gas inlet valve, V8
close turbo backing valve, V3
open Ar gas roughing valve V9 and pump for 30 seconds
close Ar gas roughing valve, V9
close ion source differential pumping valve, V2
open turbo backing valve, V3
3.1.6.5 Open STC-SAC Valve

This sequence will open the gate valve between the STC and SAC. The
sequence will not open the valve if the pressure in either chamber is > 1E-
05 torr.
3.1.6.6 Close STC-SAC Valve

This sequence will simply close the gate valve between the STC and SAC.

Vacuum Control Unit
3.1.6.7 Pump SAC

The pump SAC is used to pump out the entire vacuum system after it has
been vented. It is assumed that the vacuum system is at atmospheric pres-
sure. The sequence is defined as follows:
confirm the status of the vacuum system, that the gate valve is open and the
backing valve is closed. The pressure of either chamber is not noted.
close the nitrogen vent valve, V5
Open the backing valve, V3 and pump for 20 minutes using the rotary
pump.
turn on the pirani backing gauge
confirm the backing pressure < 1E-01 torr
turn on the turbo pump and wait 30 minutes
turn on the STC cold cathode gauge
turn on the SAC gauge
confirm the status of the vacuum system.
At the end of the pump sequence the STC and SAC will be left pumping
using the turbo pump in the STC. If the STC-SAC gate valve is closed at
this point the SAC will no longer be pumped as the ion pump is not switched
on by this sequence.
3.2. Vacuum Control Unit

As well as using the Vision software to control the vacuum components of
the spectrometer the user can perform the same operations using the vac-
uum control unit which is located in the electronics rack. The vacuum con-
trol unit (VCU) may be operated in user mode, advanced mode or
engineer mode. In user mode manual operation of the valves is not
allowed (however the automatic sequences are still available) so the user
must set the mode to advanced or engineer before the valves can be open /
closed. The VCU defaults to user mode as this is the preferred mode of
operation with control of the valves performed exclusively through the Vision
software. Running the VCU in engineer mode deactivates all safety inter-
locks and therefore extreme caution must be exercised when using the VCU
in this mode.

Vacuum Control Unit
3.2.1 Understanding the Vacuum Control Unit
As discussed in the introduction the VCU provides the user with complete
control of the vacuum system, including operation of some simple vacuum
sequences. The vacuum control unit is shown in FIGURE 4. with the main
menu selected. The buttons on the VCU are fixed, with the labels above or
next to each button reconfigured as a selection is made. To select a particu-
lar option the key pad should be pressed once. In the following pages of the
manual, the convention will be to define a sequence of key presses in the
following way:
Manual > Pumps > TMP > On >
such that the italic word represents the button to be pressed and the > rep-
resents the action of pressing the button. In the figure below the button
associated with the first key press in the sequence above is highlighted.
pressure gauge readings
SAC: 1E-09 STC : 5E-08 RP : 5E-03 12:52:05

-------------------------------- Main Menu -----------------------------------
menu label
Manual
Auto
Options Pressure Log Custom
FIGURE 4. Vacuum control unit interface
The VCU will continuously display the pressure in the SAC, STC and the
pressure in the backing line between the rotary pump and the turbo pump
regardless of the menu displayed. The gauges are displayed on the vac-
uum mimic diagram shown in the Vision software.
Note that the vacuum controller can be operated independently of the Vision
software and will control and report the status of the vacuum components
regardless of whether the Vision software is running or not. If the software is
running, operations performed using the VCU will be displayed in the vac-
uum mimic diagram in the Vision Manual window.

Pumping the AXIS Ultra DLD from Atmosphere
3.3. Pumping the AXIS Ultra DLD from Atmosphere

After venting the AXIS Ultra DLD for routine maintenance the first task will
be to pump the system prior to baking. It is assumed that the spectrometer
is at atmospheric pressure, with the vent valve open and dry nitrogen purg-
ing the SAC and STC vacuum chambers. It is further assumed that the
rotary pump is running with the backing valve, V3, closed and that the gate
valve FV1 between the SAC and the STC is open.
The vacuum control unit has a sequence of operations defined to pump the
entire system from atmosphere. To access this sequence on the vacuum
control unit, starting from the main menu as shown in FIGURE 4. use the
following sequence: auto > pump > start >. This will then start the auto-
matic pump down sequence. At this point the user must insure that the viton
sealed STC door is sealed and not leaking.
The system pump sequence followed by the software is as follows:

check status of pumps, valves and interlocks.
close vent valve V5
open backing valve V3
pump the entire system using the rotary pump for 20 minutes
turn the backing gauge on
check the status of the instrument and confirm that the RP pressure is
less than 1E-01
turn on the turbo pump and wait 30 minutes
turn STC and SAC cold cathode gauges on.
confirm status of the instrument.
At the end of the pump sequence the vacuum control unit will check the sta-
tus of the pressure in the chambers. As part of the safety interlock routine,
the vacuum controller with safely turn off the turbo pump, the STC and SAC
gauges and close the backing valve if the pressure in the STC and / or the
SAC is greater than 5E-05 and / or the backing pressure measured by the
pirani is greater than 1E-01. The VCU display will display an error in such a
case. The reason for the poor pressure in the system should be determined
before another attempt is made to pump the system. If any flanges have
been changed or removed they should be checked first along with the seal
of the viton ring on the STC entry door.
3.4. Baking the AXIS Ultra DLD

A good vacuum in the SAC relies on periodically baking the system to
remove adsorbed gases from the chamber walls and internal components.
The interval between bakes is determined to a large extent by the nature of
the samples analysed and the throughput of these samples. It is suggested
that the system requires baking if the base pressure in the SAC is greater
than 1E-7 torr after pumping non out gassing samples overnight.

Baking the AXIS Ultra DLD
The AXIS Ultra has integrated bake-out heaters situated between the cham-
ber walls and the outer cladding at various places on the spectrometer.
Prior to baking the instrument a number of the components and cables need
to be removed from the instrument and a bake-out cover placed over the
vacuum chambers.
3.4.1 Preparation for Baking the AXIS Ultra DLD
Remove all samples and sample holders from the system before bak-
ing.
The following lists the items to be removed from the machine prior to system
bake-out. Ensure that the protected mains is set to off before proceed-
ing. This is important as the supply cables may have high voltages
applied to them if the protected mains is still switched on. The switch is
located on the vacuum control unit and is protected by a plastic cover, FIG-
URE 5.
Lift flap and press button to switch on / off protected mains
FIGURE 5. Protected Mains.
1. Remove all samples.

2. Remove the CCTV camera and lens. Remove the screws securing the
2 saddle clamps holding the microscope onto the bracket, FIGURE 6.

Remove socket cap screws
FIGURE 6. SAC optical microscopy.
3. Remove the laser. Remove the laser system if this option is fitted.
4. All the cables to the ion gun are bakeable and do not need to be
removed before baking. It is not necessary to completely remove the
cables from the bake-out zone, FIGURE 7.

bakeable ion gun cables
FIGURE 7. Ion gun cabling.
5. The lens analyser and filter box cables are bakeable. The lens sup-
ply cables and the cables to the filter box may be left connected, FIGURE
8. and FIGURE 9.

The 4 bakeable lens supply cables
FIGURE 8. Lens supply cables.
Filter Box Cables

FIGURE 9. Filter box cables.
The cables do not need to be removed from the bake-out region.

6. The detector cable. The detector head cable is bakeable and does not
need removing for bake-out, FIGURE 10.
Bakeable detector cable
FIGURE 10. Detector cable.
7. Switch the stage control unit off and then disconnect the stage
cables.
8. Disconnect the iris and aperture drive cables. Disconnect the aper-
ture and iris drive cables and remove them from the bake-out zone.
9. Disconnect the entrance slit drive cable. Disconnect the entrance slit
drive cable, FIGURE 11.

Analyser entrance slit drive cable
FIGURE 11. Analyser entrance slit drive cable.
10. Place the fibre glass baking cover over the instrument. This cover
can cause skin irritation in some people so it is recommended that gloves
are used when handling the cover. Place the cover so that the turbo
pump remains outside the bake-out region, FIGURE 12.

FIGURE 12. Fitting the bake-out cover. The left picture shows how the cover should be arranged
around the turbo pump and post. The right picture shows how it should be fitted
around the autostage.
3.4.2 Baking the AXIS Ultra using Vision Software
Baking of the instrument is controlled from the vacuum control unit which is
used to set the correct state of the valves and pumping and control the time
of the baking and cool periods. A step-by-step sequence for baking the
instrument is defined below. The flap valve should be open during bake-out
and the instrument can be baked with the ion pump set to on or off.

1: At the rear of the instrument find the mains distribution panel and ensure
that the baking supply circuit breaker is switched to the on position as
shown in FIGURE 15.
FIGURE 13. circuit breakers on the mains distribution panel
2: The vacuum in the SAC and STC must be below 5E-05 torr before the
baking will start. The 5E-05 torr pressure represents the maximum pressure
interlock above which the bake sequence will not start. It is recommended
that a pressure in the E-06 torr range is attained before starting to bake the
instrument. Note that the baking will be switched off if the pressure rises
above 4E-05 torr during the bake cycle.
3: All the pressure gauges should be on and displaying a reading in the VCU
display.
4: From the Vision Manager window select mode > engineer. This will
cause the bake-out time off to be displayed at the bottom of the Vision Man-
ual window, as shown in FIGURE 14.
FIGURE 14. Bake out control from Vision Manual Window
5: The pull down menu options may be used to define the time at which the
bake out will be switched off. The maximum bake out time possible is 72
hours.
3.4.3 Baking the AXIS Ultra DLD using the VCU
Baking of the instrument is controlled from the vacuum control unit which is
used to set the correct state of the valves and pumping and control the time
of the baking and cool periods. A step-by-step sequence for baking the

instrument is defined below. The flap valve should be open during bake-out
and the instrument can be baked with the ion pump set to on or off.
1: At the rear of the instrument find the mains distribution panel and ensure
that the baking supply circuit breaker is switched to the on position as
shown in FIGURE 15.
FIGURE 15. circuit breakers on the mains distribution panel
2: The vacuum in the SAC and STC must be below 5E-05 torr before the
baking will start. The 5E-05 torr pressure represents the maximum pressure
interlock above which the bake sequence will not start. It is recommended
that a pressure in the E-06 torr range is attained before starting to bake the
instrument. Note that the baking will be switched off if the pressure rises
above 4E-05 torr during the bake cycle.
3: All the pressure gauges should be on and displaying a reading in the VCU
display.
4: Starting from the main menu shown in FIGURE 4. on the vacuum control
unit select the following sequences Auto > Baking. This will take the user to
the automatic sequence for baking with two options as shown in FIGURE
16.

SAC: 1E-06 STC : 3E-06 RP : 8E-03 2:52:27

-------------------- Automatic Sequence for Baking ---------------------
Back
Done
Start Set Bake Set Cool
FIGURE 16. Automatic sequence for baking display of VCU.
5: From this window, the total bake time (including cool time) can be set in
days: hours: minutes by selecting the Set Bake press-button. After setting
the bake time press the Back button to return to the menu shown above.
6: The total time that the system is allowed to cool after the heaters are
switched off and the ion pump is switched on is set by pressing the Set Cool
> press button and setting the time in the same manner as above for the
bake time. After setting the cool time press the Back button to return to the
menu shown above.
7: An example of typical settings would be a total bake time of 1 day and a

cool time of 12 hours. The bake out heaters would be on for 12 hours fol-
lowed by 12 hours of instrument cooling.
8: To start the bake press Start >. The VCU should display the Status OK
message on the LCD screen. Press the Start > button again to confirm
starting the bake out of the instrument. The VCU will open the flap valve
and the ion gun differential pumping valve (V2) if they are not already open.
The VCU will next check that the water flow is sufficient and then switch the
bake-out heaters on.
9: At the rear of the baking panel check that the red baking LED is illumi-
nated. Note that the baking sequence defined by the VCU will switch off the
all high voltage to the instrument, open the flap valve and the ion source dif-
ferential pumping prior to turning the heaters on.
The baking heaters should now start to heat the instrument and a rise in
pressure will most probably be observed. During the bake the only exposed
surface that gets hot enough to cause burns is the analyser on the top of the
instrument. Although it is unlikely that anyone should touch it during baking,
precautions should be taken to prevent or advise any personnel with access

to the instrument from coming into contact with this part of the spectrometer.
All other surfaces will remain at ambient operating temperature during the
baking period.
3.4.4 Failure to start baking

As mentioned above the pressure of the SAC & STC is monitored before
starting and during the baking. There are two common reasons which pre-
vent the starting of the bake out sequence. The first reason is that the
instrument pressure is above the set limit (5E-05 torr) when starting the bak-
ing sequence. In this case an error message will be reported in the VCU
display. The user should wait for the pressure to fall below the maximum
defined pressure and then follow the steps described in Section 3.4.3.
The baking sequence is also interlocked to the cooling water flow through
the instrument. The water flow is monitored as a signal from the crystal
backplane, turbo and magnet water flow sensor. If it is suspected that there
is insufficient water flow through the instrument then baking should not be
attempted without contacting a member of Kratos staff.
3.4.5 Degassing Filaments and Sources After Baking

To degas the X-ray source filaments go to the Manual window and scroll
down to the X-ray source section, FIGURE 17.
Degas Option
FIGURE 17. X-ray PSU.
Click on the degas button to open the degas parameters section, FIGURE
18.
FIGURE 18. X-ray filament degas parameters.
The degas option allows the user to slowly increase the current passing
through the selected filament in order to gently degas it. If the inside of the
vacuum chamber has been exposed to the atmosphere or the X-ray gun
hasnt been used for some time then the filament will be contaminated.
Ramping the filament current up in a controlled manner allows the filament

Venting the AXIS Ultra DLD to Atmosphere
to warm up gradually and contaminates are driven off slowly. This increases
the filament lifetime by reducing surface damage of the filament.
The ramp time is divided into two regimes so that the rate of increase can be
relatively fast until higher currents are reached and then a slower ramp rate
can be set for larger values, FIGURE 19.
Degas On / Off
Max current 1
Ramp time 1
Ramp time 2 Max current 2
FIGURE 19. Degas regime.
The ramp times and maximum currents can only be changed if the instru-
ment is in Engineer mode. Typical standard values for the mono source
are shown in FIGURE 19. Select each anode in turn to display the degas
ramp times for each filament. Typical values for the dual anode are: 1st
regime: ramp time 10 minutes, filament current 3 amps; 2nd regime: ramp
time 10 minutes, filament current 3.5 amps. If the X-ray source is off then
then the Degas on light will be yellow. Left clicking on the On light will start
the degas sequence. The progress can be followed by clicking on the Sta-
tus button which makes the filament current visible.
The Degas sequence can be halted at any time by left clicking on the off but-
ton. The ion gun filament should also be degassed, see Section 5.5.6, on
page 143.
3.5. Venting the AXIS Ultra DLD to Atmosphere

Before venting the system it is sensible to ensure that all samples have
been removed. The x-ray source must be turned off rather than stand-by
for at least 20 minutes before venting in order to allow the source to cool to
ambient temperatures after operation.
The vacuum control unit has a sequence of operations defined to vent the
entire system to dry nitrogen. To access this sequence on the vacuum con-
trol unit, starting from the main menu as shown in FIGURE 4. use the fol-
lowing sequence: auto > vent > start >. This will then start the automatic
vent sequence. In order to prevent over pressuring the spectrometer the
user should ensure that the screws are released on the sample entry cham-

Venting the AXIS Ultra DLD to Atmosphere
ber door. Once the system is vented this door will open and release the
pressure.
The system vent sequence followed by the software is as follows:

close the ion source pump valve V9
close the ion source gas inlet valve V8
turn off the ion pump and the high voltage
turn off the SAC and STC gauge
turn off the turbo pump
open the ion source differential pumping valve V2
close the baking valve V3
open the flap valve between the STC and SAC
open the vent valve V5 for 1 second
close the vent valve and wait 60 seconds, allowing the turbo to slow down
turn off the backing pirani gauge
open the vent valve
The VCU will wait for 10 minutes until it reports that the sequence is com-
plete. However, the instrument will remain with the vent valve open and the
system purging with dry nitrogen until the vent valve V5 is closed by the user
or the pump sequence is initiated.

13 July 2009
Chapter 4
Basic Operation
4.1. Introduction
This chapter is intended to introduce the user to the Vision 2 software and
aid in starting to acquire data and control spectrometer functions. As such
the chapter will focus on the manual operation of the instrument using the
Manual window. Following chapters will describe detailed operation of the
instruments various components, automated data collection and data
processing functions.
4.2. The Mouse
Vision 2 uses a three button mouse to control the various software func-
tions, FIGURE 1. The left hand mouse button is used to select objects or
rows so that parameters may be selected or text entered. The right hand
mouse button is used to open pop up menus when the mouse pointer is in
specific positions. The wheel, or middle mouse button can also be clicked.
This is used to paste objects.
63
Opening the Manager Software and Vision Zones
Left: Selects Middle: Pastes Right: Opens Menus
FIGURE 1. The mouse
4.3. Opening the Manager Software and Vision

Zones
To start the vision software double click on the Manager icon on the desktop.
This launches the Vision 2 Manager software. The Manager window will
appear together with a VME Initialisation window, FIGURE 2 and
FIGURE 3.
64 Chapter 4 Basic Operation

File Menu Edit Menu Mode Menu Window Menu View
FIGURE 2. Manager Window.
Chapter 4 Basic Operation 65

FIGURE 3. VME Initialisation window.
During the VME initialisation sequence the down load program is sent to the
instruments control processor and the instrument is configured. As part of
the configuration procedure the aperture and iris drives will be automatically
calibrated. However, the sample stage will not be moved.
Once the VME initialisation sequence is complete then the other Vision 2
windows associated with data acquisition can be opened following the pro-
cedure outlined below:
1. Left click on Window in the title bar. This opens up a menu, FIGURE 4.
FIGURE 4. Window menu.

2. The menu option are:

Manual window
Real-Time Display
Element List
Status Window
VME/Slave Messages
Host Messages
KRAM Debug
[VCU Engineers tool]-Engineer Mode only
Version Information
3. Left click on the Manual option, this will open the manual window. Note
that the manual window will only be displayed once the Vision Acquisition
software has been completely downloaded to the spectrometer.
4. Left click on the Vision Instrument icon in the windows bar at the bottom
of the screen to bring the Manager window back to the front.
5. Left click on Window in the title bar of the Manager window then click on
Real-Time Display to open the Real Time display window.
These windows now need to be arranged so that the desktop remains

uncluttered. Left click on the Windows Start menu, select Programs, Vision
then Zones. This will start the Zones software. The Zones should be
labelled Manager, Manual, Processing and Explorer.
Left click on Zones to open the Zones menu and click on Control to open the
zone control window, FIGURE 5.
FIGURE 5. Zone Control.

The Manual Window
The Zone names can be edited by double clicking on them in the Zone Con-
trol icon. Follow the instructions below to arrange the Vision windows:
1. Left click on the Instrument Manual Control icon in the control window.
2. While holding down the left mouse button drag the Instrument Manual
Control icon down to the Manual Zone and release. This should move
the Manual Window to the Manual Zone.
3. Follow the same procedure for the Real Time display window but this
time keep the control button pressed down while moving icon.
4. When the left mouse button is released the Real Time display button will
be copied to the Manual Zone.
The Instrument Manager window and the Real Time display window should
now be in the Manager Zone while the Instrument Manual control window
and a copy of the Real Time display window should be in the Manual Zone,
FIGURE 6. When configuration of the windows is complete click the close
button.
FIGURE 6. Re-arranged Zone Control
4.4. The Manual Window
This section will describe the major components of the Instrument Manual
window. Some sections such as the sample stage and the ion gun control
will be covered in their own chapters. The purpose of this section is to pro-
vide an overview of the controls available and description of how to access
the various options. Detailed operational instructions are given in the follow-
ing chapters.

The Manual Window
Select the Manual Zone icon to display the Manual window.
Slide bar
FIGURE 7. The Manual window.
To scroll up and down the window left click on the slide bar and move it in
the desired direction while holding down the left hand mouse button.
4.4.1 Entering values in boxes
Throughout the software it will be necessary for the user to input values into
specific boxes, whether it is to define the acquisition energy, or to enter
object names etc. Left click in the box to place the cursor in the box and

The Manual Window
type the text or number required. After the text or number has been typed
into the box a black rectangle appears adjacent to the text box, FIGURE 8.
Black bar appears

Text entered
FIGURE 8. Entering numbers or values
To input the value press return on the keyboard. The black rectangle will
now disappear. If return is not pressed the new value will not be recognised
by the software.
4.4.2 Modes of Operation
The mode is changed by left clicking on the Mode selection in the title bar of
the Manager window, FIGURE 9.
Mode Menu
FIGURE 9. Mode selection.
This opens the Mode menu, FIGURE 10.
FIGURE 10. Mode menu.
The three options are Engineer, Advanced and User. The instrument
defaults to Advanced mode. In this mode of operation critical instrument
parameters controlled from the Manual window are unavailable. This is a
safeguard against accidental changing of the instrument set up which may

The Manual Window
have serious consequences. Modes may be changed by left clicking on the

relevant mode in the menu, FIGURE 10.
4.4.3 Manual Window Selection
At the top of the Manual window are a number of toggle buttons,

FIGURE 11. These can be used to turn on or off the display for various sec-
tions in the Manual window. This option can be useful if you cannot find a
particular section in the Manual window. Simply turn off all the other sec-
tions.
Toggle switches
FIGURE 11. Manual window toggle buttons.
4.4.4 Optical Images
Immediately below the toggle buttons is the optical image section,

FIGURE 12.
Camera Selection
Record Image Image Name
FIGURE 12. Optical image section
This section controls the Ultra DLDs optical camera or cameras (if the
optional external microscope is fitted). The active camera is selected by left
clicking on the camera selection button, usually this will be set to camera 1.
The full scale deflection (FSD) is given in mm. This is 50% of the cameras
field of view and is dependent on the manual zoom level. It is usual to set 2
standard FSD values, one for when the camera is fully zoomed in and one
for when the camera is fully zoomed out. The relevant FSD for the current
zoom condition can then be selected by using the FSD selection control.
To store an image to a dataset follow the procedure outlined below:.
1: Activate the camera by pressing the view button. The optical image will
be shown in the real-time display window.

The Manual Window
2: An image can be stored in the computers memory by entering a name,

e.g. optical image in the name box and clicking on the grab image button,
FIGURE 12.
3: It is now necessary to define a dataset to save the stored image into.

Goto the vision manager window.
4: Drag open the bottom left hand corner of the manager window and select
acquiring, FIGURE 13.
Move this divider to

change size of
acquiring section
Save button
optical image object
Move this slider to right to

make acquiring section larger
FIGURE 13. Manger window
5: If the window you have made is large enough then the Save button
should be visible. Select the optical image object, which appears in the
acquiring window as a grey rectangular block, by clicking on it with the left
hand mouse button. It should change from grey to black. Then click on the
save button. A dialogue box opens which allows the user to specify a data-
set name and directory for the image, FIGURE 14. This can be an existing
or a new dataset.

The Manual Window
FIGURE 14. Save selection
6: Alternatively the dataset can be specified before the image is grabbed.

The advantage of opening a dataset in this manner is that all subsequent
objects saved to the memory will be written to this dataset until a different
dataset is specified by the user.
7: Drag open the bottom left hand corner of the manager window and select
acquiring.
8: Position the mouse pointer in the acquiring window and press the right
mouse button.
9: A drop down menu opens, select the Open dataset option, FIGURE 15.
FIGURE 15. Open dataset pull down menu
10: A dialogue box then opens, enter a new dataset name or select an exist-
ing dataset, Figure 14. The opened dataset name appears in the left hand

The Manual Window
top corner of the acquiring section (N.B. the actual name may appear trun-
cated depending on the relative size of the sections).
11: The optical image can now be grabbed in the usual way, the image
being automatically saved into the opened dataset.
Once an optical image of the sample has been stored the SEC camera can
be switched off by clicking on the off button, FIGURE 12.
4.4.5 Analyser Control and Parallel XPS Imaging
The next two sections provide manual control of the lens mode of the spec-
trometer and allow a real time parallel photoelectron image of the sample
surface to be displayed, FIGURE 16. Images can be intergrated and saved,
for instructions on saving images and recording them to a dataset see
Section 4.4.4 on page 71.
FIGURE 16. Parallel XPS Imaging and Analyser section.
The Analyser section is used to manually specify the current analyser state.
4.4.5.1 Analyser Mode
Left click on the analyser mode button to open a pop up menu, FIGURE 17.
FIGURE 17. Analyser mode menu

The Manual Window
This option defines the mode of operation of the analyser. When Spectrum
is selected the hemispherical analyser (HSA) is used to filter the electron
energy reaching the detector. An entrance slit (not to be confused with the
slot in the aperture drive) is automatically placed at the entrance to the ana-
lyser to limit the angular acceptance of the HSA thereby improving the
energy resolution. This is transparent to the user.
If Imaging is selected the voltage supplies are modified and photoelectrons

pass through the HSA and enter the spherical mirror analyser (SMA). This
analyser is used for parallel photoelectron imaging of the sample. The slit
used at the entrance to the analyser in spectrum mode is automatically
moved to allow more photoelectrons to enter the analyser. See chapter 3
for further information.
4.4.5.2 Lens Mode
Select the Lens mode button to open the lens mode menu shown in
FIGURE 18. This controls the lens configuration of the instrument.
FIGURE 18. Lens mode menu.
The lens modes available will depended upon the exact configuration of the
instrument. The mode chosen depends on the analysis to be performed.
Hybrid - this mode is used by the Ultra DLD for general spectroscopy
including survey spectra and high resolution narrow scans. It should
always be used in conjunction with the slot aperture (see below) and
never during imaging or small spot spectroscopy. The area of analysis is
approx. 700 microns x 300 microns when used with the slot aperture.
Magnetic - the Ultra DLD does not use this lens mode and it may not be
included in the list.
Electrostatic - this mode allows spectra to be recorded without the use of
the magnetic lens. It is only suitable in situations where use of the mag-
netic lens is inadvisable, e.g. when the sample is very magnetic. In this
mode the acceptance area of the analyser is very large (up to 15 mm)
therefore the analysis area will be defined by the X-ray source used.
Field of View 1: Survey - this mode is used by the Ultra DLD for large
area parallel XPS imaging. The field of view (FOV) for imaging will be

The Manual Window
approximately 800 x 800 microns., with the exact FOV defined for each
individual instrument.
Field of View 2: Small Spot - this mode is used for small spot spectros-
copy. Use in combination with the small spot apertures to change the
analysed area on the sample. It is also used for parallel XPS imaging.
The field of view in imaging mode is typically 400 x 400 microns.
Field of View 3: This mode is only used for the highest magnification par-
allel XPS imaging. The field of view is typically 200 x 200 microns.
Field of View 4: This mode is often set up for electrostatic parallel imag-
ing of the sample. It is a mode used for a specific engineering application
and should not be used for general spectroscopy and imaging.
4.4.5.3 Resolution
Left click on the pass energy button to open the pass energy menu,
FIGURE 19.
FIGURE 19. Pass energy menu.
The pass energy determines the energy resolution of the analyser in both
spectroscopy mode and imaging mode. Higher pass energies reduce the
energy resolution but increase sensitivity. For general large area spectros-
copy use 160 eV pass energy for survey spectrum and 20 or 40 eV pass
energy for core level spectra. For ultimate energy resolution 10 eV or even
5 eV pass energy can be used but acquisition times will need to be
increased to account for the reduced sensitivity.
In imaging mode 160 eV pass energy is the norm. For chemical resolution
the pass energy is reduced but acquisition times will increase as a conse-
quence.
4.4.5.4 Area of Analysis
Left click on this button to open the area of analysis menu, FIGURE 20.

The Manual Window
FIGURE 20. Area of analysis.
This controls the analysis area on the surface of the sample by altering the
aperture and iris positions, see Chapter 3.
Slot - when selected the aperture drive moves to the slot position and the
iris is opened fully. This option should be used in conjunction with hybrid
mode for general spectroscopy. It gives an analysis area of approxi-
mately 700 x 300 microns on the sample surface.
110 um - when selected a 2 mm aperture is driven into the lens column
and the iris may be closed slightly. This gives a 110 um analysis area on
the sample when it is used in conjunction with the FOV 2 lens mode for
small spot spectroscopy. If FOV 1 is selected the analysis area will be
approximately 220 microns.
55 um - when selected a 1 mm aperture is driven into the lens column
and the iris is closed slightly. This gives a 55 um analysis area on the
sample when it is used in conjunction with the F.O.V.2 lens mode for
small spot spectroscopy.
27 um - when selected the 0.5 mm aperture is driven into the lens col-
umn and the iris is closed more. This gives a 27 um analysis area on the
15 um - when selected the 0.2 mm aperture is driven into the lens col-
umn and the iris is closed more. This gives a 15 um analysis area on the
imaging selection - the remaining three modes are intended for use dur-
ing parallel XPS imaging. When selected the imaging aperture is driven
into position. These modes can be used with any lens mode to vary the
field of view (the field of view is determined by the lens mode). The differ-
ent selections, imaging dia9mm, dia5mm and dia3mm (they may also be
labelled low, medium and high resolution) refer to the position of the iris.
The smaller the iris setting the better the lateral image resolution but the
lower the image intensity. In practice the dia9mm or dia5mm settings are

The Manual Window
used in conjunction with F.O.V.1 and the dia3mm setting is used when
imaging in F.O.V.2 or F.O.V.3 lens modes.
4.4.5.5 Analyser State
These bulbs show the state of the analyser. Green indicates that the ana-
lyser and detector are in the stand-by state. Grey indicates that the analyser
and detector are on. The analyser and detector should be switched to
stand-by when not in use. This will increase the life of the detector and
decrease the chance of accidental damage to the detector or analyser. A
convenient way to switch the analyser and detector to stand-by is to click
the Parallel XPS Imaging Off button, FIGURE 16. This switches the detec-
tor and analyser to stand-by regardless of whether the instrument is running
in the imaging or spectroscopic modes.
4.4.5.6 XPS Parallel Imaging On and Off
These buttons switch the parallel XPS imaging On or Off. When the On but-
ton is left clicked the analyser is set to the energy specified in the energy
box, Section 4.4.5.8 on page 79, and the detector is switched on. The par-
allel XPS image will appear in the bottom left hand side of the real time dis-
play window. When the Off button is left clicked on the analyser and
detector are switched off.
4.4.5.7 Integration Mode
This control selects the method of image integration used during parallel
XPS imaging of a sample. Left click on the button to bring up the menu,
FIGURE 21.
FIGURE 21. Integration mode
Running integral is used to view a parallel XPS image of the sample

surface in real time. It is particularly useful for positioning the sample and
looking for areas of interest which may be optically invisible. When run-
ning integral is selected the integration time determines the length of time
than images are added together for.
Single integration is used to manually record an image of the sample
surface. The image is collected for the time specified in seconds in the
integration time box. After the time has elapsed imaging of the sample

The Manual Window
will cease allowing the image to be saved to the dataset. The image
object is not saved to the dataset until the grab image button is pressed.
4.4.5.8 Energy
The energy box allows either a binding energy or a kinetic energy for the
SMA to be entered (always press return after entering a value). The energy
reference should be changed to reflect the chosen X-ray anode. The
energy value is the energy of photoelectrons which the SMA will transmit to
the detector. The spread of energies which actually pass through the ana-
lyser are determined by the pass energy. At 160 eV the energy window
transmitted will be approximately 4 eV wide.
4.4.5.9 Grab Image
The image can be stored by entering an object name in the image object
box and left clicking on the Grab button. This writes an object to the acquir-
ing section of the manager window. For instructions on how to permanently
save the image see Section 4.4.4 on page 71.
4.4.6 Acquisition Control
The acquisition control section allows the user to record manual spectra,
snapshots, line scans or scanned images and is shown in FIGURE 22. See
chapter 7 for a full description on how to automatically record spectra and
images.
FIGURE 22. Acquisition control.
Left click on the scan Type button to open the type menu, FIGURE 23. This
allows the user to manually set the type of acquisition.

The Manual Window
FIGURE 23. Scan type menu.
4.4.6.1 Spectrum
Left click on Spectrum to record spectra. Select the energy regions table
button to show the expanded acquisition section including the energy region
table. The energy scale can be either in binding or kinetic energy. The
energy reference automatically changed according to the X-ray anode
selected. Left click on the energy regions box to open the energy row table,
FIGURE 24.
select energy regions table

button to expand
FIGURE 24. Region table.
To enter a scan for acquisition type in the core level name into the Region
name box and press return, FIGURE 25. The syntax must be correct as the
software is case sensitive. If a mistake is made then click on the delete row
button and start again.

The Manual Window
FIGURE 25. Entering a region row.
Standard parameters for the selected core level scan are automatically
entered into the region row. These can be edited as required by left clicking
in the relevant box and entering a new value (dont forget to press return).
The scan limits (start and end) can be displayed by right mouse clicking on
the Centre text, and selecting start from the pop up menu, FIGURE 26.
FIGURE 26. Centre or start menu
Similarly the dwell time can be changed to total sweep time by right mouse
clicking on the dwell text and clicking on sweep s.
A custom region can also be defined by simply entering all the parameters
manually. When the On button is pressed all the Active scans will be
started in descending order. To select or deselect a scan click on or off the
active button, FIGURE 24.
For scanned spectroscopy the analyser must be set to spectrum and not
imaging. Use a combination of the lens mode and aperture setting to deter-
mine the analysed area, see Section 4.4.5 on page 74. When performing
small spot spectroscopy the analysis position on the surface of the sample
can be defined as described in Section 7.3.5 on page 223.
In the manual mode the active spectrum will be recorded continuously in a

continuous loop when the On button is pressed. At the end of each scan the
spectrometer will automatically go back to the start and begin the scan
again. The scan will be displayed in the right hand side of the real time dis-
play window. No data will be saved to the Manager acquisition window at
this stage. To save a scan click off while the scan is in progress. The off
light will flash and the spectrometer will stop scanning when the end of the
scan is reached. A scan object is automatically written to the dataset that is
currently open in the acquisition section of the Manager window. To Restart
the scan click the restart button, the spectrometer will begin the scan from
the start of the spectrum.
To stop the scan without saving the spectrum click on the Off button. While
it is flashing click on the Restart button.

The Manual Window
4.4.6.2 Map
In the manual mode choose Map to record a scanned map of the sample
surface. Such a map is usually only recorded during instrument set up or
alignment as parallel XPS imaging has superseded this option.
4.4.6.3 Line Scan
Line scans are again normally only used during instrument set up or align-
ment.
4.4.6.4 Snapshot
If snapshot is selected then the width column and step size column of the
energy region table will be greyed out, FIGURE 27. and it is not possible to
edit these columns.
FIGURE 27. Snapshot parameters
A snapshot spectrum is recorded without scanning the photoelectron

energy, therefore, width and step size are now not applicable. The HSA is
set at the energy defined in the Centre box and the spectrum width is sim-
ply determined by the pass energy used. The actual width of the spectrum
is approximately 10% of the pass energy, i.e. 16 eV at a pass energy of 160
eV. Hence as there are approximately 100 counting channels in spectrum
mode the step size at 160 eV pass energy would be approximately 0.16 eV.
A typical snap shot would be recorded in Spectrum mode using Hybrid

(large area analysis) or F.O.V.2 with a pass energy of 160 eV for small spot
snap shots. The dwell time should be greater than 2000 ms.

The Manual Window
4.4.7 X-ray PSU
The X-ray power supply unit (PSU) section allows manual control of the X-
ray source, FIGURE 28.
Selected anode Emission current selected Current Read back

Anode HT Selected Voltage Read back
FIGURE 28. X-ray PSU control.
4.4.7.1 Selecting X-ray Source
Left click on the Anode to select the X-ray anode, FIGURE 29.
Mg non-monochromated Source
Al non-monochromated Source
Al monochromated Source
FIGURE 29. X-ray Anode Selection
When the non-monochromated dual anode is selected, i.e. either Al or Mg,

the dual anode gun must be manually moved into position, FIGURE 30.

The Manual Window
Tilt Adjustment
Linear Drive
FIGURE 30. Dual Anode Bellows
The dual anode bellows is on a ratchet mechanism which can be moved in

and out of the chamber. Position the sample using the optical camera and
move the dual anode inwards until it is approx. 10 mm away from the sam-
ple. N.B. the dual anode may be moved closer but care must be taken to
avoid moving the sample holder into the Al foil window. The tilt mechanism
can then be used to select the anode. The Al coating is on the bottom face
of the anode while the Mg coating is on the upper face. Tilt the dual anode
body to maximise the signal from the chosen face.
N.B. Significant damage to the dual anode assembly and the X-ray
power supply unit can be caused by collision between the dual anode
and the sample holder / sample stage. Take care when moving the
sample stage while the dual anode is wound into the chamber and
always fully retract the dual anode before changing sample holders or
calibrating the sample stage.
N.B. Tiliting the dual anode too high can cause it to touch the charge
balance plate at the end of the lens column. If this occurs the charge
neutraliser will not function correctly. Furthermore damage may occur
to either the dual anode or the end of the lens column.

The Manual Window
4.4.7.2 Switching the X-rays to stand-by
Enter the required emission current in the Emission box and the accelera-
tion voltage into the Acceleration HT box. Values between 0 and 15 kV may
be entered but 15 kV is the usual setting. Left click on the Stand-by button.
This switches the X-ray source to stand-by after a short delay. In standby
mode the filament current is ramped up to a low stand-by value (approxi-
mately 1 A) and the high voltage is removed from the anode.
Note that when selecting the X-ray power (emission current and anode volt-
age) consideration should be made to the X-ray power density at the sample
which may cause degradation of delicate samples, and the photoelectron
signal observed by the detector. Excessively high count rates acquired for
prolonged periods will lead to a shortened detector lifetime.
4.4.7.3 Switching the X-ray Source On
After the X-ray source has reached the Stand-by state click on the On but-
ton. After a short delay the high voltage will be applied to the anode and the
filament current will be slowly increased. The filament current is controlled
by a negative feedback loop with the emission current. The current rises
until the requested emission current or the filament current limit is reached.
To monitor the filament current click on the status button, FIGURE 31.
Status
FIGURE 31. X-ray status.
The grey boxes read-back the actual values applied to the X-ray source.
4.4.7.4 Switching the X-ray Source Off
To switch the X-ray off click the off button. The X-rays may be switched off
from the stand-by state or the on state. The filament will be switched off and
the high voltage will be set to zero.
4.4.7.5 X-ray Parameters
Left click on the parameters box to open the X-ray parameters section,
FIGURE 32. The filament current limit can be increased if the requested

The Manual Window
emission is not reached. N.B. check that the Acceleration Voltage read
back is correct. Do not increase the filament current limit above 5 amps
without contacting a Kratos engineer.
The water flow rate limit is the value that the water flow through the anode
must exceed before the X-rays can be operated. Do not adjust this value
as a low water flow rate can cause extensive damage to the X-ray
source and possibly the vacuum system.
FIGURE 32. X-ray parameters.
4.4.7.6 Leakage Current
If the instrument cooling water becomes too conducting then electric current
will leak from the X-ray anode at high voltage to other metal parts that the
water comes into contact with. This can cause severe damage to the water
system and / or X-ray anode. If a significant leakage current is present then
a red warning light will illuminate. FIGURE 33. shows the leakage current
indicator in the normal mode.
FIGURE 33. Leakage current warning light.
The software continuously monitors the leakage current when the high volt-
age is applied to the anodes. By selecting the parameters tick-box in the
X-ray user interface the parameters associated with the water deionisation
can be edited. The user has control over the leakage current trip high/low-
values. These parameters define the points at which the leakage current fail
lamp is illuminated which in turn activates the solenoid valve to bypass
water through the deionisation cartridge. If the solenoid valve is opened due
to leakage current outside the defined values it will remain open and water
will flow through the deioniser cartridge for the time specified in the user
defined water deionise delay dialogue box.

The Manual Window
FIGURE 34. User controlled parameters for water deionisation.
A further indication of leakage current is a difference between the Anode

current and the Emission current, FIGURE 31.
In order to reduce the conductivity of the water supply the instrument is fitted
with a de-ioniser cartridge which is situated under the decking of the spec-
trometer. When the cartridge is spent the leakage current will increase. If
the warning light turns on for more than a brief period then check the car-
tridge, see FIGURE 35.
Grey colour - de-ioniser spent
Bright blue colour - de-ioniser OK

The Manual Window
FIGURE 35. De-ioniser cartridge.
4.4.8 The Charge Neutraliser
The control buttons allow the charge neutraliser to be switched on or off,

FIGURE 36. See chapter 3 for details of the neutraliser operation.
FIGURE 36. Charge neutraliser.
Click the On button to switch the neutraliser On and the Off button to
switch the neutraliser Off. The optimum neutraliser parameters are deter-
mined during instrument set up. These settings should provide adequate
neutralisation for a wide range of insulating samples. However, on rare
occasions it may be necessary to modify the neutraliser settings. To access
these settings click on the parameters button, FIGURE 37.
FIGURE 37. Charge neutraliser settings.
From experience the following guide lines are given for the adjustment of
neutraliser parameters.
Filament Current should be set between 1.6 and 2.1 amps.
Charge balance should be set between 2 and 3.6 volts.
Filament bias should be set between 1 and 2 volts.
Click on Restore Default Settings to revert back to the previously stored

neutraliser values. If engineering mode is selected then the current neutral-
iser settings can saved as the default, over-writing the stored values, by
clicking on the Save default settings.

Sample Mounting Techniques
Trim Coil 1 should not be adjusted under any circumstances. Trim

Coils 2 and 3 are not used.
4.5. Sample Mounting Techniques
Samples can be mounted on a number of different sample holders. These

holders are loaded into the sample treatment chamber (STC). Choice of
sample holder depends on the type of sample to be loaded and the experi-
ments to be performed. Once the STC has been pumped down the sample
holders are then transferred to the sample analysis chamber (SAC) and
loaded onto the autostage. After the sample holder has been loaded onto
the autostage then all sample movements are automatically controlled
allowing unattended multi-sample analysis.
A comprehensive discussion of sample handling and mounting techniques
is beyond the scope of this manual, however, it is appropriate to make some
general points here. For a more in depth review see ASTM ref.
4.5.1 General Requirements
In general the degree of sample cleanliness required for surface analysis is

much greater then other analytical techniques. The material under investi-
gation must be stable in an ultra high vacuum environment. Many materials
may desorb volatile surface species, e.g. water vapour and plasticisers
which may contaminate other samples. Other materials may have high
vapour pressures such as polymers, foams and porous materials. Some
elements such as Na, K, S, P, Zn, Se, As, I, Te and Hg also have relatively
high vapour pressures.
When analysing such materials it is advisable to reduce the size of the sam-
ple to a minimum if practical and bare in mind the possible effects of cross
contamination of other samples. Pumping the samples overnight in the STC
may also be advisable, however, the out-gassing of volatile materials can be
greatly increased when the sample is subject to X-ray bombardment and/or
exposure to the charge neutraliser. In extreme cases such samples can
contaminate the vacuum chamber and charge neutraliser elements.
4.5.2 Sample Handling and Storage
Samples, sample bars and sample stubs should never be touched with
unprotected hands. Even if the surface to be analysed is not touched, low
molecular weight oils present on the skin can rapidly migrate over the area
of interest. Na contamination is often detected on handled materials. It is
essential to wear powder free gloves when handling and preparing samples.
Tools should be clean and made of materials which will not transfer contam-
inates to the samples. All tools should be demagnetised.
Great care should be taken when cleaning samples prior to analysis. As a

general rule cleaning should be keep to a minimum and avoided if possible.
Ultrasonic cleaning in a suitable high purity solvent (e.g. isopropyl alcohol) is

sometimes permitted. Removal of surface particles using compressed air

should be avoided as oil and/or water contaminates are often introduced.
When storing samples the surface of interest should not come into contact
with any material. If this is unavoidable then wrapping the sample in clean
Al foil may be satisfactory. Glass jars are often preferable to plastic contain-
ers due to the risk of volatile plasticisers and/or low molecular weight materi-
als from polymers contaminating the sample surface.
4.5.3 Sample Stubs
The AXIS Ultra DLD is supplied with standard 15mm diameter stubs,
together with spring clips, FIGURE 38. This is a versatile method for sample
mounting and is generally applicable to most thin flat samples. The stubs
can also be modified by the customer to accommodate unusual sample
geometers, including holes and tapped screw holes. It is important that the
upper and lower rings used for sample transfer are kept free of obstructions.
Shallow holes may also be drilled in the top of the stubs for mounting pow-
ders.
Although clips are the preferred sample mounting method for stubs is it is
also admissible to use small amounts of double sided vacuum compatible
adhesive tape. Conductive carbon tapes are recommended (e.g. Carbon
conductive adhesive tape available from www.agar.com, part number
G3939) but it must be borne in mind that such tapes often contain mobile sil-
icate compounds which may contaminate the sample to be analysed.
Hence it is not appropriate to use carbon tape for long term fixture of sam-
ples. All traces of carbon tape must be removed from the vacuum system
prior to baking the instrument.
The maximum sample width is determined by the sample introduction sys-

tem, which will typically allow samples of 100 mm wide. The recommended
maximum width for use with stubs is 25mm diameter. The maximum sample
height is determined by the physical presence of the magnetic lens mounted
beneath the sample and a maximum thickness of 4mm on standard stubs
can be analysed. The maximum sample length is determined by the spacing
of the claws and supports on the introduction probe and XYZ manipulator.
A maximum length of about 40mm is recommended with stubs but longer
samples can be accommodated using sample bars. Care should always be
exercised with samples which extend beyond the diameter of the stub. In
particular the aluminium window on the dual anode X-ray gun is fragile and
will easily break if touched with an overhanging sample.

FIGURE 38. Standard sample stub.
Bulk powders are best mounted by pressing onto tape, and shaking to
remove loose material. Care should be exercised when pumping from
atmosphere and when starting pump down of the STC. The turbo molecular
pump is particularly vulnerable to damage by fine grained powders at this
stage. Although the pump is protected by a splinter shield which will catch
large sample fragments, fine powders can pass through and cause harm
either to the turbine blades (over a period of time) or possibly to the bear-
ings. It is possible to mount coarse grained powders and pellets (e.g. cata-
lyst fragments) on a stub with a rim, FIGURE 39. Care should be taken at
all times when handling such an arrangement.
FIGURE 39. Powder mounting stub.
Conductive silver paint or colloidal graphite may also be used to secure

samples to the sample stub. However, this method is not generally recom-
mended because of extended out gassing of the solvent. If used then the
following precautions should be observed: do not use with large or heavy
samples - the paint has poor adhesive strength; allow the paint to dry before
introduction into the vacuum system; and allow a longer pumping time (up to
20 minutes) in the sample introduction chamber.

4.5.4 Mounting on Sample Bars
The AXIS Ultra is supplied with a number of sample bars for large or multi-
ple sample mounting, FIGURE 40. In practice the user will usually find
mounting samples on bars more convenient than sample stubs as many
more samples can be accommodated at one time. Efficient utilisation of the
sample bar and autostage maximises sample throughput. However, care
must be taken when mounting samples which are likely to present a particu-
larly large out-gassing problem. Limiting the number and size of such sam-
ples on the sample bar is recommended. If large amounts of such samples
are introduced into the spectrometer at one time then unacceptably long
pump down times and / or performance degrading contamination of fila-
ments and other surfaces in the vacuum chamber may occur.
Constant height bar tool
Plane sample bar
Sample mounting clips
Constant height bar
FIGURE 40. Bars and tools supplied.
The standard sample bar has a flat surface 130 x 15 mm. Samples up to 4
mm thick may be secured on the standard bar using the sample mounting
clips or double sided, conductive adhesive tape. The maximum sample size
which can be mounted is 130 mm x 100 mm x 4 mm. Great care not to
damage the dual anode X-ray source must be taken when the sample
overhangs the bar.
The constant height bar incorporates four spring loaded disks which can
hold samples of various thicknesses, FIGURE 41. The design of the disks
ensure that the top surface of all samples mounted are at the same height

Sample Insertion
thus simplifying experimental setup. Hold down the disks with the tool sup-
plied and slip samples between the disk and the sample bar. When the disk
is released the sample should be held firmly between the sprung disk and
the top surface of the sample bar.
Samples thicker the 4 mm may be analysed by removing one or more of the

spring loaded disc.
FIGURE 41. Constant height bar.
4.6. Sample Insertion
The method for sample introduction differs depending on the exact configu-
ration of the instrument and the method of sample mounting. Therefore, the
sample insertion section is subdivided into different sections depending on
the configuration of the Sample Treatment Chamber (STC).
4.6.1 Standard or Long STC
The standard or long STC, FIGURE 42, consists of a turbomolecular

pumped chamber attached directly to the SAC via a mechanically operated
flap valve, see Section 2.1, on page 21. A long sample transfer probe is
fitted to a hinged door on the STC.

Sample Insertion
Standard STC
SAC
Transfer Probe
Sample Magazine
FIGURE 42. Standard STC.
4.6.1.1 Loading a Sample Stub
To load a sample stub follow the procedure outlined below:

1. Mount the stub on the loading tool. The lower ridge on the sample stub
should be mounted in the tool, i.e. top slot on insertion probe.
2. Vent the STC as described in Section 3.1.6.1 on page 45. When the
chamber reaches atmospheric pressure the door will open if the securing
screws are released, FIGURE 43.
3. Open the door fully and introduce the sample stub. The claw on the
introduction probe will engage with the upper ridge on the sample stub,
FIGURE 44 and FIGURE 45. Ensure the stub is pushed completely into
the claw.
4. Close the door and tighten the door retaining screws.
5. Pump the STC as described in Section 3.1.6.2 on page 45. The turbo
should then be allowed to pump the STC. The exact time required to
reach a suitable pressure will depend on the sample. Clean samples
(metals, some polymers etc.) held with clips and introduced with a posi-
tive pressure of venting gas may be ready for introduction into the analy-
sis chamber in 5-10minutes. Large volumes of out gassing materials such
as catalyst pellets, may take much longer.
6. The active pressure gauge in the STC will automatically switch on after a
pre-set time delay. This may be used to monitor the pressure. A recom-
mended pressure of 5 x 10-7 torr should be achieved before the sample
can be safely introduced into the analysis chamber. If a higher pressure is
observed which does not rapidly fall, then a longer pumping time may be

Sample Insertion
required. Longer pump down times are rewarded by a generally cleaner

analysis chamber and reduced requirement for baking the instrument.
7. After an adequate pumping time, the sample can be introduced into the
analysis chamber (see below).
Probe door securing screws
FIGURE 43. Probe Door.
FIGURE 44. Stub insertion procedure.

Sample Insertion
Top slot on probe
FIGURE 45. Stub insertion procedure.
4.6.1.2 Loading a Sample Bar
Loading a sample bar is essentially identical to loading a sample stub. How-

ever loading the sample bar onto the transfer probe is subtly different. One
end of the bar has two cylinders and the other end has one. The two cylin-
der end is designed to locate onto the sample stage in the SAC and the one
cylinder end is designed to mount on the transfer probe, FIGURE 46.
Insertion probe end SAC stage end
FIGURE 46. Sample bar.
Mount the bar onto the transfer probe, FIGURE 47.

Sample Insertion
One cylinder end
FIGURE 47. Loading the sample bar onto the transfer probe.
Once the bar is loaded follow Section 4.6.1.1 on page 94 from point 4 to
pump the sample bar down in the STC.
4.6.2 Loading Samples on to the Sample Magazine WX-489
If the sample magazine is fitted sample bars and stubs can be loaded
directly onto the sample magazine. This magazine is used to store samples
in the STC under UHV and it also enables samples in the SAC to be
changed without venting the STC, see below.
To load sample stubs directly onto the sample magazine follow the instruc-
tions outline below:
1. Vent the STC and fully open the hinged door.
2. Use the stub insertion tool, FIGURE 48, to place the sample stub on one
of the magazine stub holders. There are 5 stub holders evenly spaced on
the left hand side of the sample magazine.
3. Ensure that the stub is placed such that the bottom slot of the stub is in
the magazine and the insertion tool is inserted in the top stub slot.
4. Close and pump the STC.

Sample Insertion
Stub insertion tool located in top stub slot
Magazine stub holder
Bottom stub slot placed on magazine stub holder
FIGURE 48. Stub insertion tool.
To load sample bars directly onto the sample magazine follow the instruc-
tions outlined below:
1. Vent the STC and fully open the hinged door.
2. Push the sample bar onto one of the sample bar holders folks situated
on the right hand side of the magazine, FIGURE 49. The 2 cylinder end
of the bar should locate in the folk.
3. Ensure that the magazine folks locate in the bottom slots of the sample
bar.
4. Close and pump the STC.
N.B. Although both sample bars and stubs may be stored on the sam-
ple magazine at the same time it is not possible to load sample stubs,
from the magazine, into the spectrometer if a bar is mounted.

Sample Insertion With Fast Entry Lock WX-523
Bottom slot of sample bar pushed on magazine bar holder
Sample magazine bar holder
Bar 2 cylinder end pushed onto holder
FIGURE 49. Sample bar inserted onto sample magazine folk.
4.7. Sample Insertion With Fast Entry Lock WX-523
If the instrument is fitted with the fast entry lock (WX-523) then samples are
inserted into the fast entry lock which is pumped down by an additional
pumping station prior to introduction to the STC. The fast entry lock enables
the user to constantly maintain the STC under UHV conditions. Cooling
devices are also often supplied with the fast entry lock to allow the user to
introduce pre-cooled samples into the spectrometer. The operation of heat
and cool accessories is described in separate manuals supplied with the
accessory.
4.7.0.1 Loading a sample stub into the fast entry lock
Follow the instructions given below to load a sample onto the transfer probe
attached to the fast entry lock:
N.B. The gate valve between the STC and fast entry lock in manually
controlled. There are no safety interlocks associated with this valve.
Therefore it is imperative that the user exercises caution when operat-
ing the fast entry lock. The main risks are: venting the STC and possi-
bly the SAC via the fast entry lock by inadvertently leaving the gate
valve open when venting the fast entry lock; and closing the gate valve
on the transfer probe. These risks can be minimised by careful han-
dling and a safety conscious routine such as outlined below.

1. Check that the transfer probe is full retracted - a green light should be
visible on the probe sensor at the end of the transfer probe tube,
FIGURE 50.
Red light - Probe may be in gate valve!
Green light - safe to proceed
FIGURE 50. Probe sensor.
2. When the sensor light is green check that the gate valve is fully closed,
i.e. fully clockwise,FIGURE 51.
3. To vent the fast entry lock check that the gate valve is fully closed and
turn off the fast entry locks pumping station by simply pressing the on /
off button (see separate user manual supplied with the pumping station
for details).
Turning off the pumping station will automatically switch the pressure gauge
off, stop the turbomolecular pump and backing pump and safely vent the
fast entry lock to dry nitrogen.
4. At this stage unscrew the securing nut on the stub insertion port or undo
the security clips (FIGURE 51) to avoid over pressure in the fast entry
lock.

Fast entry lock / STC manual gate valve
Pre-cooler accessory
Fast entry lock
Security clips
Transfer probe
Stub insertion port
Transfer probe linear drive
FIGURE 51. Fast entry lock

5. Once the fast entry lock has reached atmospheric pressure fully open
the stub entry port, FIGURE 52.

Top view port
Stub entry port
FIGURE 52. Fast entry lock stub insertion port.
6. Wind in the transfer probe so it is visible through the top view port,
FIGURE 52.
7. Use the black stub loading tool to place the top slot of the sample stub
on the transfer probe, FIGURE 53.
Transfer probe
Sample stub
FIGURE 53. Loading sample stub via stub insertion port.

8. Once the stub is loaded close the stub insertion port, tighten the nut and
immediately switch the pumping station back on.
4.7.0.2 Loading a sample bar into the fast entry lock
The method for loading sample bars into the fast entry lock is similar to the
insertion of sample stubs. Follow the procedure outlined in Section 4.7.0.1
on page 99 to point number 4, paying particular attention to the safety pre-
cautions, then follow the method described below:
1. Follow points 1 to 4 in Section 4.7.0.1 on page 99.
2. This time open the securing clips and not the stub insertion port,
FIGURE 51.
3. Once the fast entry lock has vented to dry nitrogen slide back the trans-
fer probe assembly, FIGURE 54.
Transfer probe assembly
Transfer probe claw
Viton seal
Security clips
Fast entry lock
FIGURE 54. Fast entry lock transfer probe assembly.
4. Place the one cylinder end on the sample bar on the transfer probe claw,
FIGURE 55.
5. Push the transfer probe assembly back up to the fast entry lock and fas-
ten the security clips.
6. Start the pumping station immediately.

Operation of the Autostage
Slot bar onto transfer probe claw
FIGURE 55. Loading sample bar into fast entry lock.
4.8. Operation of the Autostage
This section describes general operation of the autostage accessory and

the transfer of samples from the STC to the SAC for analysis.
The Automatic Sample Handling System is designed to simplify and stand-

ardise sample manipulation procedures for the Ultra DLD. It is intended
principally to provide the basis for unattended long duration repetitive analy-
ses. The system has, however, great flexibility in both control and applica-
tion which can aid and extend one off, research style investigations and
improve and accelerate normal operation.
The system includes a high precision computer driven XYZ manipulator

(often termed the stage), FIGURE 56. Stepper motor drives coupled to
precision leadscrews provide accurate routine position repeatability.
Maximum translation of the stage is 130mm in x (the major, sample chang-

ing axis) and 7.5mm in the orthogonal y and z axes. High precision auto-
mated tilt (90o) is incorporated as standard. High temperature (+600oC)
sample heating and sample cooling (-100oC) is available as an option.

Vacuum bellows
Autostage fork
Stepper motors
FIGURE 56. The autostage.
4.8.1 Calibrating the Autostage
A set of four lights at the top of the manipulator section display the current
status of the stage, FIGURE 57: Halt; Manual; Initalised; and Calibrated. A
green light indicates that the stage is either halted, in manual mode, inital-
ised or calibrated. Automatic movements are not possible if the stage is
uncalibrated. Similarly the stage cannot be moved manually unless the
manual mode is selected. The maximum deflection of the autostage is pro-
tected by software limits and mechanical hardware limits. The software lim-
its are designed to prevent the stage making contact with the mechanical
limits and if correctly setup the autostage should remain calibrated for
extended periods of use. If the mechanical limits are hit the stage will
become uncalibrated, as shown in the software. Once this has occurred the
stage may still be moved manually but the software limits will not operate
and stage movements using Manger flow chart will not be possible until the
stage is recalibrated. The status of each axis is displayed by the colour of
the push buttons. When the buttons are green the axis is calibrated.
If the software has been re-started assuming that the stage has not been
moved while Vision was not communicating with the instrument the stage
will remain calibrated and it should be possible to continue using the stage
in either manual or manager modes.

press to enable
jog mode
FIGURE 57. Manipulator control window.
To calibrate the stage click on the calibrate button above the mimic diagram
then click confirm. The stage is driven to the limit switch in each axis so its
position can be accurately defined. After the position of the stage in each
axis has been determined the stage is moved to an pre-determined position.
The stage is now calibrated and automatic control of the stage by the data
system is possible. The calibrated light in the manipulator section should
now be green.
4.8.2 Manual Stage Control
To move the stage manually use the manual stage control buttons either on
the stage mimic diagram or the hardware box. N.B. Care must be taken
not to drive the stage into the dual anode when moving the stage man-
ually.
The manual stage control offers the capability to move in defined step sizes.
This mode of stage movement is called jog mode and is enabled by click-
ing on the jog mode radio button, Figure 57. The magnitude of the move-
ment made on a single press of the > or >> button is defined in the text
boxes associated with the jog mode box. With jog mode enabled the auto-
stage movements associated with automatic acquisitions and the go to
operation will not work.

Z-axis control
X axis control
Y-axis control
theta axis control
Current stage coordinates
FIGURE 58. Manual stage control.
Left mouse click and hold down the mouse button on the double
arrow to move the stage quickly
Left mouse click on the single arrow to move the stage slowly
FIGURE 59. Manual control buttons.
In addition to the stage controls available in the manual window the Ultra is
supplied with a remote control box, FIGURE 60.

Speed of rotation of Direction of rotation

azimuthal rotation of azimuthal rotation
device (accessory) device (accessory)
Y axis control
(towards dual anode)
X axis control (towards X axis control

STC-SAC valve) (towards instrument
rack)
Y axis control (towards
mono) Z axis control (up)
Theta X axis (tilting Theta X axis

towards mono) (tilting towards dual
anode)
Z axis control (down)
FIGURE 60. Autostage remote control.
This remote control box can be used to move the stage. For example, if the
stage needs to be moved in the X-axis towards the STC-SAC valve then
check that the stage if in manual mode and simply press and hold the appro-
priate X-axis button on the remote. If the higher speed is required, press
and hold down the opposite X-axis button while keeping the original button
depressed.
4.8.3 Automatic Stage Control
The manipulator section in the manual window can be used to save and cre-
ate lists of stage positions. This is extremely useful when more than one
sample is mounted on the sample holder as it enables the software to drive
the stage to a pre-defined position and acquire data from a different sample
or position automatically.
The first step in automated control is the creation of a stage position table.
This table is titled the Table and can be displayed by selecting the table
button in the manipulator section of the manual control window, FIGURE 61.

Positions box
General position table
FIGURE 61. Manipulator positions.
The controls available in the general table section are described below.
Save Table: Saves the current table to a file so that it can be recalled later.
After pressing the button a browser box will appear to prompt for a file
name.
Read Positions: Recalls previously saved position tables. N.B. the saved
positions replace any positions currently inserted into the general position
table. Therefore, if the current positions defined in the table are required
they must be saved using the Save Positions command before the previ-
ously saved positions are restored.
Goto: This button moves the stage to the current selected table row, i.e. the
table row which is highlighted by a black box in the figure below.

Add: This button inserts the current stage positions into the selected table
row and is the way to add new stage positions to the table.
Update: should be used to update (overwrite) the stage coordinates of the

selected table row.
Insert Row: This button is used to insert stage positions into the general
position table. When current point is selected as the Insert Mode the cur-
rent stage coordinates will be inserted into the table.
Reset Row: This button removes the X, Y, Z and theta X coordinates of the
selected table row.
Delete Row: Deletes the currently selected table row.
Clear All Rows: Deletes all rows in the table.
FIGURE 62. Insert Mode

4.8.3.1 Inserting a stage position in the general position table
To insert a stage position into the general position table follow the instruc-
tions outlined below:
1. Set the stage to manual mode.
2. Move the stage to the desired position.
3. Highlight an empty row in the position table by left clicking in the row.
When highlighted the row should be surrounded by a black box,
FIGURE 63.
Left click here to

highlight row
Table scroll bar
FIGURE 63. Highlight general position table row.
4. The Current point label may be edited by using the left mouse button to
highlight the text and typing in text more descriptive of the sample.
Many positions may be entered into the position table in this manner:
5. Move the stage to the next position.
6. Highlight the row below the first position.
7. Click on the Insert row button to enter the co-ordinates of the new point
into the position table.
8. Add more positions by moving the table scroll bar downwards to reveal
an empty table row, FIGURE 63.
To delete any position in the table simply highlight the unwanted entry and
click Delete row. Clear All Rows permanently removes all entries from the
position table.

4.8.3.2 Driving the Autostage to a Position Defined in the General Position Table
To drive the stage to one of the positions defined in the general position
table follow the instructions outlined below:
1. Highlight the desired position in the position table by left clicking on it.
When highlighted the row is surrounded by a black box.
2. Click on Goto Position, this drives the stage automatically to the posi-
tion defined in the row. Note that this will NOT work if jog mode is
selected.
During the automatic movement the axis lables change colour. Once the
correct position has been reached the Halt lamp turns to green.
4.8.3.3 Saving and Retrieving a Position Table
Once positions have been entered into the table they can be saved and
retrieved at a later date. Follow the instructions below to save a position
table:
1. Left click on the Save Positions button, this opens a dialogue window,
FIGURE 64.
Present directory
Stored position tables
Double click here to
move up a directory
Enter table name here
Click OK to save the table

and close the window
FIGURE 64. Save positions dialogue window.
2. The default directory is C:/stage positions but this can be changed by

double clicking on other directory entries.
3. Enter a file name for the table.
4. Click OK to save the table and close the window.

The table is saved as a .dset file. To recall the table follow the method out-
lined below: N.B. recalling a saved position table overwrites positions
stored in the general position table.
1. Click on Read Positions, this opens a dialogue box similar to the one
shown above, FIGURE 64.
2. Select the required dset file with the left mouse button.
3. Click OK.
The saved position table is loaded back into the general position table.
4.8.4 Automatically Finding the Correct Analysis Height
The correct height for spectroscopic analysis can be automatically deter-

mined by the software for samples of different thicknesses. This section will
describe how the auto Z routine can be performed in the manual window.
Auto Z can also be included as part of an automatic sample analysis
sequence defined in the manager window but the operational description of
this feature is included in the manager section, Section 7.3.7 on page 237.
It is assumed that a sample has been placed at the analysis position (see
Section 4.8.7 on page 120). The analysis height can be optimised on any
XPS position recorded in the stage position table but the instructions below
describe the procedure for finding the correct analysis height of a large,
homogenous sample.
1. Position the sample at the analysis position using the optical camera
system.
2. Insert the current position in the general position table, Section 4.8.3.1
on page 111.
3. A spectrum for optimisation must now be initiated. The following exam-
ple describes the procedure for a large silver sample but the same basic
method can be followed for any material. A snap shot spectrum is used
because of the high speed of data acquisition.
4. Scroll upwards in the manual window to the Analyser control section.
Set the following parameters: analyser mode - spectrum; lens mode -
fov1; resolution - 160 eV; slot, Figure 65.
Analyser Mode Lens Mode Resolution Analysis Area
FIGURE 65. Analyser control.

5. Click on the Energy regions box of the Acquisition control section,

Figure 66.
6. Change the Type to snap shot, Figure 66.
7. A peak to acquire must now be selected. In this example we will choose
the Ag 3d3/5 peak but for many samples O 1s or C 1s would be good first
guesses (N.B. dont forget to switch the charge neutraliser on for insulat-
ing samples). Enter Ag 3d in the Region Name box and press return. If
you are unsure which peak to use a rapid survey spectrum can be
recorded to quickly identify the most intense peaks.
8. Starting values for the scan are loaded into the active region row from
the element library. Edit the values as follows: Centre eV : 371; Dwell ms
: 3000; # Sweep : 1 and shown in Figure 66.
FIGURE 66. Acquisition control section.

9. Scroll down to the X-ray section, enter values for the Emission current
(e.g. 5 mA) and the Anode HT (e.g. 15 kV). Switch the X-rays on,
Figure 67.
FIGURE 67. X-ray PSU control.

10. Make sure the current position is selected by left clicking on the entry in
the position table.
11. Enter parameters for the Auto Z routine. Suggested starting values are:
No. Increments 21 (NB the number of increments must be odd, if an even
number is entered it will be automatically changed to the next odd
number); Z increment (mm) 0.05, Figure 68. Ensure that the Ordinate
Choice button is set to Area.
FIGURE 68. Auto Z parameters.
12. Ensure that the Acquisition settings box is set to Current Manual and
click on Grab Scan to load the current active snap shot settings into the
Auto Z routine. NB if the scan fails to load check that the active button in
the Energy Regions table is selected, Figure 66.
13. Click on the Optimize position button to start the Snap Shot and begin
the automatic sample height routine.
14. The stage will now move 10 steps below the current position (500
microns in this example). The area under the peak will be recorded in the
computers memory. The stage will move up one step (50 microns) and
record the snapshot area again. This will continue until the stage has
stepped through all positions finishing 500 microns higher than the point
inserted into the table.
15. On completion a Z value corresponding to the height where the maxi-
mum snapshot area was recorded will replace the original Z Axis coordi-
nate in the position table, Figure 69. Furthermore the stage will move to
that height.

Optimised Z value
FIGURE 69. Optimised position table.
16. A new object labelled Auto Scan Profi will be written to the Acquiring
section in the manager window, Figure 70.
Auto Scan Object
FIGURE 70. Auto Scan Object in the acquisition section.

17. To view the profile select it by left clicking on the object and paste it into
the right hand side of the real time display window by moving the mouse
over to the right hand side of the window and clicking on the scroll ball,
Figure 71.

FIGURE 71. Auto Scan Profile pasted into real time display.
4.8.5 Transferring a Sample Stub to the SAC
The following method assumes that the sample stub has been previously
introduced into the STC and is loaded onto the claw of the sample transfer
probe, see Section 4.6.1.1 on page 94.
1. Check the pressure in the STC and the SAC. Both the SAC and the
STC should be below 5 x 10-6 torr.
2. Check that the dual anode is fully retracted.
3. Check that the sample probe is fully retracted into the STC and the
probe sensor is green, FIGURE 50.
4. Click on the Open STC-SAC Valve automatic vacuum sequence to open
the valve between the STC and SAC. See Section 3.1.6 on page 44 for
further instructions on how to operate the vacuum system.
5. Wait for the vacuum mimic diagram to indicate that the STC-SAC valve
is open, FIGURE 72.

STC-SAC Valve in open position
FIGURE 72. STC-SAC valve in mimic diagram.
6. Wind the transfer probe through to the SAC so that the stub is visible
through the small view port adjacent to the mono housing, FIGURE 73.
FIGURE 73. Sample transfer through small view port.
7. Select manual mode for the autostage.

8. Position the autostage fork so that it is the same height as the bottom
slot in the sample stub.
9. Check the Y-axis position of the stage to make sure the sample stub will
slide onto the fork, FIGURE 74.
FIGURE 74. Sample transfer through large view port.
10. Wind the sample transfer probe in further so that the sample stub slides
onto the autostage fork. If position correctly the stub should slide easily
onto the fork. If the transfer feels tight then fine adjustment of the auto-
stage position may be required.
11. Push the sample stub full onto the autostage fork.
12. Drive the autostage in the Y-axis towards the mono X-ray gun to disen-
gage the transfer probe claw from the top slot in the sample stub. Wig-
gling the transfer probe gently helps the claw disengage smoothly.
13. Once the sample transfer claw has cleared the sample stub the transfer
probe can be fully retracted.
14. Check that the transfer probe is fully retracted and that the probe sensor
is green.
15. Close the STC-SAC valve.
Saving the standard transfer positions in a file can greatly improve the
speed and security of sample transfers. Simply re-load the relevant position
table and position the stage appropriately. For example, sample stub and
bar load and unload starting positions may be saved in a table and recalled
every time a sample transfer is performed.
N.B. the autostage fork has room for two sample stubs to be loaded at one
time.

4.8.6 Removing a Sample Stub from the SAC
Follow the procedure below to remove a sample stub from the SAC:
1. Check that the stage is in manual mode.
3. Drive the autostage to a point where it is easily visible through the small
view port to the left of the mono housing.
4. Move the stub towards the mono until the stage reaches the software
limit of its Y-axis movement. As noted above, saving a standard stub out
position greatly increases the speed of this operation.
5. Check the pressures in the SAC and STC. Both the SAC and the STC
should be below 5 x 10-6 torr.
is open, FIGURE 72.
9. Wind the transfer probe through to the SAC so that the probe claw is vis-
ible through the small view port adjacent to the mono housing.
10. Position the claw adjacent to the sample stub top slot.
11. Move the autostage in the Y-axis towards the dual anode so that the
transfer probe claw engages with the top stub slot. Wiggling the transfer
probe gently helps the claw engage smoothly.
12. Once the stub is firmly engaged on the transfer probe claw, the probe
can be carefully wound back into the STC removing the stub from the
autostage. The movement should be smooth. If resistance is left fine
adjustment of the autostage may be required.
4.8.7 Transferring a Sample Bar to the SAC
The following method assumes that the sample bar has been previously
introduced into the STC and is loaded onto the claw of the sample transfer
probe, see Section 4.7.0.2 on page 103.
1. Check the pressure in the STC and the SAC. Both the SAC and the
STC should be below 5 x 10-6 torr.
is open, FIGURE 72.
6. Wind the transfer probe through to the SAC so that the bar is visible
through the small view port adjacent to the mono housing, FIGURE 75.

FIGURE 75. Bar visible through small view port.
7. Select manual mode for the autostage.

8. Position the autostage fork so that it is the same height as the bottom
slot in the sample bar. As noted above, saving a standard bar in position
greatly increases the speed of this operation.
9. Check the Y-axis position of the stage to make sure the sample bar will
slide onto the fork, FIGURE 76.
FIGURE 76. Auto stage position during bar load.

10. Wind the sample transfer probe in further so that the sample bar slides
onto the autostage fork. If position correctly the bar should slide easily
onto the fork. If the transfer feels tight then fine adjustment of the auto-
stage position may be required.
11. Push the sample bar full onto the autostage fork.
12. Drive the autostage in the Y-axis towards the mono X-ray gun to disen-
gage the transfer probe claw from the top slot in the sample bar. Wiggling
the transfer probe gently helps the claw disengage smoothly.
13. Once the sample transfer claw has cleared the sample stub the transfer
probe can be fully retracted.
14. Check that the transfer probe is fully retracted and that the probe sensor
is green.
15. Close the STC-SAC valve.
4.8.8 Removing a Sample Bar from the SAC
Follow the procedure below to remove a sample bar from the SAC:
1. Check that the stage is in manual mode.
3. Drive the autostage to a point where it is easily visible through the small
view port to the left of the mono housing.
4. Move the bar towards the mono until the stage reaches the software limit
of its Y-axis movement. As noted above, saving a standard bar out posi-
tion greatly increases the speed of this operation.
5. Check the pressures in the SAC and STC. Both the SAC and the STC
should be below 5 x 10-6 torr.
is open, FIGURE 72.
9. Wind the transfer probe through to the SAC so that the probe claw is vis-
ible through the small view port adjacent to the mono housing.
10. Position the claw adjacent to the sample bar top slot, FIGURE 77.

FIGURE 77. Sample bar unload from SAC.
11. Move the autostage in the Y-axis towards the dual anode so that the
transfer probe claw engages with the top bar slot. Wiggling the transfer
probe gently helps the claw engage smoothly.
12. Once the bar is firmly engaged on the transfer probe claw, the probe
can be carefully wound back into the STC removing the bar from the
autostage. The movement should be smooth. If resistance is left fine
adjustment of the autostage may be required.

Aperture and Iris Drives
4.9. Aperture and Iris Drives
The aperture and iris are automatically controlled by the analysis area
selection, see Section 4.4.5 on page 74. However the current positions of
the aperture and iris drives are displayed, FIGURE 78.
FIGURE 78. Aperture and Iris drives
The default setting of the Manual window has the aperture and iris sections
shown in Figure 78 are hidden. They may be displayed by selecting the but-
tons at the top of the manual window,
FIGURE 79. Iris and aperture buttons to display these sections.
Under normal operating conditions it should never be necessary to change

or alter any of the aperture or iris positions or parameters. Access to these
settings can only be gained in engineer mode.
The status of the aperture and iris is reported at the bottom of the manual
window, where aperture and iris in bold indicate that both are calibrated,
shown in Figure 80.

bold text indicates that iris & aperture are calibrated
FIGURE 80. calibrated status of iris and aperture drives


13 July 2009
Chapter 5
Mini Beam I and III
Ion sources
This chapter describes the alignment and operation of the Mini Beam ion
sources. The AXIS Ultra is fitted with either the Mini Beam I, Mini Beam III
or the MB IV floating ion source. The next chapter will detail the operation of
the floating ion source. The sources are intended for general sample clean-
ing and depth profiling experiments. The sources are under full computer
control enabling standard settings to be saved to file and recalled for future
experiments. A general overview of the ion sources and associated elec-
tronics will be followed by an in depth description of the operation. Also
included is a section on the alignment of the ion beam with the analysis
position.
5.1. The Ionisation Chamber
The ionisation chamber is similar in operation and design for both ion
sources and will therefore be discussed in a single section. It is a classic
electron bombardment ionisation source where gas is leaked into a cham-
ber and ionised by electron bombardment. The electrons are extracted from
a hot Rhenium filament through a grid, and ions generated in the centre of
the grid cylinder are extracted through a small aperture which acts as the
source, Figure 1. The whole source assembly is at high voltage, with the
beam energy equal to that of the filament.
127
The Ionisation Chamber
FIGURE 1. Schematic of the ionisation chamber of the Mini Beam I and III ion sources.
During operation the walls of the chamber and the extraction electrode are
at earth potential. To aid explanation of the various potentials applied in the
ionisation chamber we will assume that the final ion energy required is 4000
eV. In this situation the filament supply is at +3800 V with respect to Earth
potential.
Ionisation of the gas atoms inside the grid region is by bombardment with
electrons of typically 200 eV energy. The electrons are generated by the fil-
ament (by heating it with an electric current) and are accelerated through
the grid into the middle of the ionisation region. If the filament is at +3800 V
then the grid will be between 100 and 200 V positive with respect to it, in this
case we will assume the grid is 200 V positive with respect to the filament.
This means that the grid is at a potential of +4000 V with respect to Earth.
The ions produced within the grid are accelerated out of the ionisation
region by the extraction electrode (the extractor), Figure 1. The extraction
electrode has a negative potential with respect to the filament (for positive
ions). The extraction potential can be varied between 0 and -102 V with
respect to the filament. In this case the negative extractor potential is -35 V.
This means that the potential on the extractor is +3765 V with respect to
earth.
In operation the accelerating electrode will be at Earth potential. Therefore,

in this case we have the following potentials with respect to Earth, Table 1
and Figure 2.
128 Chapter 5 Mini Beam I and III Ion sources

Overview of Mini Beam I (WX-414)
TABLE 1. Electrode voltages with respect to Earth
Electrode Potential (V)

Filament +3800
Grid +4000
Extractor +3765
Accelerating 0
FIGURE 2. Electrode voltages of the ion source for a 4 kV ion beam energy.
The actual energy of the ion beam emerging from the accelerating electrode
is 4000 eV (filament potential + grid potential). The voltages on the filament
and extractor are set approximately equal so that the extractor does not
effect the movement of electrons towards the grid.
5.2. Overview of Mini Beam I (WX-414)
The Mini Beam I Ion source provides a high current density, variable diame-
ter, scannable ion beam for precision ion beam studies and applications,
Figure 3.
Chapter 5 Mini Beam I and III Ion sources 129

Overview of Mini Beam I (WX-414)
FIGURE 3. Mini Beam I ion source.
The system consists of an ion source and an ion source control. The ion
source will provide an ion beam which can be varied from 125um in diame-
ter up to millimetres by the use of electrostatic focusing. It contains electro-
static deflection plates which allow the beam to be scanned in two
dimensions. The ion source control provides the power and control voltages
necessary to operate the ion source. The source is designed to operate
between 5 kV and 1 kV. Use inert gases only, Argon, Neon or Helium. The
ion source is differentially pumped via the STC turbomolecular pump. Dif-
ferential pumping enables the pressure in the SAC to remain 104 times
lower than the pressure in the ion source.
5.2.1 Mini Beam I Ion Optics
The Mini Beam I lens optics are discussed below, As the ions emerge from
the extractor plate (in the ion source), their trajectories are corrected to
focus either: near lens 1 (L1 - the condenser lens) for the smallest beam
sizes; or on the final aperture for the largest beam sizes; or focused approx-
imately halfway between lens 1 and the final aperture for the medium sized
beams. Lens 2, the focus lens (L2), provides the final focusing which deter-
mines the sharpness of the spot as it strikes the target.

Overview of the Mini Beam III (WX-422)
Ion beam
trajectory
from
ionisation
chamber
L1 Condenser Lens Final Aperture L2 Focus Lens Deflector Plates
FIGURE 4. Mini Beam I lens arrangement.
The deflection plates, which are located just inside the exit aperture, posi-
tion the beam electrostatically onto the target. The X and Y deflectors are
applied with saw tooth waveforms at particular amplitude and frequency
then the ion beam is deflected accordingly and is therefore rastered across
the sample surface. This allows a large area of the sample to be sputtered
but with a loss of beam current density.
5.3. Overview of the Mini Beam III (WX-422)
The Mini Beam III Ion Gun provides a high current density, variable diame-
ter, scannable ion beam for precision ion beam studies and applications.
The system consists of an ion gun and an ion gun control. The ion gun will
provide an ion beam which can be varied from 35um in diameter up to milli-
metres by the use of electrostatic focusing. It contains electrostatic deflec-
tion plates which allow the beam to be scanned in two dimensions. The ion
gun control provides the power and control voltages necessary to operate
the ion gun.
The source is designed to operate between 5 kV and 1 kV. Use inert gases
only, Argon, Neon or Helium. The ion source is differentially pumped via the
STC turbomolecular pump. Differential pumping enables the pressure in the
SAC to remain 104 times lower than the pressure in the ion source.
5.3.1 Mini Beam III Ion Optics
The ion gun contains a source with a grid and filament, an extractor plate,
electrostatic lens 1 and 2 (condenser lens L1 and focus lens L2) which are
separated by the final aperture, X and Y alignment plates, and the x-y
octapole deflection plates Figure 5.

Overview of the Mini Beam III (WX-422)
L1, Condenser Lens Octopole Deflection Plates
2 Degree Bend
X Deflection Plates Y Deflection Plates L2, Focus Lens
FIGURE 5. Schematic of Mini Beam III Ion Optics.
The ions are generated in the source and extracted by the extractor plate.
The ionisation chamber, extraction electrode and the acceleration electrode
provide a small source (approximately 1 mm diameter) of energetic ions.
The energy spread is low and the actual energy depends on the beam volt-
age and the grid voltage, see Section 5.1 on page 127. As the ions emerge
from the extractor plate, their trajectories are corrected by the X deflector
into the condenser lens L1. Ions are focused either near lens 1 for small
beam sizes, or on the final aperture for large beam sizes, or focused
approximately halfway between lens 1 and the final aperture for the medium
beam.
Between the condenser lens and the final aperture are the Y deflection
plates. These plates steer the ion beam around a 2 degree bend in the ion
column. The purpose of this bend is to remove energetic neutral atoms
from the ion beam. These fast neutrals are formed by charge transfer colli-
sions when the ion beam passes through regions of relatively high pres-
sures (i.e. at the exit of the ionisation chamber). An energetic ion may
interact with a residual gas atom losing an electron to become an energetic
neutral atom and leaving a low energy positive ion. Because of the charge
neutralisation process (which has a significant probability at pressures
above 10-6 torr) the ion beam from the source region will always have a
small percentage of energetic neutrals. The Y deflection plates deflect the
charged ion beam into the final lens whilst the energetic neutrals are not
deflected and are lost from the beam.
Following the final aperture are the octapole deflection plates which are
used to raster the ion beam across the sample surface. Lens 2, the focus
anode, provides the final focusing which determines the sharpness of the
spot as it strikes the target.

Depth Profiling
5.3.2 Ion Beam Stabilisation
The MB III ion beam is stabilised so that a constant ion current leaves the
ion source. The current of ions reaching the extraction electrode is main-
tained at a fixed value by varying the filament current. This negative feed-
back loop ensures that a constant etch rate can be maintained for a period
of time even if the argon gas pressure varies by small amounts during the
experiment.
Active stabilisation of the extraction current is only possible within a range of

values. A filament current limit is present to prevent the filament becoming
too hot due to high a current. If the source conditions change to such an
extent that the heating current of the filament increases to this value then
active stabilisation of the extraction current will cease. There is also a max-
imum filament emission current of 30 mA. This limitation prevents heat gen-
erated within the source reaching damaging levels. Thus when an emission
current of 30 mA is reached the current through the filament is limited and
active stabilisation of the extraction current again ceases.
5.4. Depth Profiling
When a relatively thick layer (hundreds of nm) needs to be removed and

inter-layer resolution is of secondary importance it is advisable to use a high
energy ion beam. This has the advantage of allowing a fast depth profile
over a well defined small area. The higher the beam energy the more rap-
idly the specimen is eroded away for a given beam current density. This is
because the sputtering coefficient (nominally the number of sputtered atoms
eroded from the surface per incident ion) is greater for higher bombardment
energies. At relatively high beam energies (e.g. 4 keV) more ion current can
be delivered and smaller beam diameters are achieved. The brightness of
the source (expressed as the current per unit area of the source into unit
solid angle (Amp/cm2/sr) is higher for higher accelerating volts. Also the
chromatic aberration at higher beam energies is smaller because the spread
of ion energies from the source is small compared with the overall beam
energy.
If an improved interlayer resolution is required the incident ion energy may

be reduced to approximately 2 KV. This reduces the chemical damage to
the sample and minimises interlayer ion beam mixing.
Rastering the ion beam across the sample surface and collecting informa-
tion from the middle of the etch crater, Figure 6, ensures that the XPS spec-
tra are representative of the middle of the square etch pit and not of the
edge where the ion beam may have caused uneven etching (edge effects),
Figure 7. Note that the ion beam centre needs to be well aligned with the
analysis position so that spectra are recorded from the centre of the etch
crater, see section Section 5.7.2 on page 151.

Depth Profiling
acceptance cone of spectrometer
rastering ion beam

ion beam etch pit
sample surface
Specimen
FIGURE 6. Schematic of the ion beam depth profiling experiment.
FIGURE 7. Schematic diagram illustrating the edge effects in a rastered ion etch pit. The
analysis area should coincide with the dark grey area in the centre of the etched
hole.

Manual Software Interface
5.5. Manual Software Interface
Manual control of the ion source is possible using the ion source interface in
the manual window. Scroll down to near the bottom of the manual control
window, Figure 8.
FIGURE 8. Ion source section of manual window.
To view the ion source controls, sample current measurement (bias), table
of stored values (table), current ion source status (status) and ion source
settings (tuning) click on the relevant button.
Once operating conditions have been chosen and argon gas has been intro-
duced into the instrument the ion source can be switched to standby then
to on manually by clicking on the respective buttons. An automated degas
sequence for the ion source filament is included for use after the machine
has been let up to atmosphere. This procedure gently increases the current
through the filament to slowly remove surface contamination, see
5.5.1 Ion source Controls
Click on Control button to open the manual control section, Figure 10 (for
Minibeam I) and Figure 10 (Minibeam III).

FIGURE 9. Ion source control for MB I
Source HT Extractor current setting Float Voltage
Beam
Energy
Raster Size (calculated) Etch Rate (calculated) Current Density readback

readback
FIGURE 10. Ion source control for MB III
Note that the user interface is slightly different depending on the ion source
present on the instrument. The control sections defined in the windows are
detailed in the following sections. Note that only emission stabilised control
is available with the Minibeam I and that a float voltage can not be defined
for either Minibeam I or III ion sources.
5.5.1.1 Source High Tension (HT)
The source high tension in kilovolts is set in this box. It can be varied
between 1 kV and 4.8 kV. N.B. this value is the voltage of the filament with
respect to earth and not the beam energy when it leaves the ion source, see
below.

5.5.1.2 Extractor / Emission Toggle and Extractor or Emission Current
The toggle button switches the ion source between extractor current control
and emission current control. Only emission control is available for the Mini
Beam I. In extractor mode the ion source monitors the current of ions
reaching the extraction electrode. This extractor current then forms the
basis of the filament current control circuit, see Section 5.3.2 on page 133.
When emission is selected the filament current is adjusted to give a con-
stant electron emission current (measured between the filament and collec-
tor). Extractor current control is directly related to the ion current at the
sample whereas under emission control the actual ion current reaching the
sample is also dependent on the gas pressure in the ion source.
The actual ion extraction current (or electron emission current) required is
set in the current box. Values of extractor current can range from 0 to 150
uA and values for the emission current can be adjusted between 0 and 20
mA.
5.5.1.3 Float Voltage
Not applicable to the Mini Beam I and III.
5.5.1.4 Beam Energy
This is a read back of the actual ion energy (singly charged ions only) leav-
ing the ion source. Details of how this value is calculated can be found in
Section 5.1 on page 127.
5.5.1.5 Etch Rate
The etch rate in Angstroms per minute expected for the current ion source
settings is displayed here.
5.5.1.6 Sample Current
The ion current expected to reach the sample is given here. N.B. the cur-
rent given assumes no affects from secondary electron / ion emission or
charging problems.
5.5.1.7 Raster Size
This setting controls the size of the crater (mm x mm) formed by rastering
the ion beam across the sample surface. The raster pattern is formed by
applying a saw toothed voltage pattern on to the octapole deflection plates.
5.5.2 Ion source Table
Click on the table tick box to open a table with a list of presets for the ion
source, Figure 11. Values stored in the table can be recalled into the ion
control section. Therefore, during standard operation of the ion source, the
user does not have to enter values for every ion source parameter. Further-

more, custom settings and changes to the preset values can be saved for
future use.
Restore row
Update row
Preset row
name
Scroll bar
Table Controls Acceleration HT Extractor Current Beam Current at 50 uA

(table value) (table values)
Extraction current
FIGURE 11. Ion source preset table.
5.5.2.1 Update Row
Updates the current row over-writing the existing values with the current ion
source settings. N.B. if this button is inadvertently pressed important set-
tings can be over written. If this happens close Vision2 without saving the
configuration file and restart.
5.5.2.2 Restore Row
Restores the values in the selected table entry to the control section. For
usage instructions see Section 5.7.4 on page 156.
5.5.2.3 Preset Row
The preset row stores the lens settings for each operating mode. For each
mode the Acceleration voltage, Extractor current and standard Beam cur-
rent are displayed to aid identification. The preset row name is editable.
5.5.3 Tuning
Click on the Tuning tick box to open the ion source tuning section, Figure 8.
This section allows manual control of lens voltages and other settings. The
values are entered automatically when a preset row from the table is
restored, see above. The various controls can be modified by moving the
slider bar or entering the new number directly in the box, Figure 12.

Filament Current Limit Grid Voltage Extractor Voltage
Focus Align X Align Y
filament selector
condenser
Scale X Scale Y Offset X Offset Y
Max FSD
FIGURE 12. Manual ion source tuning section.
5.5.3.1 Filament selector
Not applicable to the Mini Beam I and III.
5.5.3.2 Filament Current Limit
The filament current limit sets the maximum current that can pass through
the selected filament. The value chosen is usually slightly higher than the
current required to reach maximum electron emission. As the filament ages
this value may need to be increased to ensure that it is not limiting the max-
imum emission.
5.5.3.3 Grid Voltage
The grid voltage control sets the voltage on the grid with respect to the fila-
ment as described in Section 5.1 on page 127. The voltage can vary
between 100 and 200 volts.
5.5.3.4 Extractor Voltage
The extractor control sets the voltage on the extraction electrode with
respect to the filament as described in Section 5.1 on page 127. The volt-
age can take any value between 0 and 102 volts.
5.5.3.5 Condenser
The condenser control sets the voltage on the condenser lens (L1). This
lens is adjusted to change the size of the final ion spot on the specimen. It
can be varied between 0 and 5000 volts.

5.5.3.6 Focus
The focus control set the voltage on the focus lens (L2). This lens focus the
ion spot on the specimen. The focus voltage can be varied between 0 and
5000 volts.
5.5.3.7 Align X and Align Y.
This is not applicable to the Mini Beam I. The Mini Beam III ion source has
a 2 degree bend used to remove energetic neutrals from the ion beam.
These controls set the voltage on the deflection plates, X and Y. This is
used to deflect the ion beam around the bend. As the bend is only in one
axis only the align X control is usually used. The voltage can be varied
5.5.3.8 Scale X and Y
The size of an etch crater is determined by the Raster size control,

Section 5.5.1 on page 135. However, as the ion source is not mounted nor-
mal to the sample surface simply rastering the beam by equivalent amounts
in both the X and the Y directions would result in rectangular etch craters.
The scale controls add scaling factors to the voltages applied to the
octapole deflection plates to ensure that a square etch crater is formed. The
scaling factors can be varied between 0 and 200 volts.
These values directly effect the size of the etch crater produced and there-
fore should be set as close to the maximum value as possible.
5.5.3.9 Offset X and Y
Fixed voltage offsets can be applied to the octapole deflection plates to fine
tune the position of the ion spot relative to the analysis position. Voltages
between -110 and +110 may be applied to the deflection plates to account
for any mechanical misalignment of the ion source with the analysis posi-
tion. However, it should be noted that these alignment voltages should be
kept as low as possible as they may effect the maximum raster size availa-
ble. If this is the case a warning message will appear displaying the text
WARNING: Raster waveform clipped.
5.5.3.10 Max FSD
The Maximum Full Scale Deflection is measured in mm and is the maximum

crater size available. It can be varied between 0 and 6 mm depending on
the set up conditions of each ion source.
5.5.4 Status
Click on Status tick box to open the ion source status read-backs, Figure 8.
This section displays the current status of the ion source, Figure 13.

Source HT Filament current Extractor Volts Extractor Current
Float Voltage Grid Voltage Condenser (L2) Focus (L3)

Voltage Voltage
Alignment X1 Alignment X2 Emission Current
FIGURE 13. Ion source status read-backs
5.5.4.1 Source HT
This read-back displays the high voltage applied to the ion source. It will
read 0 unless the ion source is set to On. N.B. if a pre or post etch delay is
set in the manager window then the High voltage will be set to on during the
delays but the alignment voltages will be set to maximum to prevent ions
reaching the sample surface.
5.5.4.2 Filament
The filament read-back displays the present filament current. When the ion
source is set to off the filament current will fall to zero. If the ion source is in
the standby or the on state then the filament current will be varied automati-
cally to produce the requested ion extraction current, see Section 5.3.2 on
page 133. The filament current cannot exceed the filament current limit
(Section 5.5.3 on page 138).
This reads back the actual extraction voltage relative to the filament applied
to the ion source.
5.5.4.4 Extractor Current
Not applicable to the Mini Beam I ion source. The extractor current read
back displays the ion current reaching the extraction electrode in micro
amps, see Section 5.3.2 on page 133. The filament current is adjusted
using a negative feedback loop arrangement to keep this value constant
and hence ensure a constant ion current leaving the ion source. The extrac-
tion current is stabilised when the ion source is set to standby or on. Effec-
tive stabilisation is only possible over a narrow pressure range and two
limiting factors can prevent the correct extractor current being reached. The
first of these is the filament current limit (Section 5.5.3.2 on page 139). If
the filament current reaches the limit then effective control of the ion extrac-
tion current will cease. The second limiting factor is the electron emission

current from the filament. This value is limited to 30 mA to protect the ion
source from excessive internal temperatures. If the emission current
reaches this value then effective control of the extraction current will stop.
Not applicable to the Mini Beam I and III ion sources.
Read back of the voltage applied to the extractor grid in the source region of
the ion source, Figure 1.
5.5.4.7 Condenser
The voltage applied to the condenser lens (lens L2).
5.5.4.8 Focus
Read back of the voltage applied to the focus lens (lens L3).
5.5.4.9 Alignment X1 and X2
Not applicable to the Mini Beam I ion source. Displays the voltage applied
to the beam alignment plates (A1 and A2). These voltage are set to high
values when the ion source is set to standby and during pre and post etch
delays. This is to reduce the possibility of ions reaching the specimen when
etching is not required.
5.5.4.10 Emission Current
This reads back the present electron current between the filament and the
collector. The filament current is limited automatically so that this value
does not exceed 20 mA.
5.5.5 Bias Current
Click on Bias to open the bias current section, Figure 8. When active the
bias current section allows the sample current (i.e. current of ions or elec-
trons reaching or leaving the sample platen) to be read. Two modes are
available, Measure sample current and Measure ion beam current. Toggle
between them by left mouse clicking on the setting, Figure 14 and Figure
15.

Switch on / off by clicking on Active Select mode by clicking on this button
select button to auto range

Set range of read-back by clicking on this button current reading
Sample current display
FIGURE 14. Bias Current read back.
Select mode by left clicking on either row
FIGURE 15. Sample current and ion beam current modes.
The sample current mode measures the sample current directly while the
ion beam mode places a 30 volt positive bias on the sample platen while
active. This bias voltage reduces the number of secondary electrons leav-
ing the sample and hence gives a more reliable reading of the actual ion
current reaching the sample. N.B. Sample or ion currents can only be
measured on conducting samples in electrical contact with the platen.
To change the scale on the read out click on the range button, Figure 14 and
Figure 16. Three read-back ranges are available, up to 20 nA, up to 2 uA
and up to 200 uA. The meter may also be set to auto range the upper limit
if the current increases beyond the maximum reading selected.
Left click on value to set meter range
FIGURE 16. Meter range.
5.5.6 Degas
Click on Degas tick box to open the ion source filament degas section, Fig-
ure 8. In Advanced mode the user would simply click on the degas button
to start the process. In Engineer mode the degas option allows the user to

slowly increase the current passing through the filament in order to gently
degas it. If the inside of the vacuum chamber has been exposed to the
atmosphere or the ion source hasnt been used for some time then the fila-
ment will be contaminated. Ramping the filament current up in a controlled
manner allows the filament to warm up gradually and contaminants are
driven off slowly. This increases the filament lifetime by reducing surface
damage of the filament.
can be set for larger values, Figure 17.
degas display in advanced mode
degas display in engineer mode
Regime 1, ramp time and final current
Regime 2, ramp time and final current
FIGURE 17. Degas settings.
To change the degas settings follow the instructions outlined below:
1: Enter a time in minutes into the regime 1, ramp time box (dont forget to
press return). A suitable value would be 10 minutes.
2: Enter a current setting in the regime 1 current box (e.g. 2 Amps).
3: Next enter a second time into regime 2 ramp box (e.g. 10 minutes).
4: Finally enter a second current setting into the regime 2 current box (e.g.
2.3 Amps). N.B. the final current setting should not exceed the filament
limit set for the selected filament, see Section 5.5.3 on page 138.
Before beginning the degas procedure it is advisable to open the ion

source differential pumping valve (V2), see Chapter 3. When the set-
tings have been entered to start the filament degas procedure left click on
the Degas On light, Figure 18.

Standard Manual Operation
Left click here to start the degas procedure
FIGURE 18. Degas On control.
Once on is selected the filament current will increase from 0 to the value set
in regime 1 in the entered time. After this time has elapsed the filament cur-
rent will continue to rise for the time entered in regime 2 reaching the maxi-
mum current value entered in regime 2.
5.6. Standard Manual Operation
This section describes the normal manual operation of the Mini Beam I and
III ion sources. It is assumed that the ion source has been installed and a
table of standard operating conditions created. Furthermore, it is also
assumed that the ion source has been correctly aligned with the analysis
position. For alignment instructions see Section 5.7.1 on page 149. Manual
operation of the ion source is defined as switching the source on from the
manual window. For automated depth profiling the ion source is controlled
from the instrument manager window. Such etch sequences will be
described in Section 7.3.9 on page 252.
5.6.1 Starting the flow of Argon
Before setting the ion source to standby the argon gas must be introduced
into the ionisation source. The procedure below assumes that the leak
valve has previously been set to the correct pressure. Follow the instruc-
tions below to switch on the argon gas:
1: Bring up the manual window, scroll down to the Vacuum control section
and select Automatic Sequences, Figure 19.
2: Check that the STC pressure is below 1 x 10-6 mbar and that the SAC
pressure is below 5 x 10-7 mbar.
3: Check that the SAC-STC value is closed and that the ion source differen-
tial pumping value (V2) is closed.
4: Click on the Ion source Gas On automatic sequence, Figure 19.

ion source
gas off
ion source
gas on
FIGURE 19. Automatic vacuum sequences.
5: This automated sequence opens the ion source differential pumping

value (V2) and the Argon gas inlet valve (V8), see Section 3.1.6 on page 44.
6: The pressure in the STC should increase to approximately 1 or 2 x 10-6

mbar.
5.6.2 Switching the ion source on
This section describes switching the ion source to standby from off then
switching the ion source on. It assumes that the Argon gas pressure has
been set according to the above procedure, Section 5.6.1 on page 145.
1: Scroll down the manual window to the ion source section, click on the fol-
lowing tick boxes: Controls; Status; and Table, Figure 20.
Ion source off Standby On Degas
settings Table Status Tuning
FIGURE 20. Ion source control buttons.

2: Select the required ion source operating conditions by left clicking on the
relevant row in the table so that it becomes highlighted.
3: Click on the Restore Row button to download the saved ion source set-
tings from the table to the ion source control, Figure 21. Parameters down-
loaded from the table include: Source HT; Extractor or emission current;
Float voltage; Condenser (L2) voltage; Focus (L3) voltage; Align X; and
Align Y.
Left click on the Restore Row button to download the stored settings
to the Ion source control
Left click in the table to highlight the required row
FIGURE 21. Restore Ion source saved settings.
4: Left click on the Standby button, Figure 20, to set the ion source to
Standby. On pressing the Standby button the software begins to slowly
ramp up the filament current. The filament current will continue to rise until
one of three limiting factors are reached: 1, the requested ion emission cur-
rent (or electron emission current for the Mini Beam I) is achieved (see
Section 5.3.2 on page 133); 2, the filament software current limit (usually set
between 2.4 and 2.8 amps); 3, the electron emission current limit (30 mA).
It may take up to 10 minutes for the correct ion current (or electron emission
current) to be reached and the read-back value may well overshoot the set
value until proper control is established. If the requested ion emission cur-
rent is not reached it may be due to insufficient gas pressure. Increase the
pressure by turning the leak valve anti-clockwise to allow more Argon gas to
enter the ionisation chamber. The STC pressure can be varied between 8 x
10-7 mbar and 3 x 10-6 mbar.
5: Once the set ion emission current (or electron emission current) has been
reached and has stabilised left click on the On button, Figure 20, to switch
the ion beam on. The set HT will be applied and the align X1 and X2 volt-
ages will also assume their set values.

5.6.3 Switching the ion source off
Follow the instructions below to manually turn the ion beam off.
1: If the ion source is to be used again in the near future then it can be left in
the standby mode with the gas on. Click on the Standby button, Figure 20.
This sets the ion source to the standby state.
2: If the ion source is not to be used for some time or the Argon gas is to be
turn off then the ion source must be switched off. Click on the Off button
(the ion source can be switched to off from the On state or the Standby
state), Figure 20. When set to off the HT is set to zero (if on) and the fila-
ment current is ramped down to zero which reduces the ion and electron
emission currents to zero.
3: The Argon gas can now be switched off. Scroll down to the Vacuum Con-
trol section and click on the Ion source Gas Off Automatic Sequence, Figure
22. N.B. For the Mini Beam III, if the Argon gas supply is switched off
while the ion source is switched to On or Standby then the filament
current will increase to the software filament current limit. While this
may not necessary damage the filament the situation should be
avoided in normal operation. The sequence automatically closes the
Argon gas inlet valve (V8) followed by the Backing valve (V3). The Argon
gas line pumping valve (V9) opens to pump the Argon gas line out between
the leak valve and Argon gas inlet valve (V8) using the rotary pump. After a
set time the Argon gas line pumping valve (V9) closes and the backing valve
opens (V3). Finally the ion source differential gas pumping valve is closed
to complete the sequence.
Ion source Gas Off
FIGURE 22. Ion source Gas Off sequence.

Ion source Tuning
5.7. Ion source Tuning
This section describes tuning of the ion beam size and focus at the speci-
men and how to align the ion beam at the analysis position. It should be
noted, however, that several ion source operating conditions will have been
determined by the Kratos engineer and stored in the ion source table, see
Section 5.5.2 on page 137. These notes are included in case the user has a
particular application which is not covered by the standard settings or if the
ion source needs to be re-aligned for any reason. Before commencing a
detailed description of how to tune the ion source a few general points about
tuning will be considered.
Increasing the voltage on the condenser lens (L2) will generally decrease
the size of the ion spot at the specimen. At a set beam energy, as the con-
denser voltage is increased the focus voltage (L3) needed to produce a
focused ion spot on the sample will decrease. As the condenser voltage is
reduced at a given beam energy then the focus voltage (L3) will increase.
Generally the smaller ion spot sizes at the specimen are achieved at the
higher beam energies. The minimum beam diameter at 4 kV is usually
between 200 and 250 microns.
5.7.1 Imaging the ion spot
It is extremely useful to be able to image the ion spot in real time during the
alignment process. To accomplish this a separate electrostatic lens mode is
enabled which has a large field of view allowing the ion spot to be easily
located and its position adjusted. This lens mode is labelled Field of View 4
and should have been set up by the installation engineer. If it is not present
on your system then please consult Kratos.
N.B. Imaging the ion spot for prolonged periods or at high intensities
can damage the channel plate detectors. For this reason time imaging
the ion spot should be kept to a minimum, imaging high resolution
mode should always be used (to ensure that the iris is at its smallest
setting) and steps should be taken to reduce the number of secondary
electrons produced (e.g. by decreasing the extractor current setting to
10 or 20 uA or running at low emission).
Using this lens mode it should be possible to image the ion spot in real time.
To do this follow the procedure outlined below:
1: Position an area of the sample bar which has no sample mounted on it at

the XPS position and set it to the correct height.
2: Go to the Parallel XPS imaging section of the Manual window. Select

running integral with an integration time of 5 seconds and a refresh time of
0.25 seconds, Figure 23.
3: Change the analysed energy to kinetic energy and select a low energy to
image, e.g. 400 eV, Figure 23.

Ion source Tuning
Analysed energy
FIGURE 23. Ion spot imaging.
4: Select Imaging for the analyser mode, Field of View 4 for the lens mode,
Pass Energy 160 and Imaging high resolution (sometimes labelled Imaging
dia3mm), Figure 23.
5: Restore the ion source settings which are to be tuned by clicking on

Restore Row, Figure 21.
6: Start the argon gas flow, see Section 5.6.1 on page 145.
7: Switch the ion source to standby and wait for the requested ion extraction
current to be reached, see Section 5.6.2 on page 146.
8: Set the raster size to zero, Figure 24.
raster size

Ion source Tuning
FIGURE 24. Raster size.
9: Switch the ion source on, see Section 5.6.2 on page 146.
10: Reselect the imaging aperture (as the iris drive is driven to the sputter
shield in position when the ion source is switched on).
11: Switch the parallel imaging to On, Section 23 on page 150. This should
open up a section in the bottom left hand side of the real time window. If the
image fails to appear then it may be necessary to increase the size of the
imaging section, in the real time display, by left clicking on the divider tab
and dragging out the tab to make the section larger.
5.7.2 Positioning the Ion Spot
If the ion source is mechanically well aligned to the analysis position then
the ion spot should now be visible in the imaging window. However, if the
ion source has been moved mechanically it is possible that it could be point-
ing well away from the correct place. If this is the case then the ion spot can
be re-positioned by mechanical adjustment of the ion source. Please note
that it is imperative to contact a Kratos engineer before moving the ion
source as it is possible to cause a significant amount of damage to the
ion source and/or the lens column. The following instructions assume
that the preceding section on imaging the ion spot (Section 5.7.1 on
page 149) has been read and that the ion spot is now visible in the FOV4
imaging mode.
1: It is first necessary to determine the analysis position in FOV4. Switch

the ion source to standby.
2: Turn on the X-ray source and note the position of the X-ray spot in the
imaging window.
3: Switch off the X-rays and switch the ion source back to On, making sure
that the raster is set to zero.
4: Make sure that the tuning section of the ion source control is visible,
5: Adjust the offset X and Y voltages to ensure that the ion spot is coincident
with the X-ray spot, Figure 25.

Ion source Tuning
select tuning button
Offset X Offset Y
FIGURE 25. Ion beam offsets.
N.B. If large offsets (negative or positive) are required to position the ion
spot then it is an indication of poor mechanical alignment of the ion source.
As the same electrodes (octapole deflection plates) are used to provide the
offset voltages and raster the ion spot, then large offset values can reduce
the raster size available. If this is the case then a warning message will be
displayed, Figure 26. This may not be a significant problem, however, as it
still may be possible to create a sufficiently large raster area.
Warning Message Large Offset Values

Ion source Tuning
FIGURE 26. Raster waveform clipped warning message.
5.7.3 Fine Adjustment of the Ion Beam Position and Crater Size
Using F.O.V. 4 to align the ion beam as described above is useful when the
beam is grossly misaligned, however, a different approach can be used
when the mechanical alignment of the gun is close to the analysis position
and the offsets required are relatively small. This approach is recom-
mended in most circumstances as there is no risk of damaging the detector
and alignment is more accurate, however, the procedure is more time con-
suming.
In essence this method involves etching a crater in a thin oxide sample and
then imaging the crater formed using parallel XPS imaging. The crater posi-
tion can then be adjusted using the X and Y offsets, see Section 5.5.3.9 on
page 140, a second crater etched then imaged and the process repeated
until the crater is at the centre of the parallel image.
Once aligned the spot may then be rastered to produce a crater. This ras-
tered crater can be imaged using parallel imaging and the crater size meas-
ured. The scale X and Y size, see Section 5.5.3.8 on page 140, may then
be adjusted to ensure that the crater produced is the size requested.
Follow the procedure outlined below to align the ion spot with the centre of
the image and adjust the raster size.
1: Load a suitable thin oxide sample. An example of such a sample is Ta

metal with a Ta2O5 thin film electrochemically grown on the surface. These
samples are commercially available (see the end of this chapter for likely
sources) or can be made reasonably easily. The sample should have a thin
oxide approximately 30 to 100 nm thick.
2: Place the sample at the analysis position and optimise the analysis
height.
3: Switch the ion gun to standby and switch the ion gun gas on, see
4: Set the raster size to zero, Section 5.5.1.7 on page 137.
5: Switch the ion gun on for approximately 60 seconds (depending on the

oxide thickness), then switch the ion gun back to standby.
6: Use the parallel imaging mode to image the crater formed in the oxide in
f.o.v.1. For example, if Ta2O5 is used then image at a binding energy of 22
eV (Ta 4f metal from the substrate is at 22 eV while Ta 4f oxide is at 27 eV).
It should be possible to see the crater as a bright area in the XPS image. If
the crater can not be seen then use the stitched imaging facility to record an
image over a larger area or etch the sample for longer in step 5.

Ion source Tuning
7: Modify the X and Y offsets to change the beam alignment. Refer to Fig-
ure 27 to see which way to move the beam. For example, it the crater
appears at the top of the image then increase both the X and Y offsets to
move the ion spot downwards.
FIGURE 27. Beam offsets.
8: Move the sample to a fresh area of sample and repeat the process. After
several iterations it should be possible to align the sample with the centre of
the imaged area.
9: To check the raster size move to a fresh area of sample.
10: Set the raster size to 2 mm, see Section 5.5.1.7 on page 137, and
switch the ion gun on for 20 minutes (more or less time may be required
depending on the ion beam conditions used).
11: Switch the ion beam off.
12: Record a stitched parallel image of the sample surface at 22 eV (if you
are using Ta2O5). For example, using f.o.v.1, a 5 x 5 stitched Ta 4f metal
image will produce an image of 4 x 4 mm total size. As this will record 25
images keep the acquisition time per image low, 10 seconds should be
enough. Typical equitation settings are shown below, Figure 28. An exam-
ple of the type of image recorded is shown below, Figure 29. Note that part
of two other craters can also be seen.

Ion source Tuning
stitched image
settings
FIGURE 28. Stitched image acquisition settings.

Ion source Tuning
FIGURE 29. Stitched image of the crater.
13: Measure the X and Y crater size from the image by dragging the mouse
across from one edge to the other while holding down the mouse button,
Figure 30.
Place the mouse pointer on one edge of the crater. Hold down the left mouse button
and drag the mouse pointer to the other edge of the crater. The length of the line is
displayed as r at the top of the image. In this example the length is 1.688 in the x
raster direction.
FIGURE 30. Measurement of crater size.
14: Calculate the correct X and Y scale using the following equation:
New scale value = (Old scale value / Measured size) x Requested size
In the above example the measured X size was 1.688 mm. The X scale
was 200 therefore the required new scale value is 237 volts. Note, the max-
imum scale value is 250 volts.
5.7.4 Tuning the beam
This section outlines a method for tuning the ion beam to produce a smaller
beam diameter or a larger ion flux. The instructions below assume that the
ion spot can be imaged and has been positioned to be coincident with the X-
ray spot, see Section 5.7.2 on page 151.
1: Switch the ion source gas on, see Section 5.6.1 on page 145.
2: Select the pre-set row to be turned in the ion source table and switch the
ion source to standby, see Section 5.6.2 on page 146.
3: Switch the ion source on.

Ion source Tuning
shield in position when the ion source is switched on).
5: Switch on ion source imaging, see Section 5.7.1 on page 149.
6: Turn on the sample current read-out by selecting the bias button, Figure 8
and clicking on the active button, see Section 5.5.5 on page 142.
7: Set the appropriate scale to read the ion beam current. As a guide the ion
current on the sample for beam energies of 2 kV and above should be
between 1 and 5 microamps. Lower beam energies produce correspond-
ingly lower ion currents.
8: Adjust the Condenser voltage and Focus voltage to minimise the spot
size or maximise the sample current as required, Figure 31.
Condenser Focus Align
FIGURE 31. Ion spot tuning.
9: When the required settings have been optimised, change the Align X volt-
age to maximise the measured sample current. Increasing the voltage on
the condenser lens (L2) will generally decrease the size of the ion spot at
the specimen. At a set beam energy, as the condenser voltage is increased
the focus voltage (L3) needed to produce a focused ion spot on the sample
will decrease.
10: To save the changes click on Update Row, Figure 32.
update row button restore row button
FIGURE 32. Saving changes.

Determining the Etch Rate
5.8. Determining the Etch Rate
The etch rate produced on a given sample will vary with beam energy,
extracted ion current and raster size. However, it is useful to characterise
the sputter rate of the ion source in a number on standard settings. This
can be achieved by etching a sample of known thickness. Such samples
can be readily purchased from a number of supplies:
Institute of Reference Materials and Measurements (IRMM), Retieseweg, B-

2440 Geel, Belgium. Tel: +3214571705, email: bcr.sales@irmm.jrc.be.
Standard Reference Materials, National Institute of Science and Technology

(NIST), 100 Bureau Drive, Stop 2322, Gaithersburg, MD 20899-2322, USA,
Tel: +1 3019756776, email: srminfo@nist.gov, web: http://ts.nist.gov/
Geller Microanalytical Laboratory, 426e Boston St, Topsfield, MA 01983-

1216, USA. Tel. +1 9788877000, email jg@gellermicro.com, web: http://
www.gellermicro.com

13 July 2009
Chapter 6
Floating Ion Gun
This chapter describes the alignment and operation of the floating ion gun.
The gun is intended for general sample cleaning and depth profiling experi-
ments. A floating mode allows the production of relatively high current, low
ion energy beams for superior depth resolution. The gun is under full com-
puter control enabling standard settings to be recorded and recalled for
future experiments. A general overview of the ion gun and associated elec-
tronics will be followed by an in depth description of the operation. Also
included is a section on the alignment of the ion beam with the analysis
position.
FIGURE 1. Floating Ion Gun.
163
Overview of Floating Ion Gun
6.1. Overview of Floating Ion Gun
This section is intended to provide an overview of the ion gun and associ-
ated electronics. The gun is designed to operate between 5 kV and less
than 100 V. Use inert gases only, Argon, Neon or Helium. The ion gun is
differentially pumped via the STC turbomolecular pump.
Differential pumping enables the pressure in the SAC to remain 104 times
lower than the pressure in the ion source. Below is a simplified schematic of
the floating ion gun, Figure 2.
FIGURE 2. Simplified schematic of the floating ion gun.
The ionisation chamber is separated from the main optics by a transfer lens.
Differential pumping is situated between the ionisation chamber and the
remaining optics (not shown in Figure 2). A bend in the ion optics between
the condenser lens (spot size lens) and the objective lens (focus lens)
removes neutral atoms from the ion beam. Alignment plates deflect the ions
around the bend. Following the focus lens a set of deflection electrodes are
used to scan the focused ion spot across the sample surface.
6.1.1 The Ionisation Chamber
Ions are formed by electron impact ionisation in the ionisation chamber, Fig-
ure 3. Two filaments are installed (only one shown) in the ionisation cham-
ber to increase the time between servicing.
164 Chapter 6 Floating Ion Gun

FIGURE 3. Schematic of the ionisation chamber of the floating ion gun.
During standard operation the walls of the chamber and the extraction elec-
trode are at earth potential (this is not the case in all modes, see
Section 6.1.4.2 on page 171). To aid explanation of the various potentials
applied in the ionisation chamber we will assume that the final ion energy
required is 4000 eV. In this situation the filament supply is at +3800 V with
respect to Earth potential.
Ionisation of the gas atoms inside the grid region is by bombardment with
electrons of typically 200 eV energy. The electrons are generated by the fil-
ament (by heating it with an electric current) and are accelerated through
the grid into the middle of the ionisation region. If the filament is at +3800 V
then the grid will be between 100 and 200 V positive with respect to it, in this
case we will assume the grid is 200 V positive with respect to the filament.
This means that the grid is at a potential of +4000 V with respect to Earth.
The ions produced within the grid are accelerated out of the ionisation
region by the extraction electrode (the extractor), Figure 3. The extraction
electrode has a negative potential with respect to the filament (for positive
ions). The extraction potential can be varied between 0 and -102 V with
respect to the filament. In this case the negative extractor potential is -35 V.
This means that the potential on the extractor is +3765 V with respect to
earth.
In standard operation the accelerating electrode will be at Earth potential.

Therefore, in this case we have the following potentials with respect to
Earth, Table 1 and Figure 4.
Chapter 6 Floating Ion Gun 165

TABLE 1. Electrode voltages with respect to Earth
Electrode Potential (V)

Filament +3800
Grid +4000
Extractor +3765
Accelerating 0
FIGURE 4. Electrode voltages of the ion source for a 4 kV ion beam energy.
The actual energy of the ion beam emerging from the accelerating electrode
is 4000 eV (filament potential + grid potential). The voltages on the filament
and extractor are set approximately equal so that the extractor does not
effect the movement of electrons towards the grid.
6.1.2 Ion Beam Stabilisation
The ion beam is stabilised so that a constant ion current leaves the ion gun.
The current of ions reaching the extraction electrode is maintained at a fixed
value by varying the filament current. This negative feedback loop ensures
that a constant etch rate can be maintained for a period of time even if the
argon gas pressure varies by small amounts during the experiment.

Active stabilisation of the extraction current is only possible within a range of

values. A filament current limit is present to prevent the filament melting. If
the source conditions change to such an extent that the heating current of
the filament increases to this value then active stabilisation of the extraction
current will cease. There is also a maximum electron emission current of 30
mA. This limitation prevents heat generated within the source reaching
damaging levels. Thus when an emission current of 30 mA is reached the
current through the filament is limited and active stabilisation of the extrac-
tion current again ceases.
6.1.3 Ion Optics
The ionisation chamber, extraction electrode and the acceleration electrode

provide a small source (approximately 1 mm diameter) of energetic ions.
The energy spread is low and the actual energy depends on the beam volt-
age and the grid voltage, see Section 6.1.1 on page 164.
The purpose of the ion optics is to provide a final beam of ions of a suitable
diameter and of a suitable current to enable controlled ion etching of the
sample. For rapid etching and sample cleaning a high energy beam (1 - 5
keV) and high ion current (usually a few micro Amps) is used. To reduce
crater edge effects the ion beam is focused to a narrow diameter and elec-
trostatically scanned across the sample surface. For delicate or multi-layer
samples low ion energies are used to minimise chemical damage of the
substrate and ion bombardment induced mixing of layers. An outline of the
ion optics is shown schematically below, Figure 5.
FIGURE 5. Schematic of the ion gun optics.

The beam from the ionisation chamber and accelerating electrode is first
focused by the adaptor lens L1. This lens adapts the source region to the
rest of the optics and provides a volume in which the differential pumping
pumps the gas away from the source to maintain good vacuum in the rest of
the optics. The ion beam passes through an aperture before entering the
condenser lens L2. The purpose of this lens is to reduce the diameter of the
ion beam and to focus it before or into the next aperture.
The shorter the focal length of the condenser lens (L2), the smaller the
beam approaching the final lens and the smaller the current in the final ion
beam from the gun. The highest ion currents are achieved with the con-
denser lens focusing the ion beam into the back focal plane of the final
focusing lens (L3) where the final beam defining aperture (A2) is situated,
Figure 5.
Prior to the beam entering the aperture it passes through a pair of alignment
plates A1 and A2, which deflect the beam through a small angle (5
degrees), Figure 5. The purpose of this bend is to remove neutral atoms
from the ion beam. These fast neutrals are formed by charge transfer colli-
sions when the ion beam passes through regions of relatively high pres-
sures (i.e. at the exit of the ionisation chamber). An energetic ion may
interact with a residual gas atom losing an electron to become an energetic
neutral atom and leaving a low energy positive ion.
Because of the charge neutralisation process (which has a significant prob-

ability at pressures above 10-6 torr) the ion beam from the source region will
always have a small percentage of energetic neutrals. The deflection plates
A1 and A2 deflect the ion beam into the final lens whilst the energetic neu-
trals are not deflected and are lost from the beam.
The ion beam is brought to a focus on the sample by the final focus lens L3,
Figure 5. This lens is a low aberration electrostatic lens which is followed by
a set of deflector plates configured as an electrostatic octopole. These
deflection plates are used to scan the ion beam across the sample surface.
The octopole arrangement ensures that the final raster traced out be the ion
beam is distortion free.
The ion optics can be floated on a positive potential of up to 2 kV. There

are metallic, electrically isolated, screens between the various lenses so
that the ion beam does not come into contact with the earthed potential of
the vacuum enclosure of the ion gun. The floating mode is designed to
improve the ion current of the gun when low energy beams are required. It
is possible to use the gun down to output beam energies of 50 eV in the float
mode.
6.1.4 Configuration of the Ion Optics for Different Applications
The ion optics are operated under different conditions for different applicat-
ins. This section reviews the different ion beam trajectories through the ion
optics for the various modes of operation.

6.1.4.1 Rapid Depth Profiling
When a relatively thick layer (hundreds of nm) needs to be removed and

inter-layer resolution is of secondary importance it is advisable to use a high
energy ion beam. This has the advantage of allowing a fast depth profile
over a well defined small area. The higher the beam energy the more rap-
idly the specimen is eroded away for a given beam current density. This is
because the sputtering coefficient (nominally the number of sputtered atoms
eroded from the surface per incident ion) is greater for higher bombardment
energies. At relatively high beam energies (ca 4 keV) more ion current can
be delivered and smaller beam diameters are achieved. The brightness of
the source (expresses as the current per unit area of the source into unit
solid angle (Amp/cm2/sr) is higher for higher accelerating volts. Also the
chromatic aberration at higher beam energies is smaller because the spread
of ion energies from the source is small compared with the overall beam
energy.
The standard running conditions for a fast depth profile are a beam energy
of 4 keV, the condenser lens (L2) focused into the back focal plane of the
focus lens (L3) and the focus lens focusing the beam on the specimen. No
float voltage is required. The beam will be rastered by the octopole deflec-
tion assembly, Figure 5. The ion trajectories in the ion gun are shown sche-
matically in Figure 6 and the typical voltages applied to the various lenses
are indicated.
Ionisation L1 (adapter alignment and

L2 (condenser
Chamber lens) lens) neutral trap
A1 L3 (focus)
Octopole
A2
0V 2750 V
+4 kV (preset) 0V
(earth) 2550 V 0V Raster
(nominal) (earth) (earth)
FIGURE 6. Running conditions of the ion optics for fast depth profiling. N.B. a raster is used and
the condenser is focused in the back focal plane of the final lens or slightly stronger.

The ion beam is scanned in a square raster over the specimen surface. The
size of the raster should ideally be 10 times larger than the XPS sampling
area, Figure 7.
acceptance cone of spectrometer
rastering ion beam

ion beam etch pit
sample surface
Specimen
FIGURE 7. Schematic of the ion beam depth profiling experiment.
Rastering the ion beam in this way ensures that the XPS spectra are repre-
sentative of the middle of the square etch pit and not of the edge where the
ion beam may have caused uneven etching (edge effects), Figure 8. N.B.
obviously the ion beam centre needs to be well aligned with the analysis
position so that spectra are recorded from the centre of the etch crater, see
section Section 6.4.2 on page 191.

FIGURE 8. Schematic diagram illustrating the edge effects in a rastered ion etch pit. The
analysis area should coincide with the dark grey area in the centre of the etched
hole.
6.1.4.2 Low Energy Depth Profiling and the floating mode
For extremely thin layers, or many layered samples, low ion energy depth
profiles may be preferred. Any ion beam energy under 1000 eV can be con-
sidered to be low energy. Low energy bombardment reduces knock-on
effects where mixing up of the sample atoms by the incoming ions
degrades interface resolution. Preferential sputtering of lightweight compo-
nents can also be reduced using lower beam energies.
As the energy of the ion beam from a conventional ion source is lowered so
the available beam current falls. This is because the brightness (current
from unit area of the source per unit solid angle) of the source reduces with
reducing beam energy. The chromatic aberration increases because the
energy spread from the source becomes significant when compared with
the beam energy. In addition, the susceptibility of a low energy beam to
stray magnetic fields is larger. In order to improve the low energy perform-
ance the beam after leaving the ionisation chamber and extractor is acceler-
ated into the next optics which are floated at a potential of approximately 2

kV. This gives the ion beam a higher energy through the adapter and con-
denser lenses as well as part of the way into the focus lens.
This acceleration causes the beam to suffer less from chromatic aberration
in the adapter and condenser lenses as well as making the beam less sus-
ceptible to stray magnetic fields. Typical lens voltages applied when run-
ning in the floating mode are shown below, Figure 9.
Ionisation L1 (adapter L2 (condenser alignment and

chamber lens) lens) neutral trap
A1 L3 (focus)
Octopole
A2
-250 V -2000 V (preset) -2000 V 1500 V -2000 V
(float) (float) (float) 1400 V Raster
0V
(earth)
FIGURE 9. The optics of the ion gun when it is working at low ion beam energies in the floating
mode. The above shows the various electrode voltages for a final beam energy of
250 eV.
The ion beam is decelerated by an electrode at the end of the ion column
back to the original ion energy.
6.2. Manual Software Interface
Manual control of the ion gun is possible using the ion gun interface in the
manual window. Scroll down to near the bottom of the manual control win-
dow, Figure 10.

Off Standby On Degas
Controls Bias Table Status Tuning Degas
FIGURE 10. Ion gun section of manual window.
To view the ion gun controls, sample current measurement (bias), table of
stored values (table), current ion gun status (status) and ion gun settings
(tuning) click on the relevant button.
Once operating conditions have been chosen and argon gas has been intro-
duced into the instrument the ion gun can be switched to standby then to
on manually by clicking on the respective buttons. An automated degas
sequence for the ion gun filament is included for use after the machine has
been let up to atmosphere. This procedure gently increases the current
through the filament to slowly remove surface contamination, see
6.2.1 Ion Gun Controls
Click on Control button to open the manual control section, Figure 11.
Source HT Extractor / Emission Toggle Extractor or Emission Current Float Voltage
Beam
Energy
Raster Size Compucentric rotation Etch Rate Current Density

on / off
FIGURE 11. Ion gun controls

6.2.1.1 Source High Tension (HT)
The source high tension in kilovolts is set in this box. It can be varied
between 0.05 kV (50 volts) and 4.8 kV. N.B. this value is the voltage of the
filament with respect to earth and not the beam energy when it leaves the
ion gun, see below.
6.2.1.2 Extractor / Emission Toggle and Extractor or Emission Current
The toggle button switches the ion gun between extractor current control
and emission current control. In extractor mode the ion gun monitors the
current of ions reaching the extraction electrode. This extractor current then
forms the basis of the filament current control circuit, see Section 6.1.2 on
page 166. When emission is selected the filament current is adjusted to
give a constant electron emission current (measured between the filament
and collector). Extractor current control is directly related to the ion current
at the sample whereas under emission control the actual ion current reach-
ing the sample is also dependent on the gas pressure in the ion source. For
this reason the floating ion gun is usually set to run in extractor stabilisation
mode.
The actual ion extraction current (or electron emission current) required is
set in the current box. Values of extractor current can range from 0 to 150
uA and values for the emission current can be adjusted between 0 and 30
mA.
The float voltage in volts is set in this box. Usually a float of 2000 volts is
used but the value can be varied between 0 and 2000 volts as long the sum
of the float voltage and source HT remains less than 5 kV.
6.2.1.4 Beam Energy
This is a read back of the actual ion energy (singly charged ions only) leav-
ing the ion gun. Details of how this value is calculated can be found in
6.2.1.5 Etch Rate
The etch rate in Angstroms per minute expected for the current ion gun set-
tings is displayed here.
6.2.1.6 Sample Current
The ion current expected to reach the sample is given here. N.B. the cur-
rent given assumes no affects from secondary electron / ion emission or
charging problems.
6.2.1.7 Raster Size
This setting controls the size of the crater (mm x mm) formed by rastering
the ion beam across the sample surface. The raster pattern is formed by

applying a saw toothed voltage pattern on to the octapole deflection plates

(Figure 5).
6.2.1.8 Compucentric Rotation on/off
This control allows the user to select whether or not compucentric rotation
during the etch cycle take place. This enables an off-axis sample to be
rotated about the analysis position during etching thereby improving the
quality of depth profiles. For compucentric rotation to work the sample must
be mounted on the specially designed azimuthal rotation platen and the axis
of rotation must have been previously defined.
6.2.2 Ion Gun Table
Click on the table tick box to open a table with a list of presets for the ion
gun, Figure 12. Values stored in the table can be recalled into the ion con-
trol section. Therefore, during standard operation of the ion gun, the user
does not have to enter values for every ion gun parameter. Furthermore,
custom settings and changes to the preset values can be saved for future
use.
Compucentric rotation
on / off
Update row
Restore row
Preset row
Name
Scroll bar
Table Controls Acceleration HT Extractor Current Beam Current at 50 uA

Extraction current
FIGURE 12. Ion gun preset table.

6.2.2.1 Update Row
Updates the current row over-writing the existing values with the current ion
gun settings. N.B. if this button is inadvertently pressed important settings
can be over written. If this happens close Vision2 without saving the config-
uration file and restart.
6.2.2.2 Restore Row
Restores the values in the selected table entry to the control section. For
usage instructions see Section 6.4.4 on page 197.
6.2.2.3 Preset Row
The preset row stores the lens settings for each operating mode. For each
mode the Acceleration voltage, Extractor current and standard Beam cur-
rent are displayed to aid identification. The preset row name is editable.
6.2.3 Tuning
Click on the Tuning tick box to open the ion gun tuning section, Figure 10.
This section allows manual control of lens voltages and other settings. The
values are entered automatically when a preset row from the table is
restored, see above. The various controls can be modified by moving the
slider bar or entering the new number directly in the box, Figure 13.
Filament selector Filament Current Limit Grid Voltage Extractor Voltage

Condenser Focus Align X Align Y
Scale X Scale Y Offset X Offset Y

Max FSD
FIGURE 13. Manual ion gun tuning section.

6.2.3.1 Filament selector
The ion gun is fitted with two tungsten filament to increase the interval
between servicing the ion source. The filament currently in use can be
changed manually with this control. The selected filament is used regard-
less of which Pre-set row is selected. N.B. if the spare filament is selected
then it is important that it is degassed thoroughly before use, see below.
6.2.3.2 Filament Current Limit
The filament current limit sets the maximum current that can pass through
the selected filament. The value chosen is usually slightly higher than the
current required to reach maximum electron emission. As the filament ages
this value may need to be increased to ensure that it is not limiting the max-
imum emission.
The grid voltage control sets the voltage on the grid with respect to the fila-
ment as described in Section 6.1.1 on page 164. The voltage can vary
The extractor control sets the voltage on the extraction electrode with
respect to the filament as described in Section 6.1.1 on page 164. The volt-
age can take any value between 0 and 102 volts.
6.2.3.5 Condenser
The condenser control sets the voltage on the condenser lens (L2, Figure
5). This lens is adjusted to change the size of the final ion spot on the spec-
imen, see Section 6.1.3 on page 167. It can be varied between 0 and 5000
volts.
6.2.3.6 Focus
The focus control set the voltage on the focus lens (L3, Figure 5). This lens
focus the ion spot on the specimen, see Section 6.1.3 on page 167. The
focus voltage can be varied between 0 and 5000 volts.
6.2.3.7 Align X.
As described in Section 6.1.3 on page 167 the ion gun has a 5 degree bend
used to remove energetic neutrals from the ion beam. This control sets the
voltage on the alignment plates A1 and A2 (see Figure 5) used to deflect the
ion beam around the bend. The voltage can be varied between 0 and 250
volts.
6.2.3.8 Scale X and Y
The size of an etch crater is determined by the Raster size control,

Section 6.2.1 on page 173. However, as the ion gun is not mounted normal

to the sample surface simply rastering the beam by equivalent amounts in

both the X and the Y directions would result in rectangular etch craters. The
scale controls add scaling factors to the voltages applied to the octapole
deflection plates (Figure 5) to ensure that a square etch crater is formed.
The scaling factors can be varied between 0 and 200 volts.
These values directly effect the size of the etch crater produced and there-
fore should be set as close to the maximum value as possible.
6.2.3.9 Offset X and Y
Fixed voltage offsets can be applied to the octapole deflection plates (Figure
5) to fine tune the position of the ion spot relative to the analysis position.
Voltages between -110 and +110 may be applied to the deflection plates to
account for any mechanical misalignment of the ion gun with the analysis
position. However, it should be noted that these alignment voltages should
be kept as low as possible as they may effect the maximum raster size
available. If this is the case a warning message will appear displaying the
text WARNING: Raster waveform clipped.
6.2.3.10 Max FSD
The Maximum Full Scale Deflection is measured in mm and is the maximum

crater size available. It can be varied between 0 and 6 mm depending on
the set up conditions of each ion gun.
6.2.4 Status
Click on Status tick box to open the ion gun status read-backs, Figure 10.
This section displays the current status of the ion gun, Figure 14.
Source HT Filament current Extractor Volts Extractor Current

Float Voltage Grid Voltage Condenser (L2) Focus (L3)
Voltage Voltage
Alignment X1 Alignment X2 Emission Current
FIGURE 14. Ion gun status read-backs

6.2.4.1 Source HT
This read-back displays the high voltage applied to the ion gun. It will read 0
unless the ion gun is set to On. N.B. if a pre or post etch delay is set in the
manager window then the High voltage will be set to on during the delays
but the alignment voltages will be set to maximum to prevent ions reaching
the sample surface.
6.2.4.2 Filament
The filament read-back displays the present filament current. When the ion
gun is set to off the filament current will fall to zero. If the ion gun is in the
standby or the on state then the filament current will be varied automatically
to produce the requested ion extraction current, see Section 6.1.2 on
page 166. The filament current cannot exceed the filament current limit
(Section 6.2.3 on page 176).
This reads back the actual extraction voltage relative to the filament applied
to the ion source.
6.2.4.4 Extractor Current
The extractor current read back displays the ion current reaching the extrac-
tion electrode in micro amps, see Section 6.1.2 on page 166. The filament
current is adjusted using a negative feedback loop arrangement to keep this
value constant and hence ensure a constant ion current leaving the ion
source. The extraction current is stabilised when the ion gun is set to
standby or on. Effective stabilisation is only possible over a narrow pres-
sure range and two limiting factors can prevent the correct extractor current
being reached. The first of these is the filament current limit (Section 6.2.3.2
on page 177). If the filament current reaches the limit then effective control
of the ion extraction current will cease. The second limiting factor is the
electron emission current from the filament. This value is limited to 30 mA to
protect the ion source from excessive internal temperatures. If the emission
current reaches this value then effective control of the extraction current will
stop.
The voltage applied to internal metal elements of the ion gun during low
energy depth profiles (see Section 6.1.4.2 on page 171).
Read back of the voltage applied to the extractor grid in the source region of
the ion gun, Figure 3.
6.2.4.7 Condenser
The voltage applied to the condenser lens (lens L2), Figure 5.

6.2.4.8 Focus
Read back of the voltage applied to the focus lens (lens L3), Figure 5.
6.2.4.9 Alignment X1 and X2
Displays the voltage applied to the beam alignment plates (A1 and A2, Fig-
ure 5). These voltage are set to high values when the ion gun is set to
standby and during pre and post etch delays. This is to reduce the possibil-
ity of ions reaching the specimen when etching is not required.
6.2.4.10 Emission Current
This reads back the present electron current between the filament and the
collector. The filament current is limited automatically so that this value
does not exceed 30 mA.
6.2.5 Bias Current
Click on Bias to open the bias current section, Figure 10. When active the
bias current section allows the sample current (i.e. current of ions or elec-
trons reaching or leaving the sample platen) to be read. Two modes are
available, Measure sample current and Measure ion beam current. Toggle
between them by left mouse clicking on the setting, Figure 15 and Figure
16.
Switch on and off by clicking on Active Select mode by clicking on this button
Set range of read-back by clicking on this button Sample current display
FIGURE 15. Bias Current read back.
Select mode by left clicking on either row
FIGURE 16. Sample current and ion beam current modes.

The sample current mode measures the sample current directly while the
ion beam mode places a 30 volt positive bias on the sample platen while
active. This bias voltage reduces the number of secondary electrons leav-
ing the sample and hence gives a more reliable reading of the actual ion
current reaching the sample. N.B. Sample or ion currents can only be
measured on conducting samples in electrical contact with the platen.
To change the scale on the read out click on the range button, Figure 15 and
Figure 17. Three read-back ranges are available, up to 20 nA, up to 2 uA
and up to 200 uA.
Left click on value to set meter range
FIGURE 17. Meter range.
6.2.6 Degas
Click on Degas tick box to open the ion gun filament degas section, Figure
10. The degas option allows the user to slowly increase the current passing
through the selected filament in order to gently degas it. If the inside of the
vacuum chamber has been exposed to the atmosphere or the ion gun hasnt
been used for some time then the filaments will be contaminated. Ramping
the filament current up in a controlled manner allows the filament to warm
up gradually and contaminates are driven off slowly. This increases the fila-
ment lifetime by reducing surface damage of the filament.
can be set for larger values, Figure 18.
Regime 1, ramp time Regime 1, final current
Regime 2, ramp time Regime 2, final current

FIGURE 18. Degas settings.
To change the degas settings follow the instructions outlined below:
1: Enter a time in minutes into the regime 1, ramp time box (dont forget to
press return). A suitable value would be 10 minutes.
2: Enter a current setting in the regime 1 current box (e.g. 2 Amps).
3: Next enter a second time into regime 2 ramp box (e.g. 10 minutes).
4: Finally enter a second current setting into the regime 2 current box (e.g.
2.3 Amps). N.B. the final current setting should not exceed the filament
limit set for the selected filament, see Section 6.2.3 on page 176.
Before beginning the degas procedure it is advisable to open the ion

gun differential pumping valve (V2), see Chapter 3. When the settings
have been entered to start the filament degas procedure left click on the
Degas On light, Figure 19.
Left click here to start the degas procedure
FIGURE 19. Degas On control.
Once on is selected the filament current will increase from 0 to the value set
in regime 1 in the entered time. After this time has elapsed the filament cur-
rent will continue to rise for the time entered in regime 2 reaching the maxi-
mum current value entered in regime 2.
6.2.7 Pneumatic Sputter Shield (optional)

Where the hardware is configured for the pneumatic sputter shield the ion
gun control section of the manual window will include a sputter shield radio
button as shown in Figure 21 Under normal use the sputter shield will
change to the in state (i.e. the sputter shield moves across to protect the
bottom of the electrostatic lens column) when the ion gun is switched on.
When the ion gun returns to standby or off the sputter shield will retract.
Selecting the sputter shield radio button will display the manual sputter
shield control section of the ion gun control allowing the user to move sput-
ter shield either to the in or out position manually. By selecting the man-
ual override which removes automated control of the sputter shield the

sputter shield will remain in the state defined by the user during an auto-
mated acquisition.
A scrolling text box within the vacuum mimic diagram section of the manual
window, shown in Figure 21, is used to display messages relating to the
sputter shield status.
FIGURE 20. Scrolling text box with sputter shield message
FIGURE 21. Ion gun section of the Manual Window
6.3. Standard Manual Operation
This section describes the normal manual operation of the floating ion gun.
It is assumed that the ion gun has been installed and a table of standard
operating conditions created. Furthermore, it is also assumed that the ion
gun has been correctly aligned with the analysis position. For alignment
instructions see Section 6.4.1 on page 189. Manual operation of the ion

gun is defined as switching the gun on from the manual window. For auto-
mated depth profiling the ion gun is controlled from the instrument manager
window.
6.3.1 Starting the flow of Argon
Before setting the ion gun to standby the argon gas must be introduced into
the ionisation source. The procedure below assumes that the leak valve
has previously been set to the correct pressure. Follow the instructions
below to switch on the argon gas:
1: Bring up the manual window, scroll down to the Vacuum control section
and select Automatic Sequences, Figure 22.
2: Check that the STC pressure is below 1 x 10-6 mbar and that the SAC
pressure is below 5 x 10-7 mbar.
3: Check that the SAC-STC value is closed and that the ion gun differential
pumping value (V2) is closed.
4: Click on the Ion Gun Gas On automatic sequence, Figure 22.
Ion gun gas on Ion gun gas off
FIGURE 22. Automatic vacuum sequences.
5: This automated sequence opens the ion gun differential pumping value
(V2) and the Argon gas inlet valve (V8), see Section 3.1.6 on page 44.

6: The pressure in the STC should increase to approximately 1 or 2 x 10-6

mbar.
6.3.2 Switching the ion gun on
This section describes switching the ion gun to standby from off then switch-
ing the ion gun on. It assumes that the Argon gas pressure has been set
according to the above procedure, Section 6.3.1 on page 184.
1: Scroll down the manual window to the ion gun section, click on the follow-
ing tick boxes: Controls; Status; and Table, Figure 23.
Ion Gun off Standby On Degas
Controls Table Status
FIGURE 23. Ion Gun control buttons.
2: Select the required ion gun operating conditions by left clicking on the rel-
evant row in the table so that it becomes highlighted.
3: Click on the Restore Row button to download the saved ion gun settings
from the table to the ion gun control, Figure 24. Parameters down-loaded
from the table include: Source HT; Extractor current; Float voltage; Con-
denser (L2) voltage; Focus (L3) voltage; Align X; and Align Y.

Left click on the Restore Row button to download the stored settings
to the Ion Gun control
Left click in the table to highlight the required row
FIGURE 24. Restore Ion Gun saved settings.
4: Left click on the Standby button, Figure 23, to set the ion gun to Standby.
On pressing the Standby button the software begins to slowly ramp up the
filament current. The filament current will continue to rise until one of three
limiting factors are reached: 1, the requested ion emission current is
achieved (see Section 6.1.2 on page 166); 2, the filament software current
limit (usually set between 2.4 and 2.8 amps); 3, the electron emission cur-
rent limit (30 mA). It may take up to 10 minutes for the correct ion current to
be reached and the read-back value may well overshoot the set value until
proper control is established. If the requested ion emission current is not
reached it may be due to insufficient gas pressure. Increase the pressure
by turning the leak valve anti-clockwise to allow more Argon gas to enter the
ionisation chamber. The STC pressure can be varied between 8 x 10-7
mbar and 3 x 10-6 mbar.
5: Once the set ion current emission current has been reached and has sta-
bilised left click on the On button, Figure 23, to switch the ion beam on. The
set HT will be applied and the align X1 and X2 voltages will also assume
their set values.

6.3.3 Using Rotation
The rotation device enables up to two samples to be rotated about the anal-
ysis position during ion etching. This rotation improves interfacial resolution
of multilayer samples by reducing ion induced roughening of the sample
surface.
For rotation to work the sample must be mounted on the rotation bar and the
axis of rotation of the bar must be moved to the analysis position. Align the
area of interest up with the analysis position by manually switching on the
sample rotation and positioning the centre of rotation using the optical cam-
era (assumes the camera has been well aligned with the analysis position).
Note that the rotation bar places the samples much higher in the instrument
than the plane bar, therefore, the stage position will need to be lowered by
between 1.5 and 2 mm. When the ion gun is switched On the sample will be
rotated about the analysis position.
6.3.4 Switching the ion gun off
Follow the instructions below to manually turn the ion beam off.
1: If the ion gun is to be used again in the near future then it can be left in the
standby mode with the gas on. Click on the Standby button, Figure 23. This
sets the ion gun to the standby state.
2: If the ion gun is not to be used for some time or the Argon gas is to be turn
off then the ion gun must be switched off. Click on the Off button (the ion
gun can be switched to off from the On state or the Standby state), Figure
23. When set to off the HT is set to zero (if on) and the filament current is
ramped down to zero which reduces the ion and electron emission currents
to zero.
3: The Argon gas can now be switched off. Scroll down to the Vacuum Con-
trol section and click on the Ion Gun Gas Off Automatic Sequence, Figure
25. N.B. if the Argon gas supply is switched off while the ion gun is
switched to On or Standby then the filament current will increase to
the software filament current limit. While this may not necessary dam-
age the filament the situation should be avoided in normal operation.
The sequence automatically closes the Argon gas inlet valve (V8) followed
by the Backing valve (V3). The Argon gas line pumping valve (V9) opens to
pump the Argon gas line out between the leak valve and Argon gas inlet
valve (V8) using the rotary pump. After a set time the Argon gas line pump-
ing valve (V9) closes and the backing valve opens (V3). Finally the ion gun
differential gas pumping valve is closed to complete the sequence.

Ion Gun Tuning
Ion gun gas off
FIGURE 25. Ion Gun Gas Off sequence.
6.4. Ion Gun Tuning
This section describes tuning of the ion beam size and focus at the speci-
men and how to align the ion beam at the analysis position. It should be
noted, however, that several ion gun operating conditions will have been
determined by the Kratos engineer and stored in the ion gun table, see
Section 6.2.2 on page 175. These notes are included in case the user has a
particular application which is not covered by the standard settings or if the
ion gun needs to be re-aligned for any reason. Before commencing a
detailed description of how to tune the ion gun a few general points about
tuning will be considered.
Increasing the voltage on the condenser lens (L2) will generally decrease
the size of the ion spot at the specimen. At a set beam energy, as the con-
denser voltage is increased the focus voltage (L3) needed to produce a
focused ion spot on the sample will decrease. As the condenser voltage is
reduced at a given beam energy then the focus voltage (L3) will increase.

Ion Gun Tuning
Generally the smaller ion spot sizes at the specimen are achieved at the
higher beam energies. The minimum beam diameter at 4 kV is usually
between 200 and 250 microns.
6.4.1 Imaging the ion spot
It is extremely useful to be able to image the ion spot in real time during the
alignment process. To accomplish this a separate electrostatic lens mode is
enabled which has a large field of view allowing the ion spot to be easily
located and its position adjusted. This lens mode is labelled Field of View 4
and should have been set up by the installation engineer. If it is not present
on your system then please consult Kratos.
N.B. Imaging the ion spot for prolonged periods or at high intensities
can damage the channel plate detectors. For this reason time imaging
the ion spot should be kept to a minimum, imaging high resolution
mode should always be used (to ensure that the iris is at its smallest
setting) and steps should be taken to reduce the number of secondary
electrons produced (e.g. by decreasing the extractor current setting to
10 or 20 uA).
Typical lens values for Field of View 4, FAT 160 are tabulated below,
Table 2.
TABLE 2. Field of View 4, FAT 160 lens values (blank entries indicated that there is no
lens function at that kinetic energy).
Kinetic
Energy Lens1 Lens2 Lens4 Lens5 Lens6 Lens7 Magnet
0 0 0 0 0 0 0 0
50 311 23.3
100 704 50.2
160 0
200 1261 101
350 2191 247
600 3511 467
900 5186 722
1169 6922 968
1500 8381 1227
3000 2840
5000 1 1 10000 1 3000 3000 0
Using this lens mode it should be possible to image the ion spot in real time.
To do this follow the procedure outlined below:

Ion Gun Tuning
1: Position an area of the platen which has no sample mounted on it at the

XPS position and set it to the correct analysis height.
2: Go to the Parallel XPS imaging section of the Manual window. Select

running integral with an integration time of 5 seconds and a refresh time of
0.25 seconds, Figure 26.
3: Change the analysed energy to kinetic energy and select a low energy to
image, e.g. 400 eV, Figure 26.
On Off Imaging Mode Integration Time Refresh Time
Analysed
Energy
Energy Reference
Kinetic or Binding Energy
Analyser Mode Lens Mode Pass Energy Aperture / Iris Setting
FIGURE 26. Ion spot imaging.
4: Select Imaging for the analyser mode, Field of View 4 for the lens mode,
Pass Energy 160 and Imaging high resolution (sometimes labelled Imaging
dia3mm), Figure 26.
5: Restore the ion gun settings which are to be tuned by clicking on Restore
Row, Figure 24.
6: Start the argon gas flow, see Section 6.3.1 on page 184.
7: Switch the ion gun to standby and wait for the requested ion extraction
current to be reached, see Section 6.3.2 on page 185.
8: Set the raster size to zero, Figure 27.

Ion Gun Tuning
Raster Size
FIGURE 27. Raster size.
9: Switch the ion gun on, see Section 6.3.2 on page 185.
shield in position when the ion gun is switched on).
11: Switch the parallel imaging to On, Section 26 on page 190. This should
open up a section in the bottom left hand side of the real time window. If the
image fails to appear then it may be necessary to increase the size of the
imaging section, in the real time display, by left clicking on the divider tab
and dragging out the tab to make the section larger.
6.4.2 Positioning the Ion Spot
If the ion gun is mechanically well aligned to the analysis position then the
ion spot should now be visible in the imaging window. However, if the ion
gun has been moved mechanically it is possible that it could be pointing well
away from the correct place. If this is the case then the ion spot can be re-
positioned by mechanical adjustment of the ion gun. Please note that it is
imperative to contact a Kratos engineer before moving the ion gun as
it is possible to cause a significant amount of damage to the ion gun
and/or the lens column. The following instructions assume that the pre-
ceding section on imaging the ion spot (Section 6.4.1 on page 189) has
been read and that the ion spot is now visible in the FOV4 imaging mode.

Ion Gun Tuning
1: It is first necessary to determine the analysis position in FOV4. Switch

the ion gun to standby.
2: Turn on the X-ray source and note the position of the X-ray spot in the
imaging window.
3: Switch off the X-rays and switch the ion gun back to On, making sure that
the raster is set to zero.
4: Make sure that the tuning section of the ion gun control is visible,
5: Adjust the offset X and Y voltages to ensure that the ion spot is coincident
with the X-ray spot, Figure 28.
Offset X Offset Y
FIGURE 28. Ion beam offsets.
N.B. If large offsets (negative or positive) are required to position the ion
spot then it is an indication of poor mechanical alignment of the ion source.
As the same electrodes (Figure 5, octapole deflection plates) are used to
provide the offset voltages and raster the ion spot, then large offset values
can reduce the raster size available. If this is the case then a warning mes-
sage will be displayed, Figure 29. This may not be a significant problem,
however, as it still may be possible to create a sufficiently large raster area.

Ion Gun Tuning
Warning Message Large Offset Values
FIGURE 29. Raster waveform clipped warning message.
6.4.3 Fine Adjustment of the Ion Beam Position and Crater Size
Using F.O.V. 4 to align the ion beam as described above is useful when the
beam is grossly misaligned, however, a different approach can be used
when the mechanical alignment of the gun is close to the analysis position
and the offsets required are relatively small. This approach is recom-
mended in most circumstances as there is no risk of damaging the detector
and alignment is more accurate, however, the procedure is more time con-
suming.
In essence this method involves etching a crater in a thin oxide sample and
then imaging the crater formed using parallel XPS imaging. The crater posi-
tion can then be adjusted using the X and Y offsets, see Section 6.2.3.9 on
page 178, a second crater etched then imaged and the process repeated
until the crater is at the centre of the parallel image.
Once aligned the spot may then be rastered to produce a crater. This ras-
tered crater can be imaged using parallel imaging and the crater size meas-
ured. The scale X and Y size, see Section 6.2.3.8 on page 177, may then
be adjusted to ensure that the crater produced is the size requested.
Follow the procedure outlined below to align the ion spot with the centre of
the image and adjust the raster size.
1: Load a suitable thin oxide sample. An example of such a sample is Ta

metal with a Ta2O5 thin film electrochemically grown on the surface. These
samples are commercially available (see the end of this chapter for likely
sources) or can be made reasonably easily. The sample should have a thin
oxide approximately 30 to 100 nm thick.

Ion Gun Tuning
2: Place the sample at the analysis position and optimise the analysis
height.
3: Switch the ion gun to standby and switch the ion gun gas on, see
4: Set the raster size to zero, Section 6.2.1.7 on page 174.
5: Switch the ion gun on for approximately 60 seconds (depending on the

oxide thickness), then switch the ion gun back to standby.
6: Use the parallel imaging mode to image the crater formed in the oxide in
f.o.v.1. For example, if Ta2O5 is used then image at a binding energy of 22
eV (Ta 4f metal from the substrate is at 22 eV while Ta 4f oxide is at 27 eV).
It should be possible to see the crater as a bright area in the XPS image. If
the crater can not be seen then use the stitched imaging facility to record an
image over a larger area or etch the sample for longer in step 5.
7: Modify the X and Y offsets to change the beam alignment. Refer to Fig-
ure 30 to see which way to move the beam. For example, it the crater
appears at the top of the image then increase both the X and Y offsets to
move the ion spot downwards.
FIGURE 30. Beam offsets.
8: Move the sample to a fresh area of sample and repeat the process. After
several iterations it should be possible to align the sample with the centre of
the imaged area.

Ion Gun Tuning
9: To check the raster size move to a fresh area of sample.
10: Set the raster size to 2 mm, see Section 6.2.1.7 on page 174, and
switch the ion gun on for 20 minutes (more or less time may be required
depending on the ion beam conditions used).
11: Switch the ion beam off.
12: Record a stitched parallel image of the sample surface at 22 eV (if you
are using Ta2O5). For example, using f.o.v.1, a 5 x 5 stitched Ta 4f metal
image will produce an image of 4 x 4 mm total size. As this will record 25
images keep the acquisition time per image low, 10 seconds should be
enough. Typical acquisition settings are shown below, Figure 31. An
example of the type of image recorded is shown below, Figure 32. Note that
part of two other craters can also be seen.
FIGURE 31. Stitched image acquisition settings.

Ion Gun Tuning
FIGURE 32. Stitched image of the crater.
13: Measure the X and Y crater size from the image by dragging the mouse
across from one edge to the other while holding down the mouse button,
Figure 33.

Ion Gun Tuning
Place the mouse pointer on one edge of the crater. Hold down the left mouse button
and drag the mouse pointer to the other edge of the crater. The length of the line is
displayed as r at the top of the image. In this example the length is 1.688 in the x
raster direction.
FIGURE 33. Measurement of crater size.
14: Calculate the correct X and Y scale using the following equation:
New scale value = (Old scale value / Measured size) x Requested size
In the above example the measured X size was 1.688 mm. The X scale
was 200 therefore the required new scale value is 237 volts. Note, the max-
imum scale value is 250 volts.
6.4.4 Tuning the beam
This section outlines a method for tuning the ion beam to produce a smaller
beam diameter or a larger ion flux. The instructions below assume that the
ion spot can be imaged and has been positioned to be coincident with the X-
ray spot, see Section 6.4.2 on page 191.
1: Switch the ion gun gas on, see Section 6.3.1 on page 184.
2: Select the pre-set row to be turned in the ion gun table and switch the ion
gun to standby, see Section 6.3.2 on page 185.

Ion Gun Tuning
3: Switch the ion gun on.
shield in position when the ion gun is switched on).
5: Switch on ion gun imaging, see Section 6.4.1 on page 189.
6: Turn on the sample current read-out by selecting the bias button, Figure
10 and clicking on the active button, see Section 6.2.5 on page 180.
7: Set the appropriate scale to read the ion beam current. As a guide the ion
current on the sample for beam energies of 2 kV and above should be
between 1 and 5 microamps. Lower beam energies produce correspond-
ingly lower ion currents.
8: Adjust the Condenser voltage and Focus voltage to minimise the spot
size or maximise the sample current as required, Figure 34.
Condenser Focus Align
FIGURE 34. Ion spot tuning.
9: When the required settings have been optimised, change the Align X volt-
age to maximise the measured sample current. Increasing the voltage on
the condenser lens (L2) will generally decrease the size of the ion spot at
the specimen. At a set beam energy, as the condenser voltage is increased
the focus voltage (L3) needed to produce a focused ion spot on the sample
will decrease.
10: To save the changes click on Update Row, Figure 35.
Update Row button Restore Row button

FIGURE 35. Saving changes.
6.5. Determining the Etch Rate
The etch rate produced on a given sample will vary with beam energy,
extracted ion current and raster size. However, it is useful to characterise
the sputter rate of the ion gun in a number on standard settings. This can
be achieved by etching a sample of known thickness. Such samples can be
readily purchased from a number of supplies:
Institute of Reference Materials and Measurements (IRMM), Retieseweg, B-

2440 Geel, Belgium. Tel: +3214571705, email: bcr.sales@irmm.jrc.be.
Standard Reference Materials, National Institute of Science and Technology

(NIST), 100 Bureau Drive, Stop 2322, Gaithersburg, MD 20899-2322, USA,
Tel: +1 3019756776, email: srminfo@nist.gov, web: http://ts.nist.gov/
Geller Microanalytical Laboratory, 426e Boston St, Topsfield, MA 01983-

1216, USA. Tel. +1 9788877000, email jg@gellermicro.com, web: http://
www.gellermicro.com


13 July 2009
Chapter 7
Data Acquisition
using the Instrument
Manager
Adam Roberts, Simon Hutton
7.1 Introduction
This chapter introduces the use of the Instrument Manager for data acquisi-
tion. The Instrument Manager window, commonly referred to as the Man-
ager window allows great flexibility in the design of automated experiments
on a single sample or multiple samples. This chapter will outline the design
of experimental flowcharts, starting from simple survey spectra, narrow
region scans at high spectral resolution, simple parallel imaging through to
more complex depth profiling and multiple unattended sample analysis. It is
assumed that the user has read the Getting Started chapter and is familiar
with moving samples to the analysis position.
The experiments discussed in this chapter refer to analysis of samples that

are readily available in a typical surface analysis lab. Following the detailed
description of the experimental design in each section should give the new
and inexperienced user the confidence to acquire data from a number of dif-
ferent samples. The chapter on data analysis using the Vision Processing
software will use the data acquired from these experiments to explain the
features of the Processing software.
7.2 The Instrument Manager Window - An Overview
The Instrument Manager window is the default window displayed after start-
ing the Vision software by double clicking on the Manager icon on the Win-
dows desktop. The Manager window is shown in FIGURE 1. with the
different parts of the window defined for reference.
201
The Instrument Manager Window - An Overview
Acquisition status window
Parameter entry window
Data region window
FIGURE 1. Instrument Manager window.
The acquisition status window is the region that is used to define the acqui-
sition flow chart. Objects defined in the parameter entry region of the win-
dow are pasted into the acquisition status region to build up an experiment.
The data region at the bottom left hand corner of the Instrument Manager
window is used to review already acquired data or data that is currently
being acquired. The menu bar and mode buttons identified in FIGURE 1.
are discussed in the next two sections.
7.2.1 The Menu Bar

The menu bar as shown in FIGURE 2. has a number of pull down menus
that are explained here. The various options will also be explained in con-
text of the experimental design.
202 Chapter 7 Data Acquisition using the Instrument Manager

menu bar
FIGURE 2. The menu bar and pull down options
7.2.1.1 File
Options available under the File menu are:
New Run
Load Run
Save Run
Submit Current Run
Submit Run File
View dataset
New Run. When selected this option will clear an existing flow diagram in
the acquisition status window ready for the user to define an new acquisition
flow chart.
Load Run. This option allows the user to recall a flowchart that has been
saved. This presents an easy way of ensuring that the acquisition parame-
ters used are identical from one sample to the next. It also removes the
need to redefine complex acquisition flow charts that are used routinely.
When load run is selected a dialogue box, shown in FIGURE 3., is brought
up allowing the user to select the required experiment.

FIGURE 3. Load run dialogue box
Save Run. This menu option is used to save a flow chart that has been
defined in the acquisition status window. When selected a dialogue box will
appear allowing the user to browse directories and give a file name to the
experiment. The experimental flow chart is usually saved in a directory
called runspec.
Submit Current Run. Selecting this menu option will start an acquisition
flowchart and duplicates the large submit button visible above the acquisi-
tion status window.
Submit Run File. Loads a pre-defined experimental dataset and submits it

to the queue.
View Dataset. The view dataset menu option will open a dialogue box, sim-
ilar to that shown in FIGURE 3. allowing the user to open a dataset. The
data objects within the dataset are displayed in the data window section of
the instrument manager when the data toggle button is pressed. This
menu option duplicates the View button in the data window.
7.2.1.2 Edit
The only option available under this menu is save configuration file. The
configuration file contains all the instrument specific information that defines
the hardware and software configuration of the AXIS Ultra DLD. The config-
uration file should only be saved if instrumental parameters in the Manual
window have been modified by the user. Furthermore, it is important that
the configuration file of the instrument is backed up in a different location

such as a CD or another network drive in case of a hard disk failure of the

computer used to control the AXIS spectrometer. Further details of backing
up the configuration file can be found in the Appendix.
7.2.1.3 Mode
After starting the Instrument Manger the mode of operation defaults to
advanced. It is strongly recommended that the spectrometer is routinely
run in this mode as it removes access to critical parameters associated with
the configuration of the spectrometer.
The mode can be changed to engineer by clicking on the mode menu and
selecting engineer. Note that engineer mode can be password protected
and the user may be prompted to type a password to activate this mode.
Changing to engineer mode will not affect the display of the Manager win-
dow but will allow certain tick boxes in the Manual window to become active
thus giving access to instrument critical parameters.
User mode can be used to operate the AXIS spectrometers but this mode
of operation is not recommended as it removes any control over acquisition
parameters and simply allows the user to load a pre-defined experimental
flow chart used to acquire the data. This mode of operation is designed for
use with the Kratos AMICUS photoelectron spectrometer for routine quality
control and quality assurance.
7.2.1.4 Window
The window menu allows the user to open and close different windows
which comprise the Vision Acquisition Software. The options available
under this menu are:
Manual window
Real-time display
Element list
Status window
VME/Slave messages
KRAM Debug
Version Information
Manual Window. This menu option opens the Vision Manual control win-
dow providing the user with complete manual control of the spectrometer.
Spectra, parallel images and optical microscope images may all be acquired
into datasets using the Manual window. The use of the Manual window is
discussed in several places throughout these instructions.
Real-time Display. The real-time display window comprises several areas

within the single window and is shown in FIGURE 4. The real-time display
window can be used to view data in the form of images or spectra that are
currently being acquired or to review data that has already been saved into
a dataset.
During acquisition parallel images are displayed in the bottom left hand part
of the real-time display window. If the image acquisition has been submitted
from the Manager window a timer bar will be displayed across the bottom of

this part of the window indicating the proportion of the total image acquisi-
tion time that has elapsed. The real-time acquisition of a spectrum is dis-
played in the large right hand window as indicated in FIGURE 4.
spectrum / image
display window
Analyser readback window
live counts per

second scrolling display
parallel image display
FIGURE 4. Real-time display window
The part of the real-time window displayed at the top left hand corner pro-
vides information on the current energy of the analyser. Note that the
Energy is displayed in Kinetic Energy. The other entries in this part of the
window provide information of spectral features which are useful in tuning
and testing of the spectrometer.
The live counts per second displays the total number of counts seen by the
detector every second as a rolling display. This display can be useful in
observing the trend of counts as the sample is moved in the height (Z) axis
for example.
The spectrum / image display section of the window can also be used to
review spectra that have already been saved into a dataset. To do this the
user simply needs to select an object from the data review section of the
Manager window and paste it into this section of the real-time display win-
dow. This operation is shown in FIGURE 5.

paste the selected data

object here to display in
the real-time display
window
select the object

using the left mouse button
FIGURE 5. Using the real-time display window to review data from a dataset.
The displayed spectrum or image will remain in the real-time display until all
objects are un-selected in the data review section of the Manager window.
To view a spectrum that is currently being acquired all objects in the data
review section of the Manager window must be un-selected. This is most
easily done by left clicking somewhere away from the rectangular data
objects.
The Element List. An element list is used to display the position of both
photoemission peaks and Auger transitions on a spectrum. The element list
window will scroll as a function of binding energy / kinetic energy as the
mouse is dragged over a spectrum with the left select button held down.
Note that the element list is in binding energy on the left hand side, with pho-
toemission peaks displayed and in Kinetic energy on the right hand side of
the window, with the Auger peak positions displayed. The element list win-
dow is shown in FIGURE 6. Note that the energy range displayed can be
changed by clicking with the right mouse button anywhere on the element
list window to bring up a menu. The default energy region displayed is
10eV.

Auger peaks
Photoemission peaks
BE display KE display
FIGURE 6. Element list window
The Status Window, VME/Slave Messages, Host Messages and KRAM

Debug windows are used for engineer diagnostics only.
Version Information allows the user to determine the version of Vision

Acquisition and Processing software being used. Selecting this option from
the menu displays the box shown in FIGURE 7.
FIGURE 7. Software version information

Defining an Experiment in the Manager Window
7.3 Defining an Experiment in the Manager Window
7.3.1 Large Area Survey Spectrum

This experiment will be set up to acquire a large analysis area (300x700m)
survey scan from a piece of Al foil. If the user wishes to reproduce this sim-
ple experiment it is assumed that a suitable sample is in the XPS analysis
position. For this experiment a piece of household aluminium foil about 1 x
1 cm square would be suitable.
The steps outlined below should be followed to define the acquisition flow-
chart:
1. In the Manager window select the dataset button by clicking with the left
mouse button. This will bring up the dataset definition window, shown in
FIGURE 8.
2. Click on the browse button to open the dataset name dialogue box.
3. Type in the sample name - for this example the dataset is called Al_foil.
Note that an underscore _ should be used in place of a space as the
Vision software does not recognise the space character. Press the OK
button once the dataset name is typed in. The dataset name dialogue
box will disappear.

1) Select dataset button
acquisition status window 2) select the browse button
3) type in the sample name

& select OK
FIGURE 8. Dataset definition window
4. A default name of Dataset for the dataset file name object as it will
appear in the flow diagram will be entered into the Name box automati-
cally. This name can be edited by replacing the text in the box. Note that
this name is simply used to identify the object in the flowchart and does
not influence any labelling elsewhere in the dataset.
5. Paste this object into the acquisition status window using the middle
mouse button, FIGURE 9.

pasted object
FIGURE 9. Dataset object pasted to the acquisition status window
6. This object in the flowchart will simply open a dataset into which the data
objects will be saved.
7. Select the Acquisition button to display the acquisition window, as
shown in FIGURE 10.
8. The following settings should be entered to define the survey scan from a
large area using the slot aperture.
Analyser section:
Analyser Mode: Spectrum
Lens Mode: Hybrid - Survey
Resolution: Pass energy 160 eV
Slot
in the X-ray Gun section:

Anode: Al (mono)
Emission: 15 mA
Acceleration Volts: 15 kV
Scan Control:
Type: Spectrum
Energy: Binding Energy
Reference: Al (mono)
in the Analysis Position section:

region name: Survey - N.B. Typing in the word Survey and pressing
return in the region name box will automatically enter the default vales.
Start: 1200 (centre 597.5)
End: -5 (width 1205)
Step: 1
Sweep: 120.5 (dwell 100 ms)

# sweeps: 1
Ensure Active button is selected
The analysis area at the surface of the sample in this mode is 300x700 m.
2) flowchart name
1) Acquisition button
FIGURE 10. Acquisition window of the Vision Manger.
9. A default name of Acquisition for the acquisition object as it will appear in

the flow diagram will be entered into the Name box automatically, FIG-
URE 10.
10. Paste the acquisition object into the acquisition status window below the
dataset object by using the middle mouse button.
This completes the creation of the flow chart which will open a dataset
called Al_foil in the data directory on the C: drive and acquire a large area
survey scan from the Al foil. Before submitting the acquisition ensure that
the spectrometer is waiting in automatic mode, as shown by amber and
green lights in the automatic and queue active section at the top left area

of the Manager window. Press the submit button to begin recording data.
If the spectrometer is in manual mode (the manual bulb is green) the user
should press the resume button BEFORE pressing the submit button. If
the queue is not active when the experiment is submitted then the flow chart
will enter the queue. If resume is subsequently pressed the experiment will
start.
After submitting the experiment, the survey scan will be displayed as it

acquires in the real-time display window. A data object will also appear as a
pink rectangle in the data review section of the Manager window. This will
change colour to grey / black once the acquisition is complete.
7.3.2 Large Area High Resolution Spectra

Having acquired a survey scan form the Al foil this section will detail the
acquisition of narrow region spectra at high resolution from the Al 2p and O
1s regions using the Instrument Manager window.
Starting from the flow chart defined in Section 7.3.1 an object must be
added to the flow chart to define the narrow region acquisition parameters.
This is achieved as follows:
1. Make sure that none of the objects are selected in the flow chart - when
selected they appear black when un-selected they appear grey.
2. The acquisition parameters will essentially remain the same as the anal-
ysis area, defined by the slot aperture, is the same. However, as a high
resolution scan is required the pass energy will be changed to 10eV. The
settings defined in the manager window should be as follows:
Analyser section:
Lens Mode: Hybrid - Survey
Slot
in the X-ray Gun section

Anode: Al (mono)
Emission: 15 mA
3. The acquisition regions are defined in the scan control section by click-
ing on the empty row below the survey parameters and in the region
name column typing O 1s. The default acquisition parameters for the O
1s region are then automatically loaded into the acquisition fields when
return is pressed. These values are set to give a single sweep of 60 sec-
onds over a narrow region around the O 1s peak. The default acquisition
parameters are saved in the Element Library which is discussed else-
where in this manual. The user should also note that the Vision software
is case sensitive and, therefore, the element symbol should be typed with
the first letter in upper case followed by the second letter (where appropri-

ate) in lower case. If the Vision software does not recognise the pho-
toemission peak typed in it will respond with an audible beep and a red
cross. This line should be deleted using the button bellow the table
rather than the delete key of the keyboard.
4. Type Al 2p in the region name below the O 1s. This will define the
acquisition parameters for the Al 2p region. It is good working practice to
acquire the narrow region scans in order of decreasing binding energy.
5. The two region scans will default to 1 sweep each. Increase the number
of sweeps for each region to 3.
6. So that the survey scan that is also defined in this window is not
acquired at 10 eV pass energy the active tick box at the end of the row
should be ticked off.
7. Paste the acquisition object into the acquisition status window below the
pre-existing object using the middle mouse button.
8. The manager window should look the same as that shown in FIGURE
11.

FIGURE 11. High resolution scans acquired from a large analysis area - manager window
This completes the creation the flow chart which will simply open the already
created dataset called Al_foil in the data directory on the C: drive and
acquire a second large area survey scan and the O 1s and Al 2p narrow
region scans from the Al foil. To submit the acquisition ensure that the spec-
trometer is waiting in automatic mode, as shown by amber and green lights
in the automatic and queue active section at the top left area of the Man-
ager window and press the submit button.
After submitting the experiment the active scans will be displayed in the
real-time display as they are acquired. The data objects will appear as a
pink rectangle in the data review section of the Manager window. This will
change colour to grey / black once the acquisition is complete.
7.3.2.1 Spectra from Insulators
The charge neutralisation system fitted to the AXIS Ultra DLD consists of a
filament and electrode plate mounted at the bottom of the electrostatic input
lens system. The magnetic field generated by the magnetic immersion lens
is used to transport the low energy electrons from the filament to the sam-
ple. The bias electrode (charge balance) acts to direct the electrons from the
filament into the magnetic field and also to reflect scattered electrons back
onto the surface.
The charge neutralisation system is relatively simple to operate but the

operating parameters need to be optimised. Once optimised most types of
insulating samples should be neutralised by the determined charge neutral-
iser settings so it is not necessary to adjust the conditions on each sample.
Choice of sample
Any insulating sample may be used for optimising the charge neutralisation
parameters. The recommended sample is clean polyethylene sheet, which
is resistant to X-ray damage and has only one peak, with a narrow linewidth
when excited by monochromatic X-rays. It is also readily available and is rel-
atively inexpensive. Suitable alternatives would be polypropylene or polysty-
rene (not expanded polystyrene). Polyethylene terephthalate (PET), also
known as polyester can be used but optimisation is more complicated
because of the complex C 1s peak structure (at least three peaks). Fluor-
opolymers e.g. Teflon (PTFE) should be avoided for initial optimisation since
they rapidly degrade in the X-ray beam. The sample should be flat and
firmly mounted on the sample bar to avoid curling.
Procedure
1. Using the stage control in the Manual window, position the sample at the
normal analysis height so that the top surface of the sample is at the opti-
mum monochromator analysis position.

2. Switch on the monochromator and set typical operating conditions e.g.

15-20 mA emission and 15 kV acceleration voltage.
3. In manual window set up an energy region for the C 1s line. Choose a
step size of 0.1 eV, a total energy range of about 20 eV about the peak
centre and a dwell time of 50 ms per point. Use Pass Energy 40 eV. Start
the acquisition.
4. Click on the parameters button highlighted in FIGURE 12. Make a note
of the present neutraliser parameters then set the neutraliser filament to
the default parameters by pressing the restore default settings. Note
that the Magnetic Lens Utilities which are displayed if the instrument is
run in Engineer Mode are not related to the charge neutraliser however
they are critical parameters for the correct operation of the spectrometer
and must NOT be changed.
click to display parameters and/or readback
FIGURE 12. Charge neutraliser parameters defined in the Manual Window.
5. Slowly increase the charge balance by 0.1 - 0.2 eV per cycle. As the
charge balance voltage is increased, the C 1s peak should move to
lower binding energy (BE). The intensity of the peak will also increase
and the peak width (FWHM) will decrease. If the charge balance is too
high, then the peak moves back to higher BE. A typical for the charge bal-
ance value is in the range 2.5 - 3.5 eV.
6. It is usual that the charge balance is the only parameter that needs to be
modified to improve charge neutralisation of a particularly challenging
sample. However, for systems where the neutraliser has been in regular
operation for greater than twelve to eighteen months it may be necessary
to increase the filament current slightly (0.05 A) to compensate for aging
or thinning of the filament.
The aim of the optimisation procedure is to maximise the peak intensity

which should also correspond to a minimum in peak width. It may be prefer-
able to use a smaller energy range, smaller step size and increased dwell
time (3 eV range, 0.1 eV, 150 ms) to more accurately find the optimum con-
ditions once the approximate settings are known.
Note that the three neutraliser parameters are strongly interdependent and
changing one value might require the optimisation of the others. The gen-
eral rule is that the charge balance is the most critical parameter in deter-
mining the efficiency of the neutralisation process.

The real time display window can be used to display a graph of the peak by
maximum - minimum value. This is achieved by clicking menu in the real
time display window and selecting the Trace Max - Min option. The sliders
in the Charge Neutraliser section of the manual control window can then be
adjusted to obtain the maximum net signal. This is generally easier than fol-
lowing the signal maximum which changes as the peak centre moves away
from the centre of the binding energy range.
The optimum charge neutraliser conditions tend to over compensate leading

to a peak shifted to a lower binding energy than would be obtained if the
sample were an electrical conductor e.g. C 1s (carbon on metal) approxi-
mately 284.8 eV, C 1s (hydrocarbon polymer) approximately 282 eV. The
shift will be proportional to the charge balance voltage. A plateau condition
exists over a range of about 1 - 2 eV on the charge balance where neutrali-
sation is optimised.
Obtain a spectrum of the C 1s region using a pass energy of 10 eV and a

step size of 0.05 eV. A single peak with no structure visible should be
obtained if using a polyethylene sample. Slight asymmetry, due to unre-
solved vibrational fine structure, may be observed on the high binding
energy side of the peak1. A FWHM resolution of better than 0.9 eV may be
expected when using the monochromated excitation source and the acquisi-
tion parameters defined above. The exact value may depend upon the
cleanliness of the polyethylene surface. A survey spectrum should show lit-
tle or no oxygen and no other contaminants (e.g. Si, Na, Cl, S).
It may be necessary to increase the filament current in order to obtain opti-

mum conditions. However, an maximum operating current of 2.1 Amps
should not normally be exceeded.
There are various sets of operating conditions which lead to neutralisation.

As the filament bias is increased, the charge balance may also need to be
increased typically by about 1 - 2 eV per eV increase in filament bias. A
lower filament bias is generally preferable, since the peaks will be shifted
less from their true binding energy.
Once set the operating conditions should remain constant for similar sam-
ples e.g. flat smooth surfaces (polymer sheet, mica, flat glass sheet). Sam-
ples which present a rougher surface (powders, bundles of fibres etc.) may
require a higher value of charge balance to ensure optimum neutralisation.
In severe cases, it may also be necessary to increase the filament bias volt-
age. The general procedure described above can be used on any insulating
sample, so neutralisation parameters can be optimised on an individual
sample. Choose the most intense and narrowest peak to optimise the condi-
tions. C 1s or O 1s peaks are often most suitable. Adjust the neutralisation
conditions to give a maximum net peak intensity.
The charge neutralisation conditions should be checked periodically and

adjusted if necessary. Re-optimisation may be necessary when the mono-
chromator source has been changed e.g. new mono filament or mono tar-
1. G Beamson, D.T. Clark, J.Kendrick, D. Briggs, J.Elec. Spectr. Rel. Phenom. 57, 79, (1991)

get; or as the charge neutralisation filament ages and changes its emission
characteristics.
Typical recommended operating parameters are:
charge balance............2.6 to 3.6 V
filament bias................1 to 1.6 V
filament current...........1.8 to 2.10 Amps.
Spectral Acquisition From Insulators Using the Vision Manager
The charge neutraliser can be used during automated acquisition using the
Vision Manager. In the Manager window the neutraliser parameters are
defined in a section of the acquisition window, as shown in FIGURE 13.
The different modes of operation of the neutraliser in the Manager window
are defined by the pull down menu, also shown in FIGURE 13.
FIGURE 13. Neutraliser controls in the Manager window.
Using the different pull down menus will result in different behaviour of the
neutraliser during the acquisition.
Switch off will simply switch the neutraliser off at the start of the first scan
defined in the acquisition. The neutraliser will then remain off for all subse-
quent acquisition regions.
Switch on. This menu option will switch the neutraliser on using the set-
tings that are defined in the displayed text boxes as the first defined acquisi-
tion region is started. The neutraliser will then remain on with the same
settings for all following acquisition regions.
On for acquisition. Selecting this setting will turn the neutraliser on at the
start of the acquisition using the parameters defined in the text box. It will
then be turned off after all the sweeps have been completed in that Manager
window.
Under Manual Control will leave the neutraliser in exactly the same status
as it is in the Manual window. This mode of operation is recommended as
the neutraliser will remain switched on for the duration of the experiment.
This is particularly useful when running the type of experiment defined in
Section 7.3.6.2 where the samples are different and will require charge neu-

tralisation. It has also been determined that the neutralisation process using
the AXIS neutraliser works more efficiently if the charge neutraliser is on
before the X-rays are switched on. Running the neutraliser under manual
control will effectively leave it on over the duration of the experiment whilst
the x-rays will be turned off at the end of each acquisition.
7.3.3 Parallel Imaging - Field of View 2
One of the standard samples used by Kratos Analytical for testing the paral-
lel imaging is a gold finder grid. Such a grid should be left on the standard
stub after installation of the spectrometer and is useful in determining the
imaging performance. Aligning a small feature to the XPS analysis position
using the SAC camera has been discussed and it is assumed that the finder
grid is in the analysis position and at the correct height. Due to the narrow
depth of field in imaging mode, it is usual for a parallel image to have been
acquired using the Manual window to confirm that the sample is at the cor-
rect height before the Instrument Manager is used to collect a parallel
image and save it into the dataset.
The following instructions introduce the use of the Manager window to

acquire parallel images from the gold finder grid. The instructions start by
changing to a new flow chart region from that used for the spectroscopic
acquisition in section 7.3.2.
right mouse click here

and select flow chart 2
FIGURE 14. Changing between flow chart regions
1. Right mouse click over flow chart 1 of the acquisition status window as
indicated in FIGURE 14. and select flow chart 2. Note that there are a
total of five independent flowchart environments where the user can
define experiments.
FIGURE 8.
4. Type in the sample name - in this example the dataset is called Au_grid.
Note that an underscore _ should be used in place of a space as the

Vision software does not recognise the space character. Press the OK
button once the dataset name is typed in.
5. Paste the dataset name object in the flowchart region.
6. Select the Acquisition button to display the acquisition window, as
shown in FIGURE 10.
As discussed in the introduction chapter parallel imaging mode uses the

spherical mirror analyser (SMA) and the 2 dimensional delay-line detector.
The transfer of the photoelectrons to the analyser by the magnetic and elec-
trostatic lenses and the electron path through the SMA is defined simply by
selecting imaging mode in the scan control section and the appropriate
lens mode and aperture setting. Three fields of view (FOV) are defined in
the testing and configuration of the instrument. The fields of view will vary
slightly from spectrometer to spectrometer but typical parallel imaging fields
of view are:
FOV 1 - 900 x 900 m
FOV 2 - 400 x 400 m
FOV 3 - 250 x 250 m
The FOV for each spectrometer is calibrated and stored in the configuration
file.
7. The following settings should be entered to define the parallel image

from a 400x400 m area using the FOV2 lens mode.
Analyser section:
Analyser Mode: Imaging
Lens Mode: FOV 2
high resolution (aperture setting)

Anode: Al (mono)
Emission: 15 mA
8. In the scan control section of the Manager window which is highlighted

in FIGURE 15. select map from the pull down menu titled type. Note
that this automatically greys out the width and step columns in the
analysis position section of the Manager window. The user can not type
values into these two columns.

section
scan control
FIGURE 15. Imaging mode defined in the Manager window.
9. In the region name box, type Au 4f and press return. This will enter the
default values for this region into the row. Modify the name to Au 4f FOV
2 and change the centre energy to 84 eV binding energy to acquire the
image at the Au 4f7/2 peak maximum. Change the dwell time to 120 secs.
Ensure that the row is active.
10. Enter image in the object name text box at the top of the Manager win-
dow and paste the defined acquisition into the acquisition status window
to add this object to the flow chart.
11. The Manager window should be the same as that shown in FIGURE 15.
12. With the spectrometer in queue active mode as indicated by the green
bulb at the top left of the Manager window, press the submit button.
After several seconds (to allow the lenses to ramp to the correct voltages)
the parallel image will appear in the bottom left hand corner of the real-time
display window with a progress timer below. The full scale of the timer cor-
responds to the dwell time defined in the acquisition, in this case 120 sec,
with the moving black bar showing the progress of the parallel image. A data
object named Au 4f FOV2 will appear as a pink rectangle in the data review

section of the Manager window. This will change colour to grey / black once
the acquisition is complete.
7.3.4 Parallel Imaging - FOV 1 and FOV 3

The previous section introduced acquisition of a parallel image using the
Manager window. The image was acquired from a 400 x 400 m area of the
gold finder grid. In this section the imaging flow chart will be modified to
acquire images from the two other fields of view providing images from 900
x 900 m and 250 x 250 m areas of the sample.
The starting point for defining images from the additional FOVs is the acqui-
sition flow chart created in section 7.3.3 and shown in FIGURE 15. To
acquire the two additional FOVs two more objects corresponding to the two
FOVs must be included in the acquisition flowchart. This is simply achieved
by cutting and pasting objects in the flow chart and then modifying the
acquisition parameters as follows:
1. Select the image object from the flowchart in the acquisition status win-
dow of the Manager. The image object should turn black when selected.
2. Click with the right mouse button to bring up a menu and select copy
with the left mouse button.
3. Select the image object in the flowchart again and right mouse click to
bring up the menu again. Select the paste after option. You will see that
the flowchart now has three objects; file and two image.
4. To define the third FOV we require a third image object in the flow
chart. As with most software the copied object remains on the clipboard
until replaced with another copied object. An alternative way to paste an
object into the flowchart is to simply position the cursor at the position the
acquisition object is required and press the middle mouse button to
paste the object into the flowchart.
5. The flow chart should now appear as shown in FIGURE 16.
FIGURE 16. Manager window with 3 imaging objects in a flowchart

6. The acquisition flowchart as defined above contains instructions to the

spectrometer to acquire three identical images of the finder grid and save
the images into the dataset named Au_grid.dset. This is not the intention
of this experiment where an image from each FOV is required. The flow-
chart object must therefore be modified.
7. Select the first image object in the flowchart, the one directly after the
file object, by using the left mouse button.
8. With all other parameters in the acquisition window remaining the same
change the lens mode to FOV 1 - Survey and change the aperture set-
ting to imaging - medium resn. Change the Goto Standby to Leave On.
This will leave the X-rays and detector volts following the acquisition so
that the instrument will be ready to record the next image.
9. In the region name box change the text to Au 4f FOV1 and decrease
the dwell time to 60 seconds.
10. The second image object in the acquisition flowchart can remain the
same as we will collect another FOV 2 Au 4f image but change the Goto
Standby to Leave On.
11. Select the final image object in the flowchart and change the lens
mode to FOV 3. The aperture setting should remain at imaging - high
resn.
12. In the region name box change the text to Au 4f FOV3 and increase
the dwell time to 180 seconds.
13. This completes the creation of the flow chart. Note that the user MUST
select a flowchart object to display and also modify the acquisition param-
eters. Changes made when one of the flowchart objects is not selected
will not appear in the flowchart.
The acquisition should be submitted by pressing the submit button. The

parallel images will be displayed in the real-time display window as they are
acquired. Once the object displayed in the data view part of the Manager
window changes from pink to grey the image may be selected by clicking
with the left mouse button and pasting into the large display area on the right
hand side of the real-time display window.
7.3.5 Small Spot - Selected Area Spectra
In this section the acquisition of a small spot spectrum from a specific posi-
tion on the surface sample is described. As discussed in the introduction
chapter the selected area is defined by inserting an aperture into the electro-
static lens column. Furthermore, the analysis position may then be
deflected across the sample surface by applying a voltage to the electro-
static scan plates to acquire spectra from a selected area on the sample.
These operations are all controlled through the software and only require
definition of the correct parameters in the acquisition flow chart.
The example outlined below will use the parallel image from the gold finder
grid that was acquired in Section 7.3.3 page 219 to define the analysis posi-
tions. A 27 m spectrum will then be acquired from positions on and off the
gold grid. The experimental flow chart will be defined in a new acquisition
status window.

1. Right mouse click in the background region of the acquisition status win-
dow indicated in FIGURE 14. and select flow chart 3.
FIGURE 8.
4. For this example the small spot spectra will be placed in the dataset that
was already created during the parallel imaging experiment. Select the
dataset called Au_grid.dset. This will show the file pathname in file win-
dow. Paste the dataset object in the flowchart region, as shown in FIG-
URE 17.
FIGURE 17. File object added to the flowchart region.
5. Select the Acquisition button to display the acquisition window in the

Manager environment.
As discussed above the small analysis area is defined by inserting an aper-

ture into the electrostatic lens column. To achieve the calibrated selected
area defined in the aperture pull down menu (55 m, 27 m or 15 m)
spectra must be acquired with the spectrometer using field of view (FOV) 2.
In this experiment we are simply going to acquire a selected area survey
spectrum on and off one of the bars of the Au grid. The analysis position is
defined from the parallel image.
6. Define the following settings in the acquisition section:
Analyser section:
Lens Mode: FOV 2
Resolution: Pass energy 160eV
27m aperture

Anode: Al (mono)
Emission: 15mA
Acceleration Volts: 15kV

in the Analysis Position section

region name: Survey - N.B. Typing in the word Survey (note case sensi-
tive) and pressing return in the region name box will automatically enter
the default vales.
Start: 1200
End: -5
Step: 1
Sweep: 120.5
# sweeps: 2
FIGURE 18. Selected area experiment.
7. Name the acquisition object small spot and paste it into the flowchart
region, FIGURE 18.
The analysis area at the surface of the sample in this mode is 27m. How-
ever, as defined above, the spectrum will be acquired along the central axis
of the spectrometer. The analysis area must be deflected to the required
analysis position as described in the following steps:

8. Select the parallel image of the Au finder grid that was acquired in the
experiment defined in Section 7.3.3 and paste it into the right hand side of
the real-time display window. An example is displayed in FIGURE 19.
left mouse click here
FIGURE 19. Real-time display with Au parallel image displayed.
9. Click on a position on the Au grid with the left mouse button. If the
mouse button is held down and dragged, the coordinates of the mouse
are displayed at the top of the image in the real-time display.
10. In the Manager window the analysis position can be imported into the
acquisition by clicking on the import position button indicated in FIGURE
20.
use this button to import analysis position

coordinates displayed in the boxes below
FIGURE 20. Import position button in the Manager window.

11. The 27 m acquisition position will now be deflected to the point defined
from the parallel image.
12. Select the small spot object in the flow chart so that it turns black.
13. Right mouse click on a background region of the flowchart window and
select copy from the menu that appears.
14. Select the small spot object with the left mouse button so that it turns
black. Then right mouse click again on a background region of the flow-
chart area and select paste after. This will paste a copy of the small
spot acquisition object in the flow chart.
15. Select the second small spot object in the flow chart so that the acqui-
sition parameters are displayed on right of the Manager window.
16. Change the label to Survey pt2.
17. Click on a region of the parallel image in the real time display that is not
part of the grid, i.e. over the hole, as displayed in FIGURE 21. Then click
on import position to load the coordinates for the second point into the
software. This will give a spectrum that is clearly different from the one
acquired from the grid.
left mouse click here and import

into the second small spot object
FIGURE 21. Second small spot analysis position.

18. This completes the creation of the flow chart. Note that the user MUST
select a flowchart object to display and also modify the acquisition param-
eters. Changes made when one of the flowchart objects is not selected
will not appear in the flowchart.

spectra will be displayed in the real-time display when the Au 4f parallel
image that was used to defined the analysis positions is de-selected. To de-
select an object that has been selected in the acquiring section of the Man-
ager window, left mouse click on the background region and ensure that all
the objects are light grey.
In this section an experimental flow chart has been defined that will acquire
survey scans from two independent 27m areas on a surface. A similar
experiment can be defined to acquire high resolution spectra over narrow
regions from the same analysis points by changing the pass energy and the
acquisition regions.
7.3.6 Automated Spectral Acquisition From Several Samples
In this section an experiment will be defined to acquire spectra from several

related samples. The experiment will assume that the same acquisition
regions, including a survey scan, is to be acquired from each sample. This
type of experiment is useful when the user has a large number of samples
that may differ in atomic concentration, such as a number of oxide powders
with different dopant concentrations of a particular element.
The experiment is defined to place the spectra from each sample into a
dataset that is identified with that individual sample name. In this example
large area (300 x 700 m) analysis will be performed for each sample.
A similar experiment could be designed to acquire a number of spectra from

different positions on a large sample to give a statistical analysis of the sur-
face. An example of this type of experiment might be analysis of 20 points
chosen from a hard disk drive surface.
7.3.6.1 Acquiring Spectra From Similar Samples.
The stage positions at which the analysis is to be performed must be

defined in the manual window. Each analysis position should be defined
and saved into the stage position table as shown in FIGURE 22. In this
worked example it is assumed that the user has defined a minimum of three
independent stage positions which will place similar samples at the analysis
position. In this example the same spectra will be acquired from each sam-
ple using a simple loop function in the flowchart.

FIGURE 22. Stage position table
The flow chart for this experiment is defined in the Instrument Manager win-
dow as follows:
1. Select flow chart 4 by right mouse clicking on flow chart text and select-
ing flow chart 4. This will display an empty box in the acquisition status
section of the Manager window.
2. Select the acquisition button highlighted in FIGURE 23. and enter the
parameters to define a survey spectrum using the lens mode hybrid and
the slot aperture. This is exactly the same acquisition parameters as
defined in Section 7.3.1 page 209. Paste the object into the flowchart
region.
3. Select the acquisition object in the flowchart using the left mouse button
and then by right mouse clicking on the background area select the copy
option.
4. Paste the copied flowchart option after the first one by clicking with the
middle mouse button.
5. Select the newly displayed flowchart object so that it turns black and
define several high resolution scans. The analyser parameters should be
exactly the same as those defined in Section 7.3.2 page 213 but the
regions that are acquired should be modified to reflect the nature of the
samples being analysed.
FIGURE 23. Acquisition button to define the spectral acquisition parameters.

The flowchart in the acquisition status should have two objects labelled
acquisition which would simply acquire a large area survey and high reso-
lutions scans if submitted. The next step is to include the sample movement
so that data is acquired from each sample and saved into the respective
datasets.
6. Select the state changes button, shown in FIGURE 24. followed by the
sample position button to display the sample position table. Initially the
table will be empty.
select state change and

sample position buttons
path name & dataset here
FIGURE 24. State change and the position table.
7. Click the load position table button. This action will import the position
table that has been defined in the manual window. Clicking the load
position button will load the single stage position that is currently high-
lighted in the manual window.
In this example the aim of the experiment is to acquire the data from each
sample and put the spectra in a dataset specific to that sample. Therefore,
the dataset name and pathname must be included in the experiment.
8. The pathname and dataset name for each sample should be entered in
the dataset name text box, indicated in FIGURE 24. To define the path
name click the select dataset button and navigate to the folder to which
the data should be saved using the popup dialogue box. Edit the dataset
name at the end of the pathname to define the dataset that the spectra
will be acquired into. The text box should now contain the following C:/
data/dataset_name.dset text.
9. Copy the first line by triple clicking on the text box and then paste using
the middle mouse button into the two rows below or using the select
dataset button as described above.
10. Modify the dataset name of each sample position defined.

11. Name the state change object position and paste this object into the
acquisition flow chart before the first object labelled spectrum in the flow-
chart, as shown in FIGURE 25.
FIGURE 25. Automated sample move included in acquisition flowchart.
If this experiment was submitted now, the stage would move the first sample
to the analysis position and then acquire the survey and high resolution
spectra then stop. It is necessary to define a loop so that the acquisition
flowchart will loop back and acquire spectra from the subsequent two stage
positions (samples).
12. With the state change button selected, select the counter button high-
lighted in FIGURE 25. to display the window shown below.
13. Enter the number of cycles in the test box as nine (9). and name the
object count before pasting using the middle mouse button into the flow-
chart region after the second spectrum object. The flowchart should
appear as shown in FIGURE 26.
FIGURE 26. Counter in the acquisition flowchart.
14. Highlight all the objects in the flowchart by clicking and dragging a box
with the left mouse button. The flowchart objects will turn black, as
shown in FIGURE 27.

FIGURE 27. Highlighted objects in the flowchart.
15. Right mouse click in the background area of the acquisition status win-
dow (below or to the right of the flowchart) and select the loop back
option from the menu. A loop with an upward facing arrow will automati-
cally appear as the mouse button is released. The flowchart will be as
shown in FIGURE 28.
FIGURE 28. Flow chart with a loop back operation.
The flowchart as defined will continue to loop back until all nine loops have
been made as the user was instructed to enter nine cycles. However, we
have only defined three sample positions so multiple spectra would be
acquired for each sample. To prevent this from happening a jump to oper-
ation must be included in the flowchart. This type of loop is particularly use-
ful when there is some ambiguity regarding the exact number of samples or
positions defined in the manual window. The jump to operation will force
the position object to dominate over the cycle object. In this example the
jump to will force the experiment to end when all the sample positions
have been run.
16. To complete the experimental flow chart and define the jump to,
ensure that all the objects in the flowchart are highlighted as shown in

FIGURE 27. and right mouse click in the background region of the acqui-
sition status window to bring up the menu.
17. Select the jump to menu option. The flow chart is now complete and
should have a structure similar to that shown in FIGURE 29.
FIGURE 29. Completed flowchart to acquire spectra from a number of samples with automated
stage movement and data saved in individual datasets.

sample stage will move the samples in turn to the analysis position. The
sample position can be confirmed by looking at the stage control section in
the Manual window. The spectra can be viewed in the real-time display win-
dow as they are collected.
7.3.6.2 Acquiring Spectra from Dissimilar Samples
The experiment defined in the section above assumed that the samples that
are to be analysed are all similar and that it is appropriate to acquire the
same narrow region spectra from each sample. This may not be the case if
there are a number of different types of sample mounted on the platen, for
example, several polymer samples and two inorganic metal oxide samples.
The principles of designing the flow chart in this case are exactly the same
as those discussed above in Section 7.3.6.1 but, in each case the acquisi-
tion object in the flowchart must be unique to the particular sample. A quick
overview of the flowchart design for such an experiment is given below.
1. In the Manual window define the analysis positions of all the samples
ensuring that each sample is at the correct analysis height. The sample
position table should contain all the analysis positions. Click on the first
row so that it is highlighted by a black box around the complete row.
2. In the Manager window, select the state change button and then the
sample position button, as shown in FIGURE 30.

FIGURE 30. State change - position table in Manager window.
3. Click the load position highlighted above. This will import the sample
position that was highlighted in the Manual window.
4. Either type or copy and past the pathname into the dataset name text
box. A dataset name should be used that is associated with the sample
according to the users lab. practices.
5. Name the state change object - again it is recommended that the sam-
ple name is used to easily identify the object during the acquisition - and
paste into the flowchart region.
The next step is to define the spectral acquisition that is required from the
sample. In this example a large area survey scan, followed by narrow
region, high resolution scans will be defined.
6. Click on the acquisition button in the Manager window and define a
large area (Hybrid, slot), low resolution (pass energy 160 eV) survey scan
as in Section 7.3.1. Name the object survey and paste into the flowchart
area after the sample object by using the middle mouse button.
7. Ensure that the survey object is de-selected in the flowchart and modify
the acquisition parameters in the Manager window to acquire the high
resolution (10 eV pass energy) large area (Hybrid, slot) spectra from the
photoelectron lines. In this example spectra are acquired from the O 1s,
N 1s and C 1s regions of a polymer material.
8. Name the flowchart object regions and paste into the flowchart region
of the window. The flow chart should appear as shown in FIGURE 31.

FIGURE 31. Sample movement, survey and high resolution objects in a flowchart.
The simplest way to create the rest of the flow chart is to cut and paste the
objects already defined in the flowchart and then modify the sample posi-
tion, dataset name and acquisition parameters as described below.
9. Click and drag using the left mouse button so that the sample, survey
and regions objects are highlighted in the flowchart. Each object will
appear black when highlighted.
10. Right mouse click on the background of the acquisition status window to
bring up the menu and select copy.
11. Select the regions object using the left mouse button and then paste
the copied objects using the middle mouse button, or by selecting the
paste after option from the same menu used moments earlier.
12. Repeat this sequence a number of times to build up a flowchart with the
required number of sample movements.
Note that the above instructions have simply duplicated the sample move-
ment and data acquisition steps for the first sample. Each object must be
modified to move to the next sample and acquire the appropriate regions.
The steps involved are detailed for the second sample and should be used
for all subsequent samples defined in the position table.
13. Highlight the second sample object in the flowchart so that it turns
black. The state change sample position window will be displayed.
14. In the Manual window highlight the second sample analysis position.
15. Return to the Manager window and select the import position button.
The position name that was given in the Manual window will be displayed
in the first row. If the first sample position is also displayed in the table
delete it by selecting the row and pressing the delete row button at the
bottom of the table.
16. Enter the pathname and the dataset name corresponding to the second
sample.

17. The large area survey scan is still required from the second sample so
this may be left unchanged.
18. Select the second regions object in the flow chart. Edit the regions
required to reflect the composition of the sample. In this example a F 1s
region is required and is added into the acquisition table before the O 1s
by selecting the O 1s row and then pressing the insert row button. This
gives an empty row ABOVE the row that was highlighted into which the F
1s acquisition parameters can be added.
19. For the second polymer, in this example, no N 1s region is required.
The N 1s region can be made inactive so that the N 1s spectrum will not
be acquired by simply pressing the active button shown in FIGURE 32.
Alternatively the N 1s row can be deleted by highlighting this row and
pressing the delete row button at the bottom of the table.
active button
FIGURE 32. Active button in the acquisition parameter section of the Manager window.
20. The subsequent objects in the flowchart should be edited to move the
next sample to the correct position and acquire spectra appropriate to
that specific sample.
When construction of the flowchart is completed it may be submitted. The

progress of the experiment can be followed by selecting the follow button in
the Manager window and observing the spectra in the real-time display as
they are acquired. In follow mode the currently active acquisition is dis-
played in pink in the flowchart. Follow mode also allows the user to increase
or decrease the number of sweeps for a particular region after the acquisi-
tion has been submitted. This is useful if the signal to noise ratio needs to
be increased by increasing the number of sweeps on a particular region or
conversely if the user wishes to decrease the acquisition time because the
S/N ratio is already sufficient.
7.3.6.3 Adding a Delay to Automated Acquisition

The user has the option to include a defined delay in a flow chart during
automated acquisition. Such a delay may be useful if time dependent
experiments are being undertaken.

The delay function can be found in the state change window, shown in FIG-
URE 33. The time delay is defined in minutes, or fractions there-of. The
maximum time delay permitted is 1440 minutes (24 hours). Note that the
status of the instrument remains unchanged by the time delay object so if
the previous object in a flow chart has the x-rays set to leave on they would
remain on during the time delay.
When a time delay is included in a flowchart a countdown display is shown

in next to the delay object in the flowchart when follow mode is selected.
An example is shown in FIGURE 33.
FIGURE 33. Time delay state change (insert shows delay count down in follow mode)
7.3.7 Automatically Finding the Sample Analysis Height (AutoZ)
Often the samples to be analysed will be of different thicknesses. To make

automatic data acquisition from a number of these samples possible the
instrument can be set-up to optimise the height of the stage on each sample
individually before the data acquisition starts. The method is essentially an
extension of the AutoZ procedure described for one sample in Section 4.8.4
page 113.
In this example it will be assumed that the optical camera has been used to
identify samples or areas of interest and that these positions have been
recorded into the position table, Section 4.8.3.1 page 111. Follow the
instructions below to define positions, set-up the AutoZ parameters and
include this information in a flow chart for automated analysis.
1. Insert the position for the Ag sample in the general position table.
2. Scroll up to the Analyser and Acquisition Control section of the manual
window and define suitable settings for an Ag 3d Snapshot spectrum,
FIGURE 34.
Analyser Section:


Lens Mode: Hybrid
Resolution: Pass Energy 160
Slot
Acquisition Control:
Type: Snapshot
Region Name: Ag 3d
Centre eV: 371
Dwell ms: 6000
# Sweeps: 1
X-ray PSU:
Emission (mA): 5
Anode HT (kV): 15
FIGURE 34. Analyser, Acquisition and X-ray parameters for a Ag 3d Snapshot spectrum.

3. Make sure that the Ag 3d Snapshot is at the top of the Acquisition

Regions table and that Active is selected.
4. Scroll down to the Manipulator section and ensure that the Ag sample
position entered in the table is selected by left clicking on it. The row in
the table should now be surrounded by a black box.
5. Enter the following information into the AutoZ sub-section of the Manipu-
lator section, FIGURE 35.
No. Increments: 21
Increment size (mm): 0.05
Ordinate choice: Area
Acquisition Settings: Current Manual
FIGURE 35. AutoZ settings.
6. Click on Grab Scan to download the scan settings from the top row of
the region table into the AutoZ section.
This action saves the Ag Snapshot settings with the defined Ag sample
position. The abbreviation Req. will be entered into the AZ column of the
General position table to reflect that the AutoZ routine is required for that
position. Also the Snapshot parameters will be entered into the AutoZ
acquisition settings boxes, FIGURE 36.

Req.
Snapshot Centre Snapshot Width

(readback only) (readback only)
FIGURE 36. AutoZ Snapshot parameters.
7. Move the stage to the next sample and import the next samples XPS
coordinates, e.g. the Ta foil sample.
8. Scroll up to the Acquisition Control section, delete the Ag 3d Snapshot
and enter settings for a new Snapshot spectrum relevant to the sample
been analysed, FIGURE 37.

FIGURE 37. Ta 4f Snapshot settings.
9. Scroll down to the Manipulator section and ensure that the Ta2O5 sam-
ple position entered in the table is selected by left clicking on it. The row
in the table should now be surrounded by a black box.
10. Enter the information into the AutoZ sub-section of the Manipulator sec-
tion following the same procedure as for the Ag sample above, FIGURE
35.
11. Click on Grab Scan to download the scan settings from the top row of
the region table into the AutoZ section.
This saves the Ta Snapshot settings with the defined Ta2O5 sample posi-
tion. The abbreviation Req. will be entered into the AZ column of the Gen-
eral position table to reflect that the AutoZ routine is required for that
position. Also the Snapshot parameters will be entered into the AutoZ
acquisition settings boxes, FIGURE 38.

FIGURE 38. AutoZ Snapshot parameters entered for the last sample.
12. Follow points 7 to 11 above for the third gold sample using C1s instead
of Ta 4f for the Snapshot spectrum.
13. Three XPS analysis points should now be defined, FIGURE 39.

FIGURE 39. Three positions defined.
This table can now be used in a flow chart in the same way as a standard
table as described in Section 7.3.6.2 page 233. Now when a position is
loaded into the Sample Position section of the manager window the AutoZ
parameters associated with that position will also be displayed, FIGURE 40.
AutoZ Parameters
FIGURE 40. Sample Position with AutoZ parameters
It is possible to edit the number of increments or the increment size from this
window.
When the flow chart is submitted the instrument will automatically determine
the correct analysis height by measuring the area under each Snapshot
spectrum defined for each position at a number of different sample heights.
In this example the stage will be driven down by 500 microns from the start-
ing height and then move up in 50 micron steps until it has moved 500

microns above the initial height. The height where the maximum area was
measured will be entered into the table and the stage driven to that height
for the data acquisition. Furthermore, the Req. message in the AZ column
of the position table will change to Done to indicate that the AutoZ routine
has been performed for that sample. If you wish to perform the AutoZ rou-
tine for a second time on a position where Done is displayed then click on
Reset Row, FIGURE 40. After each AutoZ height optimisation an object
labelled Auto z Profile is written to the file.
The appropriate number of increments and the increment step will depend
upon the thickness of the sample. To check that the maximum position was
found paste the Auto z Profile object into the real time display window, FIG-
URE 41. A maximum in the count rate should be obvious. If the sample is
thicker than 4 millimetres then it is advisable to use the SAC microscope to
define the XPS position.
FIGURE 41. Auto Scan Profile

7.3.8 Angle Resolved XPS
Reducing the take-off angle of photoelectrons reduces the depth from which
the XPS information is obtained. The AXIS Ultra DLD can be used for
ARXPS using the standard strip or constant height bars to rotate the sample
about the horizontal x-axis. The user should note that whilst the general
principles of angular dependent XPS are well known, the ability to obtain
accurate and unique quantified concentration depth profiles from this tech-
nique are not straightforward. The user is encouraged to read the many
articles published to gain further information on the determination of ARXPS
concentration depth profiles.
Further comment should be made regarding the use of the magnetic lens
based AXIS Ultra DLD for ARXPS. The solid acceptance angle of the lens /
analyser is relatively large in normal spectroscopy modes. Consequently
the depth resolution in depth profiles can be degraded since photoelectrons
over a range of angles are being acquired. This effect can be reduced by
closing the iris situated at the end of the electrostatic lens column and thus
reducing the angular acceptance. Alternatively, for larger samples where
the area illuminated by the mono spot can be used to define the analysis
area, it is possible to switch to electrostatic lens mode in which the magnetic
lens is not used. This has the effect of also reducing the angular accept-
ance of the lens.
The experimental procedure outlined below will be split into two sections.
The first will describe the process of defining the sample positions at the
various angles required for the ARXPS experiment in manual mode. The
second part will outline setting up the Manager window to acquire the angu-
lar resolved spectra.
7.3.8.1 Defining the Sample Positions for ARXPS in Manual Mode
Samples for ARXPS should must be flat and mounted securely on the sam-
ple bar. The geometry of the constant height bar is such that the sample
surface should be on the axis of rotation of autostage. It is therefore recom-
mended that this bar is used for ARXPS where possible. The experimental
set-up procedure detailed below defines the position of the sample at each
required angle by optimising the XPS signal.
1. After mounting the samples on the constant height bar, load the bar onto
the auto stage and optimise the sample height using snapshot mode.
The auto Z mode detailed in Section 7.3.7 could be used to achieve this.

2. Ensure that the position menu option is selected as shown in FIGURE

42. and save the optimised sample position into the sample position
table.
position menu option
FIGURE 42. position menu option
3. From the Manual window start a snapshot spectrum using 160 eV pass
energy (ca. 16 eV energy window). The following acquisition conditions
are suggested:
Analyser Section:
Lens Mode: Hybrid
Resolution: Pass Energy 160
Slot
Acquisition Control:
Type: Snapshot
Region Name: O 1s (or as appropriate)
Centre eV: 530
Dwell ms: 6000
# Sweeps: 1
X-ray PSU:
Emission (mA): 5
Anode HT (kV): 15

4. Using the autostage software control, shown in FIGURE 43., rotate the
sample towards the monochromatic X-ray source by -15 degrees. This
should cause a small decrease in the signal displayed in the real time dis-
play.
5. To ensure that the sample position is optimised move the sample in the
y-axis, monitoring the bottom left hand rolling display of the in the real
time display.
use these buttons to rotate sample towards mono
FIGURE 43. Autostage schematic control in Manual window.
6. Rotate the sample a further -15 degrees so that the sample is now at -30
degrees with respect to the vertical axis of the electrostatic lens. Repeat
the optimisation of the y-axis described in (4) above.
Note that during rotating the sample care should be taken that the sample
bar does not collide with the top of the magnetic lens.
7. Rotate the sample a further -15 degrees so that the sample is now at -45
degrees with respect to the vertical axis of the electrostatic lens. Repeat
the optimisation of the y-axis described in (4) above.
8. Repeat steps 6 and 7 so that the sample table now has positions defined
for -60 and -75 degrees. This procedure can also be performed for other
samples on the sample bar.
9. The sample positions for the 4 angles are now defined. These can be
included in an experimental flow chart as outlined in Section 7.3.8.3.
7.3.8.2 Using the rotation about a point routine to define the sample positions
The Vision software has an algorithm that will increment the angle of the
sample whilst keeping the same sample point at the analysis position. This

is useful when ARXPS is required from a specific point on the sample such
as a patterned or inhomogenious sample.
The algorithm relies on the axis of rotation of the auto stage having been
defined in the Vision software. This should be completed during the installa-
tion of the spectrometer. Two points with x, y & z coordinates are used to
define the axis of rotation and can be seen by clicking on the increment
point use rot. axis button, shown in FIGURE 44. If the values in the boxes
are all zero, the axis of rotation has not been set up. If this is the case
please contact a Kratos applications specialist (surface.applications@kra-
tos.co.uk) for further instruction.
increment point using click radio button highlighted

axis of rotation
above to show points defined
for rotating axis (left)
FIGURE 44. The x,y & z coordinates that define the rotation axis.
Using the increment point about the rotation axis algorithm to automatically
define the ARXPS sample positions is achieved as follows:
1. With the sample normal to the electrostatic lens column (sample hori-
zontal) optimise the sample height using snapshot mode so that the
required part of the sample is at the analysis height. The auto Z mode
detailed in Section 7.3.7 could be used to achieve this.
2. Ensure that the position menu option is selected as shown in FIGURE
42. and save the optimised sample position into the sample position
table. Name this position 0 degrees to indicate that the sample is normal
to the lens axis. Follow the instructions below to enter the various angles
required:
3. Left click on the row directly below the 0 degree position so that it is high-
lighted by a black box around the row.
4. Scroll down to the Increment section and left click on the Insert Point
Use Rot. Axis menu option in FIGURE 45. This action will bring up the
defined rotation axis.

FIGURE 45. Increment mode.
5. Enter a number of degrees tilt for each step and the number of steps, or
increments, FIGURE 45. e.g. 15 degrees for each step and 5 increments.
6. This automatically increments the 0 degrees point in the position table by
15 degrees each step for 5 steps. The software uses the axis of rotation
information to keep the initial point at the analysis position while the sam-
ple is tilted. This ensures that the analysis is taken from the same gen-
eral area on the sample at all take off angles.
7. Label each position 15 degrees, 30 degrees etc., FIGURE 46.
FIGURE 46. Position table.
The sample positions have now been defined therefore the next step is to
construct the experimental flow chart.

7.3.8.3 Defining the ARXPS Experiment in Manager

In this section it is assumed that the user has defined a set of sample coor-
dinates in the manual window and these are present in the position table.
The steps required to achieve this are discussed in the previous section.
Here the user is guided through setting up the ARXPS experiment using the
Vision Manager.
1. Chose a new flow chart area or cut the existing flowchart to create an
empty acquisition status window.
2. Select the dataset button and enter the pathname using the browse
button. Modify the dataset name to ARXPS.dset, give an object name
file for the flowchart display and paste the filename object into the flow-
chart region.
3. Select the acquisition button and define a large area survey scan, as
detailed in Section 7.3.1. Note that this lens mode uses the magnetic
lens and will therefore have an acceptance angle of +/- 20 degrees.
Name the flowchart object survey and paste into the acquisition status
window.
4. Make sure that the survey flowchart object is not selected and appears
light grey. Edit the acquisition parameters to define a high resolution, nar-
row region scan over the O 1s, C 1s and Si 2p regions, similar to the
experiment defined in Section 7.3.2. Note that if the Al foil sample is
being used, the Si 2p region should be replaced by Al 2p.
5. Type the name regions and paste into the flowchart after the survey
object.
The flowchart should appear as shown in FIGURE 47.
state change
FIGURE 47. file name, survey and narrow region scans defined in the Manager window.
6. Select the state change button highlighted in Section 47.

7. Select the position table and then load position table software buttons.
The position table with the sample positions for the ARXPS experiment
will now be displayed in the window with each angle on a separate row.
Leaving the dataset name column blank type in angles in the object
name and paste into the flow chart between the file and survey objects.
The flow chart should appear as shown in FIGURE 48.

FIGURE 48. AR stage movements included in flow chart.
8. In the state change window, select the counter button. Type 9 in the
text box for the number of loop back operations required. Name this
object loop and paste into the flowchart after the regions object.
9. To acquire the spectra from all the defined angles, a loop back com-
mand must be included in the flowchart. To do this, highlight the four
objects; angles, survey, regions and loop in the flowchart and right
mouse click on the background region to bring up the menu. Select loop
back and then jump to. The flowchart is now complete and should be
the same as that shown in FIGURE 49.
FIGURE 49. Completed ARXPS flowchart in Manager window.
The jump to operation in the flowchart will ensure that the experiment
moves to the end after spectra have been collected from each of the stage
positions defined in angles. If the jump to operation was omitted from the

flowchart, the loop back operation would dominate and the operation would
simply loop round nine times.
The experimental flowchart can now be submitted and the ARXPS data
acquired automatically. Discussion on processing the ARXPS data in given
in the next Chapter.
7.3.9 Automated Depth Profiling

This section describes the procedure for defining automated depth profiles.
It assumes that the thin film or multi-layer sample to be profiled has been
placed at the XPS position and the correct sample height determined. In
this example a thin oxide coating on tantalum metal is used to demonstrate
the procedure. Such oxide films are easily grown on clean tantalum metal
using a self limiting electrolytic method. Spectra will be recorded using
snapshot mode. This mode is useful for depth profiling experiments (or any
acquisition where a large number of spectrum are recorded) as detector
overscanning time is eliminated leading to significantly shorter total experi-
ment times when compared with scanned spectra. This mode of operation
is not suitable for all samples however, as the region width is determined by
the pass energy and the ultimate resolution is limited. Depth profiles can of
course be defined using standard scanned spectra as well as snapshots.
It is appropriate at this point to make some general remarks concerning

depth profile experiments and how these affect the experimental design.
The aim of the experiment is usually to investigate the composition of a
sample as a function of depth. As XPS is a surface sensitive technique the
depth to which information is gathered from is usually approximately 5 nm.
In depth profiling experiments a XPS spectrum of the surface is recorded
and then a pre-determined amount of the surface of the sample is removed
by ion bombardment. A second XPS spectrum is then recorded of the
newly created surface. These etch / analysis cycles are repeated until the
required depth into the sample is reached. Therefore, the experimental
design must take into account the need for multiple analysis / etch cycles.
The ion gun settings used will be determined by the sample to be analysed
and the information required. As a general guide high beam energies are
used for fast profiles through samples with one or two layers. If multi-lay-
ered samples are to be analysed then lower beam energies will provide
improved inter-layer resolution at the expense of etch rate. Inter-layer reso-
lution can also be improved by using the azimuthal rotation platen.
For a given beam energy and extraction current the etch rate can be varied
by changing the raster size. Increasing the raster size increases the size of
the etch crater produced and decreases the etch rate. It should be borne in
mind that for well defined depth profiles edge effects must be reduced to a
minimum. This means in practice that etch craters should be at least ten
times the size of the analysis area. Hence, if an analysis area of approxi-
mately 100 microns is used then the etch crater must be at least 1 mm
square.
The Vision acquisition software can be used to turn the Ar gas supply on
and off at the start and end of a depth profile experiment. This is achieved

by including a state change object in a flow chart and is of great benefit in

reducing the gas load on the ion-pump in the sample analysis chamber.
The steps required to produce an atomic concentration depth profile are out-
lined below:
1. Choose a new flow chart area, or cut the existing flowchart to create an
empty acquisition status window.
2. Select the dataset button and enter the pathname using the browse
button. Name the dataset Ta_depth_profile.dset, give an object name
file for the flowchart display and paste the filename object into the flow-
chart region.
3. Select the state change and the ion gun gas radio buttons as shown in
FIGURE 50. This state change object can be used to switch on or switch
off the Ar gas depending on the option selected in the gas state pull
down menu.
gas on object pasted into

flowchart region
FIGURE 50. Ion gun gas status in state change box.
Select switch on as shown above and type gas on in the name box.
Paste this object into the flow chart.
4. Select the acquisition button, the following settings should be entered to
define the snapshot from a defined area using the 55 um aperture, FIG-
URE 51.
Analyser section:
Lens Mode: FOV 2 - Small Spot
Resolution: Pass energy 160eV
110um

Anode: Al (mono)

Emission: 15mA
Acceleration Volts: 15kV
FIGURE 51. Analyser mode for a typical depth profile.
Slot mode is avoided as the etch crater formed is usually not significantly
larger than the area analysed. Hence the profile would show significant arti-
facts due to crater edge effects.
5. Set up the snapshot spectra by entering the following information into

the Scan Control, FIGURE 52.
Type: Snapshot
First Region Name: O 1s
Centre eV: 533.95
Dwell ms: 20000
# Sweeps: 1
Second Region Name: Ta 4f
Centre eV:
Dwell ms: 20000
# Sweeps: 1

FIGURE 52. Scan control for a typical etch.
6. Give an object name acqn for the flowchart display and paste the acqui-
sition object into the flowchart region.
N.B. When performing snapshot spectra it is important that only one sweep
is selected or that if multiple sweeps are required that only one region per
object in the flow chart is used. This is because if multiple O 1s and Ta 4f
sweeps were selected in the same acquisition object then the analyser volt-
ages would have to jump between O 1s and Ta 4f between each sweep.
This would limit the speed advantage of the snapshot mode and reduce the
accuracy of the results as lens settle times would become important.
7. Select the State Change button then the Ion Gun Etch button, FIGURE
53.
FIGURE 53. Ion Gun etch object.
8. Enter an object name etch for the flowchart display and paste the ion
gun etch object into the flowchart region. An audible beep will be heard to
warn the user that the etch times have not been entered correctly. Ignore
this warning for the moment.

9. Set up the etch parameters by left clicking on the 4kV (no float) row in
the table so it is highlighted by a black box and then left clicking on restore
row button, FIGURE 54.
enter raster size
define post gas on standby time
click on the 4kV(no float row) and

press restore row button
FIGURE 54. Ion gun table.
N.B. The choice of ion gun settings is determined by the experiment to be

performed. See Chapter 5 for more details.
10.The Post Gas On Standby Time must be defined in minutes. This

option will cause the ion gun to pause for the defined time before the first
etch cycle. This is an important parameter as the ion gun may take several
minutes to stabilise after it has been switched to standby by the software.
Note that this delay only occurs in the first cycle as it is assumed the ion
gun will need to stabilise when it is turned on but then will remain in the
standby state inbetween subsequent etch cycles.
11. Set the desired raster size, in this example 3.
12. Set the following etch parameters, FIGURE 55.

Pre-Etch Delay (s): 10
Post-Etch Delay (s): 10
Start Etch Time (s): 30

Etch Cycles: 30
FIGURE 55. Etch time and number of cycles.
13. All the components of the etch experiment have been defined but we
must now ensure that the instrument completes the requested number of
cycles. Move to the flow chart and select the acqn and the etch objects.
14. Right mouse click to bring up the pop up menu, FIGURE 56.
FIGURE 56. Loop back pop up menu.
15. Left click on the Loop Back to make the instrument complete the
requested number of etch cycles, FIGURE 56.
16. Assuming that another depth profile experiment is not to be attempted,

an ion gun gas off state change object should be included in the flow chart.
The completed flow chart should be the same as that shown in FIGURE 57.

Acquisition Conditions Reference Sheet
FIGURE 57. Completed depth profile experiment.
17. If the ion gun gas on option has not been included in the flowchart
before submitting the experiment it is first necessary to set the ion gun to
stand-by. Follow the instructions outlined in Chapter 5 to set the gun in the
stand-by mode with the argon gas flowing.
18. Once the requested ion emission current has been reached and stabi-
lised the experiment can be submitted.
7.4 Acquisition Conditions Reference Sheet
Note that these parameters should only be considered as a reasonable

starting point. Acquisition parameters must be optimised depending on the
instrument or the overall experimental goal.
Charge Neutraliser Conditions
Exact conditions will vary dependent on instrument;

Charge balance 2.4 - 3.6 V
Filament current 1.6 - 2.1 A
Filament bias 1 - 1.6 V

Spectroscopy (based on use of monochromatic x-ray source)
TABLE 1. Large area (300x700m) - slot aperture.
pass energy acqn time /

spot size lens mode / eV step size/ eV mins
survey Hybrid 160 1 1-3
region Hybrid 10 or 20 0.1 1 - 10
Valence Hybrid 20 - 40 0.2 5 - 20
band
TABLE 2. Small area - small area spectroscopy must be acquired using the lens mode
indicated for the correct analysis area
*pass energy acqn time /

spot size lens mode / eV step size/ eV mins
110um FOV 2 10 - 40 0.1 1-4
55um FOV 2 10 - 40 0.1 1 - 10
27um FOV 2 20 - 40 0.1 3 - 15
15um FOV 2 20 - 80 0.1 - 0.2 5 - 20
* use 160 eV pass energy for selected area survey scans
TABLE 3. Parallel imaging (elemental)
experiment lens mode (FOV) PE / eV Acqn. time / min

general alignment FOV 1 160 1
(900m2)
small area spectroscopy FOV 2 160 1-5
position referencing
(400m2)
Highest lateral resn FOV 3 160 2-8
(250m2)

TABLE 4. Chemical State Parallel Images and spectra from images
lens mode
experiment (FOV) PE / eV Acqn. time / min
general alignment FOV 1 160 1
(900m2 )
small area spectroscopy FOV 2 40 or 80 1 -10
position referencing 2
(400m )
Highest lateral resn FOV 3 40 or 80 3 - 15
(250m2)

13 July 2009
Chapter 8
Vision Processing
Software
Kevin Good.
This chapter is split into two sections. The first section will describe the
processing of data that was acquired in the Data Acquisition chapter in a
step by step manner. This will introduce the user to the commonly used fea-
tures available in the Vision Processing software package for data reduc-
tion and report generation.
The second part of this chapter is a reference section that provides a com-
prehensive review of the Vision Processing software package.
The Vision Processing software package runs independently of the Acqui-

sition software and can be opened and closed without detrimental effects to
acquisition routines that are presently running.
257
Examples of data processing.
8.1 Examples of data processing.

The data acquired in the previous chapter will be used to demonstrate the
typical steps involved in quantification of survey spectra and narrow scans.
The dataset that was created is called Al_foil.dset and contains two survey
scans and narrow region, high resolution scans of the O 1s and Al 2p photo-
electron lines.
To start the software, double click on the Processing icon and the Vision
Processing window will appear as shown in FIGURE 1.
FIGURE 1. The Vision Processing window.
8.1.1 Quantifying a large area survey spectra.
1. Select File > Open Data for Processing and open the Al_foil.dset as
shown in FIGURE 2.
FIGURE 2. Al_foil.dset opened for processing in the Vision Processing window.
258 Chapter 8 Vision Processing Software

2. Select the first survey data object by clicking it with the left mouse button
(the data object should turn black).
3. Select Options > Processing to load the selected survey scan into the
Processing window as shown in FIGURE 3.
FIGURE 3. The Processing window showing the Al_foil.dset survey spectra.
4. Ensure Quantify > Quantification Regions is selected.
The survey scan (shown in FIGURE 3.) contains photoemission peaks due
to oxygen, carbon and aluminium. We shall therefore proceed with the
quantification by defining O 1s, C 1s and Al 2p quantification regions.
5. Type O 1s in the Name column of the first row of the region table and
press enter.
The region table parameters will be automatically filled in from the Element
Library and the region be superimposed over the spectra in the display sec-
tion. A linear background is defined for the O 1s region by default.
Chapter 8 Vision Processing Software 259

Due to physical effects like charging the Start and End positions defined in
the element library might not be appropriate and may need adjusting.
6. In the region table click inside the O 1s text box to highlight the row.
7. In the display section left click and drag a box around the O 1s peak.
8. In the display section right click and select Zoom in.
The display will zoom into the defined box. We can now redefine the Start
and End energies for the O 1s quantification region.
9. In the display section left click at the high binding energy where the region
should start and drag to the low binding energy side of the peak where
the quantification region should end.
10. Select the O 1s row in the region table and press enter to accept the new
region.
A suitable range for the O 1s region is shown in FIGURE 4.
FIGURE 4. Redefinition of the O1 s Quantification Region.
11. In the display section right click and select Zoom Out > Fully.

12. Type C 1s in the Name column of the second row of the region table
and press enter.
13. Type Al 2p in the Name column of the third row of the region table and
press enter.
14. Redefine the regions around the C 1s and Al 2p photoemission peaks in
the same way as defined for the O 1s region.
To save the defined regions in the spectra data object (so that they are
present if the dataset is closed and reopened) they need to be applied.
15. Press the Apply button.
8.1.2 Survey spectra quantification report generation.
Having defined regions for the survey spectra the next step is to generate
the quantification report.
1. In the Vision Processing window, select the first survey data object in
the Al_foil dataset.
2. From the menu bar select the Options > Browser Actions. Along the top
row are a set of options, click on the Profile Spectra selection arrow.
3. In the Quantify Using section select Region.
4. In the Quantify By section select Area.
In this example, there are no independent variables, so this section may be

ignored as can the smoothing section. The options should be as depicted in
FIGURE 5.
FIGURE 5. Browser Actions > Profile Spectra options for Region quantification.
5. Press the Display in Window button.

The generated quantification report will appear on the screen as depicted in

FIGURE 6. The report can be printed via the Print menu in the Quantifica-
tion Report windows menu bar.
FIGURE 6. Region Quantification Report for the first survey spectra in the Al_foil dataset.
8.1.3 Propagation of defined regions to other spectra.
Processing that has been applied to one spectra can be propagated to other
spectra in the same or different datasets. This will be demonstrated by prop-
agating the Quantification Regions defined in the first survey spectra onto
the second survey spectra in the Al_foil dataset.
1. In the Vision Processing window select both survey data objects in the
Al_foil dataset.
2. Select Options > Processing to load the spectra into the Processing
window and select the History option.
The defined regions of the first survey spectra will appear superimposed on
the spectrum, as shown in FIGURE 7.
3. Use the right hand scroll bar in the display section to advance the display
to the second survey spectra.
The user should note that there are no regions associated with this spectra.
4. Scroll back to the survey spectra that has the regions defined.
The processing History associated with the displayed spectra will be shown
in the table. Here, the only applied processing is Quantification Regions.
5. Ensure both the Active button in the Quantification Regions entry in the
history table and the Start from Raw Data buttons are selected.
6. Press the Apply button.
Scrolling to the second spectra will show that both spectra now have defined
Quantification Regions.

History selection
Processing options
History table
Use to scroll
to next spectrum
FIGURE 7. The History section of the processing window.
A quantification report must be generated separately from each survey

spectra using the steps outlined in Section 8.1.2. otherwise a single (aver-
age) quantification report will be produced. This is because the objects are
not separated by a state change data object. If a state change data object
(e.g. a stage movement) were present a quantification report would be gen-
erated from each survey spectra. Two spectra from different datasets will
result in independent reports displayed in the same Quantification Report.
8.1.4 Peak synthesis and curve fitting.
This section is intended to demonstrate the extraction of chemical informa-

tion from high resolution spectra. By way of example the procedure for cre-
ating synthetic line shapes representing the chemically modified states of
aluminium will be described and how stoichiometric relationships can be
exploited to identify the underlying lines that are responsible for the
observed Al 2p photoemission peaks in an XPS spectrum.

1. In the Vision Processing window select the Al 2p data object from the
Al_foil dataset.
window.
3. Ensure the Quantify option is select and that Quantification Options is
set to Quantification Regions.
4. Type Al 2p in the Name column of the first row of the region table and
press enter.
FIGURE 8. The Al 2p spectra with a defined Quantification Region.
The standard parameters that are stored in the Element Library will be
entered into the table and the region defined in the display section as shown
in FIGURE 8.
5. Again the default region from the element library might not be appropri-
ate. If so Modify the Start and End positions as described earlier.
Note that the Start and End values displayed in the region table change as
soon as the mouse button is released, but the new values do not become
active until the enter key is pressed.

Once a Quantification Region (and hence a background) is defined, syn-

thetic components can be generated. The chemical information apparent in
the Al 2p spectra results from the elemental Al 2p which is spin-orbit split
into two components Al 2p1/2 and Al 2p3/2 and a single peak due to Al oxide
(which is a common approximation for the Al 2p1/2 and Al 2p3/2 components
of the oxide). It is known that the theoretical area ratio of the spin-orbit split
Al 2p1/2 and Al 2p3/2 is 1:2.
We will now proceed to define synthetic components to represent each of

the Al 2p components with the aim of extracting the chemical information.
6. Select Quantification Options > Components.
7. Ensure the GL(30) option is selected in the Model section.
8. Type Al 2p in the Name column of the first row in the component table
and press enter.
Duplicate
component
section
Auto-Fit
components
section
FIGURE 9. Al 2p component defined in Processing window.
A synthetic component will be fitted to the part of the Al 2p spectra with the
highest counts. In this example this corresponds to the aluminium oxide
component of the spectrum as shown FIGURE 9. Another synthetic compo-

nent is needed to fit the peak in the Al 2p spectra with the next highest
counts.
9. Type Al 2p in the Name column of the second row in the component
table and press enter.
From the Al 2p spectra it is apparent the second peak is comprised of more

than one component. We will now use the Duplicate Component section to
create a third Al 2p synthetic component from the second Al 2p synthetic
component that has the required area ratio of 1:2.
10. Select the second Al 2p row in the component table by clicking the any
of the rows text boxes.
11. In the Duplicate Component section (FIGURE 9.) set the Offset, Width
Factor and Height Factor parameters to 0.4, 1.0 and 0.5 respectively,
then press enter.
12. Press the Duplicate button.
A third Al 2p synthetic component will be generated that has the same

Width, half the Height and is 0.4 eV shifted to higher binding energy rela-
tive to the selected Al 2p synthetic component, as shown in FIGURE 10.
FIGURE 10. The result of the Duplicate Component operation.

Before any autofitting is applied to improve the fit between the defined
synthetic components and the data, the two Al 2p elemental synthetic com-
ponents must be grouped into an ensemble so that the 1:2 area ratio is
maintained during the auto fit. It is important that the steps are followed in
exactly the order outlined below to ensure that the two synthetic compo-
nents are linked together to form an ensemble. The ensemble may then be
altered independently of the synthetic component due to the aluminium
oxide to give the best fit of the model curve to the actual data.
13. Select the Linked Components option from the Quantification Options
pull down menu.
14. Click inside the Name box in the row directly below the Unlinked row in
the ensemble table. Enter the label spin and press enter. The RSF and
Atomic Mass entries will automatically default to 1.
15. Select Width and Height in the Linked Parameters section and ensure
the Position is deselected as shown in FIGURE 11.
Linked
Components
Option
FIGURE 11. The Linked Components window.
In this example the ensemble was labelled spin to indicate that the two
linked synthetic components in the ensemble are the spin-orbit split syn-
thetic components of elemental aluminium. The Width and Height of the

synthetic components will be fixed but their relative positions will be allowed
to change, as the spin-orbit splitting defined when duplicating the synthetic
components may not be precise. Note that the Unlinked row cannot be
edited or deleted.
16. Move back to the Components window using the pull down menu.
17. Highlight the second Al 2p row in the component table, type spin in the
Ensemble Name text box and press enter.
Note that the ensemble name must be exactly the same as that defined in
the Linked Components ensemble table and that the text is case sensitive.
18. Highlight the third Al 2p row in the component table, type spin in the
Ensemble Name text box and press enter.
The two synthetic components are now linked so that their relative heights
and widths remain fixed. The position of each synthetic component remains
independent. To complete the fitting procedure it now becomes necessary to
auto-fit the components.
19. Press the Auto-Fit button.
Auto-Fit attempts to minimise the residual between the model envelope

and the data. To review the residual plot, the residual plot window must be
opened up by clicking and dragging either of the two tabs indicated in FIG-
URE 12. The stoichiometric relationships and the relative positions of the
synthetic components may not be exact and it may be necessary to relax
some of the relative areas and positions for the synthetic components to
achieve a good fit.
At this point it is wise to Apply the processing steps to the spectra so that
they will be saved.
20. Select Quantification Options > Components and press Apply.
21. Select Quantification Options > Linked Components and press Apply.
22. Select Quantification Options > Auto-Fit Components and press
Apply.

Left click and

drag to open
residual plot
window
Correctly fitted
Al 2p spectrum
from Al foil
FIGURE 12. Residual display between the model envelope and spectral data.
8.1.5 Components quantification report generation.
In the example above, all the synthetic components have the same name,
therefore, a quantification report would report 100% atomic concentration of
Al 2p. It is necessary to rename the synthetic components.
1. Select Quantification Options > Components.
2. In the Name columns of the first three rows of the component table type
Al oxide, Al elem and Al elem respectively (pressing enter for each).
We can now determine the relative concentration of the elemental alumin-

ium to aluminium oxide in the quantification report.
3. In the Vision Processing window, ensure the Al 2p data object in the
Al_foil dataset is selected.
4. Select Options > Browser Actions and click on the Profile Spectra
selection arrow.
5. In the Quantify Using section select Component.


FIGURE 13.
FIGURE 13. Browser Actions > Profile Spectra options for Component quantification.

FIGURE 14. The report can be printed via the Print menu in the Quantifica-
tion Report windows menu bar.
FIGURE 14. Quantification Report for Al 2p spectra from the Al foil dataset.
8.1.6 Components and regions quantification report generation.
During quantification it is often required that certain regions be quantified

using synthetic components as in the Al 2p example above. However, for
other regions it is not always necessary or indeed practical to define a syn-
thetic component. In these cases quantification by region would suffice. We
shall now demonstrate how quantify by synthetic components and regions.
Start with the Al_foil dataset with the Al 2p processing completed as in the
previous section opened up in Vision Processing.

1. In the Vision Processing window select the O 1s data object from the
Al_foil dataset.
window.
3. Select Quantification Options > Quantification Regions.
4. Type O 1s in the Name column of the first row of the region table and
press enter.
5. Modify the Start and End positions of the background by left clicking in
the display section and dragging a box across the BE range required for
the background and press enter.
A suitably defined O 1s region is shown in FIGURE 15.
FIGURE 15. The O 1s spectra with a defined Quantification Region.
We can now determine the relative concentrations of the elemental alumin-

ium, aluminium oxide and oxygen in the quantification report.
6. In the Vision Processing window, select the Al 2p and O 1s data
objects in the Al_foil dataset.
7. Select Options > Browser Actions and click on the Profile Spectra
selection arrow.
8. In the Quantify Using section select Component.

9. Select the Default to region option that appears when Component is

selected.

FIGURE 16.
FIGURE 16. Browser Actions > Profile Spectra options for Component quantification with
Default to region selected.

FIGURE 17. The Al oxide and Al elem quantification rows are Type
labelled Comp indicating that they have been quantified using synthetic
components. The O 1s row is Type labelled Reg indicating it has been
quantified using the defined region. The report can be printed via the Print
menu in the Quantification Report windows menu bar.
FIGURE 17. Quantification Report for Al 2p and O 1s spectra from the Al foil dataset using a
combination of synthetic components and defined regions.
This now ends the examples of data processing. The next section will
describe in detail the relevant functions of each section of Vision Process-
ing.

Reference section.
8.2 Reference section.
This section is designed to be used as a reference guide to the options

available in the Vision Processing software package.
8.2.1 Vision Processing.
Menu options
Browser mode Current dataset

selection name
Dataset comment
Dataset scrollbar Scratch data

objects browser
area
Object names Data objects

browser browser area
Data objects
browser
scrollbars
FIGURE 18. The Vision Processing window.
The Vision Processing window as depicted in FIGURE 18. consists of the

following:
A menu bar used to start up the different sections of the application.
Radio buttons to toggle the data object view mode.
A status area to display the name of the selected open dataset file.
A dataset comment area.
A Scratch section for temporary storage of data objects.
Ten browser sections which allow the user to browse through the contents of the
datasets and select data objects for processing.
A background menu pop-up that can be invoked by right clicking in the Scratch
object area or the data object browser areas.
Each part of the Vision Processing window now will be covered in detail,
starting with the menu bar options.

Reference section.
8.2.1.1 File.
The options available under the File menu are:
Open dataset for processing. This menu option will open a dataset that
can subsequently be modified by processing operations but no new data
can be put into the dataset. A maximum of 10 datasets may be opened at
any one time. A dataset may be opened for processing using this option,
even if it is open and receiving data in the Manager window. The data
objects will not appear in the Processing window until the acquisition has
completed - and the object is no longer pink when viewed in the Manager
window in follow mode. Note, to view the newly acquired dataset the Data-
sets option in the Browser Mode section will need reselecting to refresh
the display.
Open dataset for new data. This option allows the user to open a dataset
which will be displayed in the main processing window and then save data
objects into the dataset. This is useful when the user wishes to save an
object from the temporary Scratch file into a specific dataset. A dataset that
has been opened using open dataset for new data is identified by the note
Append in the top right hand corner of the display, as shown in FIGURE 19.
Append
Dataset opened using Open Dataset for New Data
FIGURE 19. Dataset opened for new data in the processing window.
Note that data in a dataset that has been opened using this option cannot
be processed. The dataset must be closed and reopened using the open
dataset for processing menu option.
Furthermore, a dataset may only be opened for new data once within the
Vision suite of software. If a dataset is currently open and data objects are
being saved in the Manager section of Vision it will not be possible to use
this option to open the same dataset in Vision Processing.
Clear scratch. Selecting this option will delete all the objects from the
scratch area. The scratch area is only a temporary file and once deleted the
objects can not be restored.

Reference section.
Close specific.dset. When a single dataset is selected in the main

processing window (by highlighting an object in that dataset) this command
will close that specific dataset.
Close all datasets. This closes all datasets that are currently open in Vision
Processing, leaving the Scratch area unchanged.
Close all datasets and clear scratch. This option will close all datasets
that are currently open in Vision Processing and also clear the Scratch
area.
8.2.1.2 Options.
The Options menu allows the user to open other windows associated with
data processing. The menu options are:
Display - Invokes the Display window and transfers any selected data
objects (spectra/images) into the window, see Section 8.2.2.
Processing - Invokes the Processing window and transfers any selected

data objects into the window, see Section 8.2.4.
Browser Actions - Invokes the Browser Actions window that contains var-
ious options that allow the user to extract information from processed spec-
tra and images, see Section 8.2.5.
Element List - Invokes the Element List window that contains a scrolling
display of photoemission and Auger peak positions, see Section 8.2.6
Version Information - Invokes the Version Information window displaying

the current version of Vision Processing.
8.2.1.3 View.
The View menu contains the single option Filter which invokes the
Browser Filter, see Section 8.2.9.
8.2.1.4 Data object view modes.
At the top left of the main processing window are a pair of radio buttons
which allow the user to choose between two different view modes for the
data objects, as depicted in FIGURE 20. The default setting is the Datasets
view mode, FIGURE 20. (a), where all objects (except those excluded by
the filter) are present.

Reference section.
(a) Datasets
view mode. All
data objects are
displayed.
(b) Selection
view mode. Only
the selected
data objects are
displayed.
FIGURE 20. Vision Processing windows depicting the Datasets and Selection view modes.
If only a sub-set of these data objects are of interest, the user may select the
interesting ones and then change to Selection mode, FIGURE 20. (b). This
causes all un-selected objects to be removed from the screen. The function-
ality of the browser sections remains the same in both view modes. N.B.
data objects in the Scratch area remain visible in both view modes.
8.2.1.5 Current Dataset.
The current dataset area is uneditable and simply displays the name of the
currently selected open dataset.
8.2.1.6 Dataset comment area.
The dataset comment area simply displays any comments associated with
the selected open dataset. The dataset comment area is editable and is
associated to the whole of the opened dataset NOT to the individual data
objects within the dataset.
8.2.1.7 The Scratch section.
Once a dataset has been opened, the Scratch section of the browser
appears at the top of the browser. This is not associated with any disk file

Reference section.
but receives objects created by the Browser Actions window. Any objects
which are required permanently must be transferred to another dataset. If
you wish to discard the contents of the scratch area, left click on the word
Scratch and use the Close Dataset option on the File Menu; this empties
the scratch area and the discarded objects can not be recovered. It is not
possible to visually remove objects in the scratch area from the screen by
using the Selection view mode option.
8.2.1.8 Data object selection mechanisms.
The browser shows the user the data and state change objects in currently
open datasets. The user selects a number of these objects for display and
processing. Only these selected objects are available to the rest of the pro-
gram. A data object appears in the browser as a small light coloured rectan-
gular block (see FIGURE 20.). Once selected (by clicking with the select
mouse button for example), the block changes to a darker colour.
There are several ways of selecting and de-selecting data objects from the
browser:
Basic selection - Point at a data object and click the select mouse button.
This selects a single object and de-selects all other objects. Clicking with the
mouse pointer, when the mouse is pointing at the background in the
browser, de-selects all objects.
Use of the shift key during selection - When selecting items from the
browser window, if an item is selected first, and then the shift key is
depressed whilst a second item is selected, this will cause all items between
the first selection and the second selection to become selected.
Use of the control key during selection - The control key is used in a sim-
ilar manner to the shift key except when the control key is pressed, selecting
an object simply adds that object to the selection and does not affect any
other object. Control clicking on a selected object de-selects it.
Selecting a complete row - Inside the browser window, each row of data
objects has a different name. Clicking the select mouse button whilst the
pointer is over this name will select a complete row from within the window.
Selecting a complete dataset - Clicking the select mouse button whilst the
pointer is over the dataset name will select the complete dataset.
Multiple selection via the mouse - The mouse can be used to select a
series of objects by depressing the select mouse button and dragging out a
box surrounding the required items. The limitation on this is that only a rec-
tangular area can be dragged out.
Selection via the selection bar - At the top left hand corner of the data
object browser is a small black box, (see FIGURE 19) This box can be
stretched to the pitch of the dataset items which should be selected.
Clicking on a name in the object name browser activates the selection bar
for that row of data objects. Clicking on the dataset filename in the object
name browser activates the selection bar for the whole dataset. When the

Reference section.
selection bar is activated, the first data object in a row will be selected fol-
lowed by a gap of the number of data objects which fit the pitch of the selec-
tion bar. This feature can be used, for example, to select every other or
every third object in the dataset as in FIGURE 21.
Selection
bar pitch.
FIGURE 21. Data object selection via the selection bar.
Selection of data objects applies, not just to the browser, but program wide.
Data objects must have been selected before they are available in the Dis-
play, Processing and Browser Action windows. Once a data object is dis-
played, it is possible to add or remove it from the selection from within the
window where it is displayed. This is done by pointing at the displayed data,
instead of the object in the browser; the control key may be used as
described above to select or de-select individual objects. This has exactly
the same effect as if the selection or de-selection was done from the
browser. The browser will immediately darken or lighten the colour of the
data object to reflect changes to the selection done from other windows. De-
selecting an object which is displayed does not cause it to disappear from
the Display or Processing window.
8.2.1.9 Background menu pop-up.
A background pop-up menu is available from the Scratch and browser data
object areas by clicking the right mouse button. The pop-up menu options
are:
Display - The Display window is invoked if it is not already present. All

selected objects are each pasted into separate tiles in the display window.
Note that the selected objects do NOT need to be in the browser panel from
which the background menu is invoked. Any previously existing contents of
the display window are discarded.
Processing - The Processing window is invoked if it is not already present.

All selected objects are each pasted into separate tiles in the display area.
Note that the selected objects do NOT need to be in the browser panel from
which the background menu is invoked. Any previously existing contents of
the display window are discarded.

Reference section.
Save Selection - This has effect if the dataset in the browser section was
opened for new data (the word Append will be in the top right of the panel).
All currently selected objects are appended to the dataset and immediately
written to disk. If the dataset was not opened for new data this option has no
effect. In the Scratch area the selected datasets are copied, but NOT writ-
ten to disk (there is no disk file associated with the Scratch section).
8.2.2 Display window.
At the top of the Display window is a menu bar containing two menus
labelled Options and Print. The Options menu allows the way the data is
displayed to be configured via the following windows:
Tile Display (Section 8.2.7).
Page Display (Section 8.2.8).
Colour Editor (Section 8.2.10).
The Print option allows the contents of the display window to be printed via
the print dialogue (Section 8.2.11). Each area within the Display window
that contains a data object is called a tile, a typical view is depicted in FIG-
URE 22.
FIGURE 22. The Display window.
8.2.2.1 Display window selection mechanisms.
There are a number of different selection mechanisms tied to the Display

window. These include:

Reference section.
Using the paste mouse button to drag data objects from the Vision Processing
Scratch or browser data object areas to the Display window. This pastes all
selected objects into the window, each in its own tile, removing any previous
contents.
Using the select mouse button, data objects in the Scratch or browser areas may
be selected or de-selected by pointing at a tile in the display window as described
in Section 8.2.1.8.
The coordinates at the pointer within the graphical display are displayed as text
when select button is pressed. In the case of images, the intensity at the point and
the offset from the initial position are also displayed. These numbers are con-
stantly updated as the mouse is moved with the select button held down.
If the Element List window is open then it displays a range of energies centred
on the energy at the pointer when the mouse select button is pressed. The energy
list scrolls if the mouse is moved with the select button held down.
Holding the mouse select button down within a Display window tile and mov-
ing it draws out a rectangular area. Releasing the button defines that area as an
area that can subsequently be zoomed into (see Section 8.2.2.2).
Using the select mouse button to point to a specific tile in the Display window
and then clicking the mouse paste button. All data objects that are individually
displayed in the Display window will be pasted into the selected tile. In the
case of images, no more than three will be visible.
Clicking the right mouse button in the display area invokes the background
pop-up menu with the following options:
Zoom In - Zooms into a previously defined rectangular area (see Section

8.2.2.1). If required, you can zoom in repeatedly to smaller regions.
Zoom Out - There are two sub-options: Partially and Fully. The latter
undoes the last zoom-in action and the former undoes all previous zoom-in
actions. If you have only zoomed-in once both sub-options result in the
same action.
Export Tile - The only sub-option available is Data to an ASCII File. This
option can be used to export the currently displayed spectrum to an ASCII
type file. This file can then be imported into other windows based programs
such as Excel. Selecting this option invokes a dialogue window allowing the
user to specify the file name and location, enter a file name and click on OK.
A typical generated file is shown in FIGURE 23.
Display - This invokes the Display Parameters Window (Section 8.2.7)

which is also available via Options on the menu bar.
Colour Scale - This invokes one of the two forms of the Colour Editor win-
dow (Section 8.2.10) dependant upon the type of displayed data object
(spectra or image).

Reference section.
FIGURE 23. ASCII formatted data imported into Microsoft Excel.
If there are any components defined within the data object and the Display
Regions and Data option in Display Parameters (Section 8.2.7) is set then
the synthetic components will be exported in the columns after Back-
ground.
N.B. to use the data for quantification each data point must be divided by
the transmission value at that energy. Always check that the quantification
results produced are the same as those produced in the quantification
report, see Section 8.2.5.3.
8.2.3 Overlaying Objects in the Display Window
As mentioned briefly in section Section 8.2.1.8 objects such as spectra and

images may be displayed overlaid together in a single display tile. To over-
lay objects simply select the objects that you wish to overlay, move the
mouse pointer to the display window and press the middle mouse button to
paste the objects in the display window.
This feature is particularly useful when several small spot images have been
recorded from a sample where a parallel image has been used to define the
positions. To display the analysis positions on the parallel image simply
select both the parallel image and small spot objects, FIGURE 24. Move the

Reference section.
mouse pointer over the display window and paste all the objects into the real
time display window. The parallel image will be displayed with labels indi-
cating the analysed points, FIGURE 25.
FIGURE 24. Objects selected.

Reference section.
FIGURE 25. Image overlay.
8.2.4 Processing.
At the top of the Processing window is a menu bar containing two menus
labelled Options and Print. The Options menu allows the way the data is
displayed to be configured via the following windows:
Tile Display
Colour Editor

Reference section.
The Print option allows the contents of the display window to be printed via
the print dialogue (Section 8.2.11). The remainder of the Processing win-
dow is split into two main areas, the top area being the processing control
section, and the bottom area being the display section, see FIGURE 26. The
display section is very similar in operation and appearance to the Display
Window, but with only a single tile permitted on the page and no overlaying
of data objects. The control section allows the user to choose processing
operations, set associated parameters and then apply them to a single
spectrum or image or series of spectra or images.
Before an object or series of objects are available for processing they must
have been selected using the browser and/or display windows and pasted
or dragged and dropped into the Processing window display area. Only
one object will be visible at a time, but the scroll bar can used to view each
in turn. The usual sequence of operations is to select (using the browser
and/or the display window) one or more spectra or image data objects and
paste them into the Processing Window display. Then some processing
operations can be applied to the visible data whereupon the display
changes to reflect the changed data and the results are written into the data-
set.
FIGURE 26. The Processing window.

Reference section.
Also written into the dataset is a record of the processing operations done
and the original (raw) data is also preserved. When the user is satisfied with
the results, the same sequence of operations can be automatically applied
to all the other data objects. Often, a series of objects will be processed and
then used in the Browser Actions Window to create new data objects such
as depth profiles.
The processing control area contains a number of radio buttons each allow-
ing the selection of a particular operation. Some of these operations have
parameters associated with them. At the bottom of the display area there is
an Apply button, which is used to carry out the selected operation on the
dataset which is currently visible or, in some cases, all the datasets currently
in the Processing window display area.
8.2.4.1 Smooth.
Applicable to XPS, AES and ISS spectra, linescans, SIMS and SNMS pro-
files. The Method menu offers a choice of two types of smoothing algo-
rithms:
Savitzky-Golay - Performs a local polynomial regression (of degree k) on a

distribution (of at least k+1 equally spaced points) to determine the
smoothed value for each point. The approach tends to preserve features of
the distribution such as relative maxima, minima and width, which are usu-
ally 'flattened' by other adjacent averaging techniques (e.g. moving aver-
ages). The Kernel Width free parameter controls the number of data points
within the smoothing kernel. A large value results in a wide convoluting pol-
ynomial, giving greater smoothing, more broadening of features, and
greater suppression of narrow peaks. The Kernel Width in points is
reported for the users information. This is calculated by dividing the Kernel
Width by the step size of the experiment and is rounded down if necessary
to ensure that the number of points is odd. The supported degrees (k) are
Linear, Quadratic and Quartic. N.B. The Linear Savitzky-Golay Kernel
Width is fixed at three data points and cannot be altered.
Gaussian convolution - Convolutes the data with a Gaussian. The full

width half maximum (FWHM) of the convoluting Gaussian is the free
parameter. A greater FWHM results in more smoothing, more broadening of
features and the suppression of narrow peaks. It may be useful to bear in
mind that when a Gaussian of FWHM a is convoluted with another of FWHM
2 2
b, the result is a Gaussian of FWHM a +b .
8.2.4.2 Differentiate.
Applicable to XPS, AES and ISS spectra, linescans, SIMS and SNMS pro-
files. There is a choice of two variants of a Savitzky-Golay differentiation
algorithm, selected from the method menu.
At each data point in the spectrum, a polynomial of given degree (Quadratic

or Quartic) is fitted to a number of data points centred on the one under con-
sideration, and the required derivative at that point is calculated as the
equivalent derivative of the least squares fit polynomial at the same
abscissa value. The Kernel Width parameter controls the number of points

Reference section.
over which the fit is calculated. Too narrow a width results in the noise in the
original spectrum dominating, whereas too wide a width results in excessive
smoothing, with narrow peaks obliterated.
8.2.4.3 Integrate.
This operation is applicable only to XPS, AES and ISS spectra, linescans,
SIMS and SMNS profiles. Integration can be performed from left to right, in
x
which case the result is x f(x')dx' ,
1
or right to left, leading to the result
x
x f(x')dx' ,
2
where x1 and x2 are the lower and upper abscissa bounds,
respectively, and f(x') is the intensity of the original spectrum at abscissa x' .
8.2.4.4 Deconvolute.
The finite width of a photoelectron peak has contributions from a number of

factors:-
a) an intrinsic energy spread (the real line width) arising from quantum
uncertainty effects (the interaction of core hole lifetime and Heisenberg
uncertainty).
b) solid state broadening (matrix interaction) and intrinsic loss effects (ine-
lastic scattering).
c) the width of the exciting X-ray line.
d) the finite resolution of the analyser.
The first two are essential features of the data; the latter two are undesirable
adjuncts of the measuring process which deconvolution seeks to eliminate.
The theoretical limits to instrument resolution is likely to be about 70meV for
the analyser itself (at 5eV pass energy), and about 150meV for a monochro-
matic Al K1 line source (non-monochromatic Mg K1,2 = 0.6eV approxi-
mately).
The convolution function (instrument broadening function, A ( x x' ) )

used in Vision is gaussian, the half width of which must be user specified.
The approach to deconvolution involves Fourier transforms and manipula-

tion of the transformed spectrum in the frequency domain. The convolution
function modifies the spectrum frequency response, emphasising high fre-
quency components, so noise is generally amplified as well as the peak
being narrowed.
If the convolution function width is set too high then noise may be amplified
excessively and large oscillations (ringing) on the shoulders of peaks, may
be produced. Also, due to end effects, similar oscillations are likely at
either end of a spectrum, so convolution may be useless if the peak is too
close to one end.
8.2.4.5 Calibrate.
The calibrate option is used to apply a user specified energy shift to a spec-
trum. The shift may be applied to the spectrum alone, or if the Shift Regions
box is ticked, the shift is applied to the region specification (if any) as well as

Reference section.
the spectrum. The calibrate option is particularly useful when correcting the
shift to lower binding energy that results when the charge neutraliser is used
on an insulating sample.
A positive number in the calibrate text box will shift the spectrum and any
regions / components that have been defined with the spectrum to higher
binding energy. Conversely, a negative number will shift the spectrum to
lower binding energy.
8.2.4.6 Quantify.
This option is applicable to spectra data objects only.
The production of a quantitative report and the creation of depth (and other)
profiles are done in two stages. The first stage, done here, enables the user
to process spectra by defining energy region(s) with background subtraction
and, possibly, to break up peaks of complex shape into their likely compo-
nents. The second stage is done in Browser Actions and uses data usually
from more than one species to create a quantitative report and to profile
peaks. The Browser Actions window is described in Section 8.2.5
The following options are available from the Quantification Options pull
down menu.
Quantification Regions.
This option allows the user to specify one or more quantification regions for
each spectrum data object and also the background to be used for each
quantification region. Examples of Quantification Regions in quantifying
survey spectra and narrow regions scans have been detailed in Section
8.1.1 - Section 8.1.5. Quantification regions may be specified when the
acquisition is performed, in which case, the specified region(s) appear in the
Quantification Regions table automatically. All defined regions will be
shown graphically superimposed over the selected spectra in the display
area as depicted in FIGURE 27.
Each region is defined in one row of a scrolled list and has the following
parameters:
Name - This may be any text, but will usually be a spectral line from the Ele-
ment Library or Periodic Table.
Start and End (eV) - The start and end of the quantification region. Default
spectral line values are set by the Element Library.
RSF - The Relative Sensitivity Factor is the sensitivity of the spectral line to
the excitation process (e.g. photon bombardment in XPS) relative to the F
1s peak. Default spectral line values are set by the Element Library or
Periodic Table. In the photoemission peaks with core level splitting the
RSF applied to BOTH components. Should it be necessary to quantify
using only one component the RSF should be modified with reference to the
table below to give the correct quantification.

Reference section.
TABLE 1. Library sensitivity factors with modification factors
Level use
s SF
p SF
p3/2 SF x 2/3
p1/2 SF x 1/3
d SF
d5/2 SF x 3/5
d3/2 SF x 2/5
f SF
f7/2 SF x 4/7
f5/2 SF x 3/7
where SF is the library sensitivity factor (applicable to the whole doublet).
At. Mass - Atomic mass, default spectral line values are set by the Element
Library or Periodic Table.
Av. - The number of data points from the spectrum, at the start and end of
the quantification region, that are averaged together to give the start and
end data values.

Reference section.
Individual
quantification
regions
FIGURE 27. Setting up regions via Quantification Regions.
BG Type - Background type, specifies the algorithm to be used to calculate

the background within the quantification region. There are five possible
algorithms:
Simple - This is an algorithm based on over-smoothing the data, skipping over
areas where a peak is detected (a peak is assumed to be around 2 eV wide). This
is a pragmatic algorithm with little scientific basis, but gives reasonable results
for most spectra. This algorithm is always used, if the background is drawn in
any parts of a spectrum that are outside any quantification regions.
Constant - The background is a horizontal plateau set at the data value at either
the start or end of the quantification region, whichever is lowest.
Linear - The background is a straight line between the data values at the start
and end of the quantification region. This is the default option.
Shirley - This implements Shirleys algorithm (D. A. Shirley, Phys. Rev. B, 5, 5,
4709, 1972).
Tougaard - This implements Tougaards algorithm. (S. Tougaard, Surf. Inter-
face Anal., 11, 453, 1988).
To enter these parameters click the select button on a line in the list of quan-
tification regions, fill in the parameters and press enter on the keyboard. By

Reference section.
typing a specific photoemission peak into the Name text box all parameters
will be automatically filled in via the Element Library. This method, how-
ever, cannot be used to modify an existing region. Dragging and dropping a
selected peak from the Periodic Table into the display area enters the
Name, RSF and At. Mass parameters only. The Start and End parame-
ters may be chosen by using the select mouse button to drag out a box
which surrounds the region of interest.
Once the quantification region table has been created press the Apply but-
ton to incorporate the quantification regions into the spectra data object. To
quickly apply the same quantification regions to a series of spectra, use the
History option (Section 8.2.4.10).
Components.
This option is used if two or more peaks are too close in energy to be inde-
pendently resolved by the instrument. The Al elemental and oxide peaks
(FIGURE 28.) are an example where peaks are present but not independ-
ently resolved.
The user specifies peaks (referred to as synthetic components) that are

believed to be present. The Position, Height and Width of these synthetic
components can then be adjusted so that the sum of the components
(called the synthetic envelope) matches the actual data as closely as possi-
ble.
Synthetic components are specified in a similar way to quantification

regions. However, specific fields contain constraints that affect the fit of the
synthetic envelope. These constraints are displayed in the box to the right of
the table. All defined synthetic component are shown graphically superim-
posed over the current spectra in the display area as depicted in FIGURE
28.
Each synthetic component has the following parameters:
Name - This may be any text, but will usually be a spectral line from the Ele-
ment Library or Periodic Table.
Position - The position of the component in eV, displayed in either Kinetic

Energy or Binding Energy, depending on the setting in the Display Param-
eters window. The Position value is constrained to lie within a specific
energy range displayed as either Min to Max or Max to Min depending
on the abscissa scale.
Height - The height of the peak in Counts or Counts Per Second, depend-
ing on the setting in the Display Parameters window. The Height is con-
strained between minimum and maximum values.
Width - The Full Width Half Maximum of the peak in eV. The Full Width
Half Maximum is constrained between minimum and maximum values.

Reference section.
Select and drag

peak top to
adjust position
and height
Select and drag

peak edge to
adjust width
FIGURE 28. Setting up the synthetic components of a peak.
Model - The shape of the synthetic component. An option menu above the
Model field allows the user to choose from several standard shapes. These
are:
GL(n) - A combination of Gaussian and Lorentzian, with n being the percent-
age of Lorentzian. The user may enter any value for n between 0 and 100, not
just the values offered by the menu. The default option is GL(30).
AS(n, m) - Asymmetrical peak shape. This is similar to GL(n), but has the
addition of a tail on the high BE side of the peak. The user may enter any value
between 0 and 10, with the tail being larger for the smaller numbers. It is best to
try out some values - start with, say, AS(30, 0.4). Some elements give asymmet-
rical XPS peak shapes and should use this model instead of the GL(n) models.
DATA - The shape is a part of a spectrum.
COMP - Composite, the shape is a part of a synthetic envelope.
RSF - The Relative Sensitivity Factor is the sensitivity of the spectral line to
the excitation process (e.g. photon bombardment in XPS) relative to the F
1s peak. Default spectral line values are set by the Element Library.
Atomic Mass - Atomic mass of the synthetic component, default spectral

line values are set by the Element Library.

Reference section.
Ensemble Name - The name of the ensemble which the synthetic compo-
nent is a member. The default ensemble for a synthetic component is
Unlinked. Any other ensemble name entered must first be defined in the
ensemble table in the Linked Components section (see page 293).
To enter these parameters click the select button on a line in the list of syn-
thetic components, fill in the parameters and press enter on the keyboard.
By typing a specific photoemission peak into the Name text box all parame-
ters will be automatically filled in via the Element Library. If the component
already exists, however, only the name is modified. The Position, Height
and Width are chosen automatically to match the displayed spectrum as
closely as possible. No account is taken of the position (energy) of the peak
stored in the Element Library. The Position, Height and Width constraint
parameters are automatically set to values appropriate to the original data.
The Position, Height and Width parameters may be modified by using the
select mouse button to pick-up and drag the synthetic component in the dis-
play area. If the synthetic component is picked up near the top, then the
Position and Height parameters can be changed. If the synthetic compo-
nent is picked up at the side or near the bottom the Width parameter can be
changed (see FIGURE 28.). If a synthetic component is a member of an
ensemble other than Unlinked then any changes to the synthetic compo-
nents Position, Height or Width will change the respective values of all
other components within the ensemble dependent on the ensembles linked
parameters settings.
The Duplicate Component section can be used to create a duplicate of an

existing synthetic component, an example of which is done in Section 8.1.4.
Three parameters are used to create the new synthetic component from the
original synthetic component:
Offset - The difference in Position in eV between the original synthetic com-
ponent and the new synthetic component.
Height Factor - The factor by which the new synthetic component Height
should differ from the original synthetic component Height.
Width Factor - The factor by which the new synthetic component Width
should differ from the original synthetic component Width.
The new synthetic components Name, Model, RSF and Atomic Mass
values are set to those of the original synthetic component. The Position,
Height and Width constraint parameters of the duplicated synthetic com-
ponent are automatically set to values likely to be suitable. The new syn-
thetic components Name should be subsequently altered to distinguish it
from the original synthetic component. The new synthetic component can be
subsequently modified using the mouse pick-up and drag operations as
discussed above.
After making changes to a component either in the text row or in the graphi-
cal display it is necessary to press the enter key on the keyboard for the
changes take effect. If DATA or COMP have been selected for the Model
and the peak shape for the component is undefined, it is then defined as the
shape of the data or synthetic component enclosed by the most recent
selection box dragged out by the select mouse button.

Reference section.
The Auto-Fit button can be used to change the Position, Height and
Width for ALL synthetic components to fit the synthetic envelope as close
as possible to the data subject to the synthetic component and ensemble
constraints. Pressing the Auto-Fit button in the Components section does
NOT record the operation in History.
Linked Components.
This option is used to set up constraints which link the Positions, Heights
and Widths of synthetic components to each other. Each synthetic compo-
nent should have been set up to represent a particular peak which is
expected in the spectrum. Often, considerations of physics and chemistry
indicate certain fixed relationships between these peaks. An unconstrained
Auto-Fit operation could change the Positions, Heights and Widths of the
components to achieve a good mathematical correlation between the syn-
thetic envelope and the data, but the result could be nonsense from the
point of view of the physics and chemistry of the sample and instrument.
Correctly linking components improves the reliability of the results.
Ensembles are groups of components which are expected to have the same
relative size or have a constant energy offset or the same width, because
they are associated with the same element or a similar molecule.
Each Ensemble may have one of its components used as a reference com-
ponent which is linked to a component in a different Ensemble. Auto-Fit
keeps the two linked components a fixed energy apart from each other, so
effectively the two Ensembles are linked.
FIGURE 29. shows the Processing window with the Linked Components
option selected. Ensembles are specified in a similar way as quantification
regions. A worked example is provided in Section 8.1.5.
Each ensemble has the following properties:
Name - This may be any text (other than Unlinked) but is usually named to
indicate the type of relationship between the synthetic components in the
ensemble (e.g. spin).
RSF - The Relative Sensitivity Factor is the sensitivity of the ensemble as a

whole to the excitation process (e.g. photon bombardment if XPS) relative to
the F 1s peak. There are no set combination rules for the RSF values of
synthetic components in an ensemble and as such this value defaults to 1
when a name is entered.
Atomic Mass - The Atomic Mass of the ensemble as a whole. There are
no set combination rules for the atomic mass values of synthetic compo-
nents in an ensemble and as such this value defaults to 1 when a name is
entered.

Reference section.
FIGURE 29. Setting up ensembles in Linked Components.
Linked Parameters - The Position, Width and Height constraints

between the synthetic components within an ensemble can be set via their
respective toggle buttons. If a toggle is unset then that parameter of the
components within the ensemble is independently adjustable (either manu-
ally or during optimization). Conversely, if a toggle is set then that parameter
of the components within the ensemble is constrained. The constraint keeps
the ratios of the specific parameter between the components fixed to their
initial values. The component can still be adjusted (either manually or during
optimization) but the linked properties of the other components within the
ensemble are automatically adjusted to maintain the initial ratios.
Reference Component - Defines an inter-ensemble Position constraint

between two synthetic components. To create the constraint the following
steps must be adhered to:
In the Components section, note the offset in eV between the two synthetic
components that are to be linked. Note that the two synthetic components MUST
NOT be in the same ensemble.

Reference section.
In the Linked Components section check that the Link option in the Refer-
ence Component section for the ensemble of the first synthetic component to be
linked is unset.
In the display area select the first synthetic component and then CTRL select the
second synthetic component.
Set the Link option in the Reference Component section for the ensemble of
the first synthetic component. The two synthetic component names should
appear in the text boxes.
Enter the value of the required offset in the Offset text box to restore the offset
between the two synthetic components.
To enter these parameters, click the select button on a line in the list of
ensembles. Apart from the reference component names, parameters may
be entered by typing them in. An ensemble may be created or changed by
dragging and dropping a selected peak from the Periodic Table in the
Browser Actions window, into the display area. This affects the Name,
RSF and Atomic Mass parameters only.
The Position, Height and Width parameters of every component in an

ensemble may be modified by using the select mouse button to pick up and
drag any component in the display. If the component is picked up near the
top, then the Position and Height can be changed. If it is picked up at the
side or near the bottom the Width can be changed.
The Duplicate Ensemble section can be used to create a duplicate of an

existing ensemble. Three parameters are used to create the new ensemble
from the original ensemble:
Offset - The difference in Position in eV between the original ensemble and
the new ensemble.
Height Factor - The factor by which the new ensemble Height should differ
from the original ensemble Height.
Width Factor - The factor by which the new ensemble Width should differ
from the original ensemble Width.
The new ensembles Name, RSF, Atomic Mass, Linked Parameters and
Reference Component values are set to those of the original ensemble.
The new ensembles Name should subsequently be altered to distinguish it
from the original ensemble. N.B. When an ensemble is duplicated all the
synthetic components within the ensemble are duplicated as well and are
placed as new entries within the synthetic components table in the Compo-
nents section of Quantify. The properties of the new synthetic components
(including the Name) will be set to those of the synthetic components of the
original ensemble.
The Auto-Fit button can be used to change the Position, Height and
Width for ALL synthetic components to fit the synthetic envelope as closely
as possible to the data subject to the synthetic component and ensemble
constraints. Pressing the Auto-Fit button in the Link Components section
does NOT record the operation in History.

Reference section.
Once the ensembles table has been created press the Apply button to
incorporate the ensembles into the spectra data object. To quickly apply the
same ensembles to a series of spectra, use the History option.
Auto-Fit Components.
This option is used to change the Position, Height and Width for ALL syn-
thetic components to fit the synthetic envelope as closely as possible to the
data subject to the synthetic component and ensemble constraints. The
auto-fit options are:
Optimize - These radio buttons control the way in which the Auto-Fit algo-
rithm operates. In each case ALL the constraints set up in the Components
and the Linked Components option pages apply during Auto-Fit.
Collectively - Every component whether Unlinked or from an Ensemble is
changed together. If the energy range covered by the Ensembles overlap, this is
the best option.
Ensemble-Wise - Each Ensemble is treated separately. If each Ensemble
applies to data peaks that are well separated in energy, the option will save time,
but it must not be used if Ensembles overlap in energy.
Selected Ensemble - Only one Ensemble is treated. The Ensemble to be fitted
must have been selected by clicking select on the outline of a component of the
Ensemble (which causes the components outlines to be filled with solid colour).
This option is only normally used whilst setting up components in Ensembles.
Number of Iterations - This is the maximum number of iterations of the

Auto-Fit algorithm carried out if the Tolerance for the fit is not achieved first.
Tolerance - As the Auto-Fit algorithm works it measures the correlation (or

fit) of the synthetic envelope with the real spectrum. The tolerance is the
value for this fit which is considered to be good enough and when that figure
is achieved Auto-Fit stops without attempting more improvement. A lower
Tolerance requires a better fit but takes longer and may not be achievable.
Pressing the Apply button on this option performs the Auto-Fit and records
the operation in the history of the spectrum data object.

Reference section.
8.2.4.7 Annotate.
The Annotate option allows the user to write comments onto spectra or
images. Annotations are often made prior to printing the data for incorpora-
tion into a report. Some of the annotate options make measurements of fea-
tures in the data, such as peak width at half height, which is useful even if
the data is not to be printed.
The various options available are all affected by the Orientation setting.
This setting consists of two radio buttons to switch between horizontal and
vertical annotation. FIGURE 30. shows an example of annotation consisting
of horizontal text.
FIGURE 30. Text annotation via the Annotate section of the Processing window.
The following sections cover the various annotation options available. In

each case the apply button must be pressed before any annotation written
onto the screen becomes a part of the data set. Annotation, like other
changes to the data set made by processing, can be removed using the His-
tory processing option.

Reference section.
Text.
When this option is selected the user can type the text required into the
Label field, the Orientation setting decides whether the text should run
vertically or horizontally. Next the user must use the select mouse button to
define a place on the spectrum / image. If the button is pressed and
released the text is written at that place. If, however, the select button is
dragged an arrow will be drawn along the dragged axis and the text placed
at the end of the arrow where the button is released. Prior to pressing the
Apply button, a label may be removed by pressing the paste mouse button.
An existing label may be moved, complete with its pointer (if any), by picking
it up with the select button with the shift key held down. An existing label
may be moved, but a new arrow created, by drawing the new arrow using
the select button, and then moving the pointer to the old label and holding
down the control and shift keys while clicking select again (after which the
control and shift keys may be released).
Ruler.
Selecting the Ruler option allows the user to use the select mouse button
to drag out a line (horizontal or vertical) with an arrow at both ends. Text in
the Label field will be written in the appropriate direction (horizontal or verti-
cal) at the centre of the line. If a horizontal line is dragged out left to right,
then the text will appear above the line, but if it is dragged out right to left,
then the text will be below. Similarly, if a vertical line is dragged out down-
wards, then the text will appear to the right of the line, but if it is dragged
upwards, then the text will be to the left.
Axis.
The Axis option allows the user to change the text used for the horizontal or
vertical axis according to the Orientation setting. The text of the appropriate
axis appears within the Label field text box, and may be modified by the
user.
Title.
At the top centre of the spectrum or map is a horizontal title string which can
be modified by this option. The text of the title appears within the Label field
text box and may be modified by the user.
Range.
The Range option works in a similar way to the Ruler option but writes the
distance between the arrowheads (in the same units as the corresponding
axis) instead of the user text.
An additional function of this command enables the horizontal axis scale to

be adjusted if the data is a depth profile or spectrum. The select mouse but-
ton is first used to drag out a line between two points on the data. The user
can then type in a start and end value into the Axis Range boxes and these
will then be used to adjust the scale so that it indicates those values at the
arrowheads. This, in conjunction with the Axis option, allows the user to
change a depth profile axis calibrated in seconds to be calibrated in nm, for

Reference section.
example. Note that this feature is for presentation only, it does NOT alter the
underlying values in the dataset, so any area calculations or reported posi-
tions will not be affected. It would be unusual to need to use this feature for
spectra; usually the required effect should be achieved using the Calibrate
processing option, which DOES affect the underlying dataset.
Measure Peak.
This option annotates a spectrum with the full width half maximum
(FWHM) for the largest peak in the spectrum. The FWHM is the width (in eV
for XPS/AES data) of the peak half way between the background and the
top of the peak.
Measure Edge.
This option annotates a linescan with an edge sharpness measurement.

This is the distance over which the intensity falls from 80% to 20% of the
intensity difference between the top and bottom of the edge. If there is more
than one edge in the linescan, Vision chooses the one with the greatest
intensity between the top and the bottom. The user may choose a different
edge by zooming in to cover the edge of interest, but it is important to
include the top and bottom points of the edge; if you zoom in too closely the
result will be meaningless. A pair of radio buttons allows the user to choose
to have the calculation based on 16% and 84% intensity instead of 20% and
80%. Additionally the maximum and minimum values can be calculated
automatically or as user input via the Max/Min auto toggle button. In user
mode you can enter the values directly into the text boxes and press enter
or use select click on the mouse in the display area to position the maximum
and minimum bars.
8.2.4.8 Normalise.
The Normalise option can be selected and applied to alter the scaling of
data where the various spectra have been acquired using different condi-
tions. This works by applying a factor to the intensity at each point in a spec-
trum, so that the sum of all the resulting intensities is unity. This allows
spectra with very different intensities to be overlaid for comparison. This
destroys the quantitative information content in the object so is incompatible
with the Quantify option.
8.2.4.9 Data Editing.
Data editing of a spectrum can be used to remove unwanted spikes. Points

can be modified either by selecting and dragging using the mouse or by
entering values into the Intensity and Energy text boxes. Using the mouse
pointer to move a point is best done by selecting the Plot Mode Symbols
from the Tile Display window and then zooming into the region of interest.
The mouse pointer can then be used to drag the point immediately to its left.
It should be noted that this is not an instant click and drag operation and
that the data point will not actually be moved to the new position until the
Apply button is pressed.

Reference section.
8.2.4.10 History.
It is possible to apply the processing history in different ways, as defined by

the buttons along the middle of the processing history section, highlighted
in FIGURE 7.
Start from raw data will apply the processing steps defined in the table in
the same sequence and will start from the raw spectrum. This is the most
commonly used option and is the setting that the software defaults to.
Add to processed data is usually used when a single additional process-

ing step needs to be added to the spectra without applying all the process-
ing actions defined in the table. To apply a single processing step from a
table of several steps, all the processing steps that are not required should
be made inactive by deselecting the active button next to that operation. By
then having only one active processing step and using the add to proc-
essed data option only this processing step will be applied, with any previ-
ous processing remaining unchanged.
Undo all processing will simply remove all the processing steps from all
the spectra open in the processing window. Note that this operation can not
be undone and any processing steps previously carried out on the spectra
are permanently removed from the spectra.
The delete row and clear all rows buttons will remove a row description
from the processing history table or all the processing history rows depend-
ing on which button is selected.
As each processing operation is carried out the operation is recorded in a

list to form a history of the processing performed on each object. The history
window displays this list and enables the same list of processing operations,
or a modified list, to be applied to the entire set of objects in the processing
window. Furthermore, all processing to all objects can be undone with a sin-
gle operation.
On selecting the history option, the history of the currently visible object is
displayed in the list, with each item in the list active. Items may be removed
from the list by clearing the Active button for a specific processing step and
pressing the apply button. Only the active processing steps will be applied
to the spectrum, thus removing any non-active steps.
When the Apply button is pressed, ALL of the objects in the window are
affected, even those scrolled out of view. A popup message box appears
allowing you to stop the history propagation at any stage. The action on
pressing the Apply button depends on which of the following radio buttons is
pushed:
Add to Processed Data - The active processing options displayed in the
list are all applied to each object in the window. The object which is cur-
rently visible, is treated as a special case because that object has already
been processed; that object is reset to its original (un-processed) form,
prior to being processed again. (this resetting and reprocessing is neces-
sary because it is possible that one or more items in the history have
been de-activated).

Reference section.
Start From Raw Data - The active processing options displayed in the list
are all applied to each object in the window starting with each original (un-
processed) data object, so any pre-existing processing is undone.
Undo All Processing - The history list is ignored and each object in the
window is reset to its original (un-processed) form.
The Scroll To Selected Object button is a quick way of scrolling a particular

object. To do this, select the required object in the Browser and press the
Scroll To Selected Object button. Note that the selected object must
already be in the Processing window, but is usually scrolled out of view.
Clicking the right mouse button in the Processing display section invokes a
background pop-up menu with the following options:
Zoom In - This works as described in Section 8.2.2.2.
Zoom Out - This works as described in Section 8.2.2.2.
Cut - This copies the currently selected region, component or ensemble into
the paste buffer and removes the selection from the relevant list. For
ensembles, the components of the ensemble are removed from the compo-
nents list. The display section is subsequently updated to reflect the
changes. Note, this option is NOT available in the Auto-Fit Components
section.
Copy - This copies the currently selected region, component or ensemble

into the paste buffer. Note, this option is NOT available in the Auto-Fit Com-
ponents section.
Paste - This pastes into the region, component or ensemble list a copy of
the region, component or ensemble stored in the paste buffer. For ensem-
bles, the components of the ensemble are added to the components list.
The display section is subsequently updated to reflect the changes. Note,
this option is NOT available in the Auto-Fit Components section.

Reference section.
8.2.5 Browser Actions.
The Browser Actions window can be invoked via the Options menu of the
Vision Processing window. The window consists of five (option) arrow but-
tons along the top and an action area. The currently selected option appears
in the action area.
8.2.5.1 Periodic table.
The Browser Actions window with the Periodic Table option selected is
depicted in FIGURE 31. If no element has been selected the library browser
area on the right hand side displays the types of analytical techniques for
which there are library entries. For the AXIS Nova, only the Al (mono) and
Ag anodes are likely to be used. The left hand side of the window shows the
periodic table which can be used to choose an element by clicking select on
the element. Once an element has been selected the library browser area
shows the various library entries for spectral lines associated with that ele-
ment and the selected analytical technique(s).
FIGURE 31. The Browser Actions periodic table option.
The Element Library may be modified by the user in this window. The
parameters that are saved as part of the element library are used in both
Vision Processing and Acquisition. The parameters that can be modified are
seen as light grey text boxes FIGURE 31.

Reference section.
The following parameters are associated with the acquisition software and
are used to define the acquisition parameters for a region when it is typed in
either the Manual or Manager windows:
RSF (relative sensitivity factor)
dwell time
step size
number of steps
Acquisition > start (eV). Note that the end binding energy is not an edit-
able value as it is defined by the step size and number of steps. However,
the end binding energy is calculated and displayed.
The following parameters define the region for background subtraction and
are used principally in the processing part of Vision software.
start (eV)
end (eV)
peak (eV)
As the parameters are changed the Element Library is automatically

updated and the new parameters will be saved into the Element Library. It is
therefore suggested that a copy of the original Element Library is made
before any changes are made. The Element Library file can be found in
C:\Program Files\Vision2\element_library.dset. Note that any changes
made in the data in the element library only will become active in the Acqui-
sition and Processing sections of Vision after the respective software is
restarted.
8.2.5.2 Calculator.
This option allows spectra, linescans or parallel images to be mathemati-

cally manipulated on a point by point basis creating a new spectrum, lines-
can or parallel image. The original data objects are not altered and the new
data object is placed in the scratch area. The calculator interface is shown in
FIGURE 32.

Reference section.
FIGURE 32. The Browser Actions calculator option.
For all operations on spectra, the energy range of all the spectra must be
the same. For images the size and number of points in X and Y directions
must be the same.
There is a set of 5 radio buttons which select the operation required. The
sum and topographic correction buttons work differently from the standard
arithmetic buttons (+, -, * and /).
To sum two or more data objects, press the Sum button, select the
required objects in the browser and drag and drop them (holding down the
middle paste button) into the list area on the left hand side of the display.
Enter a new name into the Result Name text box and press the = button.
The new spectrum (which appears in the Scratch area) will be an average
of the selected spectra.
The Topographic Correction button is used with parallel images to correct

for sample roughness. Selecting this radio button will perform a
(peak - background) / background operation to be performed on the images.
To do this the peak image should be dragged and dropped into the left
hand box (labelled empty list in FIGURE 32.) and the background image
should be dragged and dropped into the object box. Enter a result name
and press the = (equals) button to perform the calculation. The resultant
image is stored in the temporary scratch file in the main Processing win-
dow.
The background image smoothing mask size option available when using
the topographic correction procedure is used to smooth the background
image. When a setting other than none is selected, the background image
will be modified by replacing the centre pixel with an average of an n times n
array about the centre pixel, where n is the number selected from the pull
down menu. This operation is repeated for each pixel in the image. The user
should note that the resultant image will be reduced in size by n-1, so for a
parallel image recorded at 256 x 256 pixel after using the topographic cor-
rection with a background image smoothing mask size of 5, the resultant
image would be 252 x 252 pixels.

Reference section.
To do one of the four basic arithmetic functions on two objects, press the
appropriate radio button, select one or more objects in the browser and drag
and drop them into the list area. Select one object from the list area to be the
first operand. From the browser, drag and drop the second operand into the
Object field on the left hand side of the = button, then press the = button
and the resulting object will appear in the Scratch area.
Spectra can also be manipulated by a constant amount by entering a suita-

ble integer or floating point value in the Constant text box.
If a permanent record of the results is required, then the data objects must
be transferred into a dataset (and so to disk) as described in Section
8.2.1.9.
8.2.5.3 Profile spectra.
This option is used to quantify spectra in a dataset and may be used simply
to determine relative peak ratios in a single region, over a number of
regions, to give quantitative characterisation of a material or extract a set of
profiles, such as a depth profile, from series of spectra separated by state
change objects. At the same time a quantification report in text format is
generated. This is a temporary file and may be saved to disk and/or printed
out. The layout of the profile spectra option is shown in FIGURE 33.
FIGURE 33. The Browser Actions profile spectra option.
A profile data object contains a list of intensity data, derived from a series of
spectra separated by state changes. The type of state change defines the
type of independent variable in the profile data object. For example, if the
state changes are etches, then the profile is a depth profile which describes
how the intensity varies with etch time from the original surface of the sam-
ple. Before using this option, the spectra must have had at least background
regions applied.
The simplest operation can be demonstrated by the generation of a quantifi-

cation report from a survey spectrum. After selecting the survey scan of
interest, a quantification region for each photoemission peak to be used in
the quantification must be defined, as detailed on page 287. The survey

Reference section.
scan may then be quantified by selecting the Region radio button under
Quantify Using and Quantify By selecting the Area radio button. Pressing
the Apply button will generate a quantification report, the format of which is
discussed further below.
For more involved quantification, such as a depth profile, a series of spectra

must first be selected using the browser where each series of spectra must
contain the same type and number of regions. All spectra must be sepa-
rated from their neighbours in the series by one of the state changes, in the
case of a depth profile this will be an etch.
The following options define the type of profile to be produced.
Quantify Using:
Region - each spectrum must have been set up to contain one or more
regions each with the background type specified. A profile data object is
created for each different region name. If two or more regions have the
same name, then only one profile data object is created for those regions,
with the intensities being summed. The RSF and Atomic mass used for
quantification are those contained in the Quantification regions list.
Component - each spectrum must have been set up to contain one or
more components. If the expected position (energy) of a component is
not within a region then the default simple background type is used. If a
different background type is required, then a region must be defined
which will contain the component. The situation where a component is
partly inside a region and partly outside must be avoided (unless the
regions background type is simple). A profile data object is created for
each different component name. If two or more components have the
same name, then only one profile data object is created for those compo-
nents, with the intensities being summed. The RSF and Atomic mass
used for quantification are those contained in the Components table
inside Quantify. If the Default to region button is selected for Compo-
nent quantification then the quantification report will include any defined
regions inside the spectra where there are no components defined. The
report will also specify which method of quantification was used for each
entry either Reg or Comp. If the Default to region button is not selected
and the spectra contain regions with no defined components then the
report will fail to be produced.
Ensemble - each spectrum must have been set up to contain one or
more ensembles. If the expected position (energy) of an ensemble is not
within a region then the default simple background type is used. If a differ-
ent background type is required, then a region or regions must be defined
which will contain all the components of the ensemble. The situation
where a component is partly inside a region and partly outside must be
avoided (unless the regions background type is simple). A profile data
object is created for each different ensemble name. If two or more
ensembles have the same name, then only one profile data object is cre-
ated for those ensembles, with the intensities being summed. The RSF
and atomic mass used for quantification are those contained in the
ensemble list.

Reference section.
Quantify By:
Intensity - The intensity of the peak, components or ensemble is taken to
be the maximum height.
Area - The intensity of the peak, components or ensemble is taken to be
the maximum area.
Independent Variable: The type of state change object that indicates the
type of profile. The type must correspond with selected series of state
change objects.
SG Smooth:
The user can specify the extent of a Savitzky-Golay quadratic smooth on

operations performed in Browser Actions. This is particularly useful when
calculating a concentration depth profile from a dataset. The smoothing is
done before the concentrations are calculated.
Having chosen the conditions pressing the Display in Window button brings
up a quantification report in its own window and creates the profile display
objects and puts them into the Scratch area. If a permanent record of the
results is required then these profile data objects must be transferred into a
dataset (and so to disk) as described in Section 8.2.1.9. An example of a
quantification report is shown in FIGURE 34.
FIGURE 34. Example quantification report generated from profile spectra.
An option is available in the report window menu bar to print the quantifica-
tion report to a printer.
The user can also choose to output the quantification report directly to file by
pressing the Save to File button which invokes the Export Quantification
Report window shown in FIGURE 35. In this window the user must specify
the path and file name for the data to be written to. If the filename is given
the extension .xls the file will be opened by MS Excel. When creating the
file the user can also select the data that is written by selecting the boxes so
that they are dark grey next to the text.

Reference section.
FIGURE 35. Export quantification report window with export options.
The report is divided into states. There is a state report for each spectrum in
the series of spectra. Each state report contains a line for each peak; a peak
could be a region, component or ensemble, depending on the Quantify
Using setting. There will be a profile data object for each peak. Each line in
the report has several columns:
Peak - The region, component or ensemble name.
Type - The type of quantification, i.e. region or component.
Position - The position in Kinetic or Binding energy.
FWHM - The full width half maximum for the peak. The FWHM is the
width (in eV for XPS/AES data) of the peak half way between the back-
ground and the top of the peak.
Raw Area or Raw Intensity - This is the Area or Intensity of the peak
depending on the Quantify By setting before any sensitivity factor has
been applied.
RSF - The Relative Sensitivity Factor is the sensitivity of the region, com-
ponent or ensemble.
Atomic Mass - The atomic mass of the region, component or ensemble.
Atomic Conc.% - The atomic concentration as a percentage of the total
atomic concentration of all the regions, components or ensembles in the
report. The atomic concentration is calculated by dividing the raw area or
raw intensity by the RSF.
Mass Conc.% - The mass concentration as a percentage of the total
mass concentration of all the regions, components or ensembles in the
report. The mass concentration is calculated by dividing the raw Area or
raw Intensity by the RSF and multiplying by the atomic mass.
8.2.5.4 Profile images.
This option can extract a linescan from an image or extract a spectrum from
a series of images of different energies. The original data objects are not

Reference section.
altered and the resultant linescan or spectrum data objects are placed in the
Scratch area. FIGURE 36. shows the Profile Images option.
FIGURE 36. The Browser Actions profile images option.
Two radio buttons are used to choose the creation of a linescan or the crea-
tion of a spectrum. Both options act upon the current browser selection(s)
and create output object(s) of the same name unless a different name is
typed into the Data Object Name field.
If the Image->Linescan button is pressed the fields: Start X, Start Y, End X

and End Y define the coordinates on the map or the linescan start and end.
These values are filled in when the cursor is dragged between the required
start and end positions with the select button depressed on the image of
interest. When the Apply button is pressed a linescan data object is cre-
ated for each selected map object.
If the Image->Spectrum button is pressed the fields: Start X, Start Y, End

X and End Y define the rectangular area for each map where the intensity
(counts) is to be summed to create the intensity for a single point in the
spectrum. These values are filled in when the cursor is dragged between the
required start and end positions with the select button depressed on the
image of interest. There must be more than one map selected because
each map results in only one point in the spectrum and all maps need to be
pasted into a single tile (note only the first three maps will be visible). When
the Apply button is pressed a single spectrum data object is created in the
Scratch area.
If a permanent record of the results is required the data objects must be

transferred into a dataset (and so to disk) as described in Section 8.2.1.9.
8.2.5.5 Describe.
The describe function in the browser actions window allows the simple crea-
tion of an annotated VAMAS / ISO file which may be either written to file or
the window.

Reference section.
FIGURE 37. The Browser Actions describe option.
This file format is an internationally recognised standard format for spectro-

scopic data transfer and will allow Kratos data to be imported into any other
data system which will read VAMAS / ISO format data. As well as the data
points the file contains useful information on the acquisition parameters,
including any independent variable used in the acquisition such as etch time
or theta angle of the autostage, which could be useful to the operator when
reviewing data. The relative transmission function is also saved with the
spectra and output to the VAMAS / ISO file.
FIGURE 38. Describe file displayed in a window.
A VAMAS / ISO format file can be created for a single, or multiple spectra by
selecting the files required in the processing window before pressing apply
in the describe window of browser actions. If the VAMAS / ISO file is to be
written to disk by selecting the VAMAS file radio button a window will
appear allowing the file name and path to be defined. The file will be given a
*.vms file extension.
8.2.6 Element List.
The Element List window can be brought up by selecting the relevant

option in the Options menu of the Vision Processing window. This window
is normally used in conjunction with the Display or Processing windows.

Reference section.
The Element List window displays a list of spectral lines from the element
library showing the corresponding energy. XPS core lines are shown in bind-
ing energy on the left hand side of the window and Auger peaks are shown
on the right, in kinetic energy as depicted in FIGURE 39.
Clicking the select button at any point on a spectrum displayed in the Dis-
play or Processing window will cause the scale in the element list window
to become centred at that energy. Clicking the select button on the energy
scale within the elements list window will also cause the scale in the ele-
ment list window to become centred at that energy and repeated clicking
has the effect of scrolling the energy. Right clicking in the Element List win-
dow pops-up a menu which allows the user to select the range of the scale
being displayed. Clicking select on a peak name in the Element List draws
a vertical line at the corresponding energy in the Display or Processing
window. This allows the user to easily browse through the spectra, clicking
on peaks to see which elements produce spectral lines in the region of the
peaks observed in the data. To remove all spectral lines in the display win-
dow click select on a region of the Element List containing no spectral
lines.
FIGURE 39. Using the element list window with the display window.

Reference section.
8.2.7 Display Parameters.
This Display Parameters window allows the user to control the way data is
presented within each tile. This should not be confused with the Page Dis-
play window (Section 8.2.8) which controls the tile layout.
The window is invoked from the options menu or the dis-

play background menu and brings up the window shown
in FIGURE 40.
Initialisation Mode
This section has two sets of options, the first allows the
user to select that the data be displayed using the colour
information and range information that is stored in the
data by selecting the From Data option. The From Set-
tings option in comparison takes the scales etc. from the
remainder of this panel. The second available setting is
to select between displaying the Raw Data before any
processing was performed or Processed Data after all
the processing selected has been performed.
Graph Display Options
This section allows the user to adjust the way spectra are
presented graphically on the screen.
The counts option allows the user to display the data as

a graph of the number of counts at each energy channel.
The counts per second option displays the data in
counts per second.
The Kinetic Energy option allows the user to select the

kinetic energy scale for the display whereas the Binding
Energy option changes the scale to display binding
energy instead. If Raw Data is selected an extra option
to change the energy reference via a drop down menu is
available. This changes the energy reference stored in
the dataset and should be used with caution.
The Display Data Only option displays the data without

displaying any associated regions whereas the Display
Data and Regions allows the user to display the region
information over the data.
The Describe Level menu allows the user to select the

amount of detail about the experimental conditions
included (as text) with the graphical display.
FIGURE 40. The Display Parameters window.

Reference section.
Tile Parameters
This section shows the lower and upper values of the X and Y scale being
displayed. If the From Settings option is set in Initialisation Mode, the user
can change these numbers, allowing the tiles to be adjusted to display only
the area of the data which is currently of interest. The Intensity Scale set-
ting allows the user to decide whether the scale of the data should be pre-
sented on a logarithmic or a linear scale; for spectra this applies to the Y
axis and for images it applies to the colour scale.
Tile Display
The 2-D setting allows the user to look at data which is directly overlaid
allowing several spectra to be compared. The 3-D option allows the user to
display a set of spectra displaced in the Z direction to allow the user to have
a three dimensional view of the data, which is useful for seeing trends over
many spectra. There are several tick boxes to enable various features on
the 3D display and the shape of the display is affected by the 3D Back Plane
Parameters. The settings will depend on personal choice and the data being
displayed. The operation of these parameters is best understood by trying
out a few settings - if you have not used these parameters before, start with
all boxes ticked and all slide bars set to the left hand side.
The offset plot section allows spectra to be displayed with a vertical offset
in the same window pane, as shown in FIGURE 41. The spectra to be offset
must be pasted into the Display window. The degree of offset is entered
into the % text box and the Apply button pressed.
FIGURE 41. Spectra displayed using the offset plot function.
Image Parameters

Reference section.
The image mode can be set to either interpolation mode or replication

mode. This decides which method will be used to represent an image or part
of an image, when more than one screen pixel is available to represent each
point of the image. In replication mode, each image point is translated into a
colour which is used for the whole of a rectangular block of screen pixels. In
interpolation mode, the colour of each screen pixel is calculated as a
weighted average of 4 image points, with the nearest points having greater
weight. This results in a smoother looking image compared to the block like
appearance of replication mode. FIGURE 42. shows a small part of a
zoomed image displayed in both modes.
(a) Interpolation (b) Replication
FIGURE 42. Image modes (a) Interpolation and (b) Replication.
The Colour Scale and Cutoff options are used when images are displayed
individually. The Colour Scale chosen is a matter of taste. If the defaults
offered are unsuitable a user defined colour scale can be used. To do this,
select the default scale closest to what you want, then point at the image
itself, click on the menu mouse button, and select the Colour Scale option
from the resulting menu and choose the colours required; this automatically
changes the colour scale to User Defined. The Cutoffs are the image val-
ues (counts) which produce the darkest and lightest colours. They can be
changed by the user, perhaps to increase the image contrast if there is too
little contrast because there are a few points in the image which are unusu-
ally high or low.
The Overlay First, Second and Third Image Colours and the Cutoffs
beneath them are used when 2 or 3 images are displayed in the same tile.
In this case only colour scales can be used and, probably, only the two com-
bination red/green/blue and cyan/magenta/yellow are useful for three
images. If you choose black, you can temporarily blank out an image, with-
out having to de-select it, allowing the others to be seen more clearly.

Reference section.
8.2.8 Page Display.
The Page Display window is invoked via the Options menu in the Display
window menu bar. The number and arrangement of tiles displayed on a
page may be selected by the user. An example layout configuration is given
in FIGURE 43.
There are sixteen preset Tile Format layout configurations provided. Each
configuration is set to display the same number of tiles as the format
number. The user is free to alter the preset configurations via the following
options:
Major Direction - Specifies the major direction to be either row7s or col-

umns.
Major - Number of Tiles - Specifies the number of tiles in the major direc-
tion.
Minor - Number of Tiles - Specifies the number of tiles in the opposite

direction to the major direction.
FIGURE 43. Example of a Page Display layout configuration.

Reference section.
8.2.9 Browser filter.
The Browser Filter window is shown with the default settings in FIGURE
44.
FIGURE 44. The Browser Filter window.
The Browser Filter window contains options that change the view of the
dataset as it is shown in the Vision Processing window. The ticked boxes in
the second column indicate the type of data that can be displayed in the
Vision Processing software subject to the correct accessories being fitted
to the instrument.
Selecting the etch button will display each etch cycle in the dataset. This is
shown as a vertical line with the data objects in the Vision Processing win-
dow. Similarly, with the position and counter buttons ticked, these opera-
tions will also be displayed as a vertical line. Note that these objects are only
included in the dataset if the etch,position or counter have been included
in an automated flow chart acquisition.

Reference section.
8.2.10 Colour editors.
The Graph Colour Editor can be started from the Options menu in the
menu bar or the background pop-up menu in the Display or the Process-
ing windows. The editor allows the user to change the colours used to dis-
play spectra on the screen or printer. The Colour Scale Editor can be started
from the background pop-up menu of an image and allows the user to
change the colours used to represent the intensity in an image. These two
editors are identical in operation, but the appearance is slightly different.
Modify mode
options
Background colour True white,
Colour of quantification window use this
for the
Colour of synthetic peak
background
Colour of graph axis
colour to
save ink
Colour of raw data points
and to
or lines. The first spectrum
prevent
in a display is set to the
speckling
colour of the lowest line.
in image
The next spectrum is the
grabs.
colour of the next line up,
in this case blue, and so on.
FIGURE 45. The Graph Colour Editor window.
The Modify Mode menu allows the user to select from one of two methods
of operation. These two methods perform the same task, but allow the user
to work differently as follows:-
Click to Change - This option allows the user to select a colour from the
available selections and replace the colour in the left hand list box by select-
ing the lines in the box which the user wishes to be that colour. This method
of working allows the possibility of the user wanting two different spectra to
be displayed in the same colour.
Browse to Change - In this mode of operation, the user first selects the col-
our to modify from the list on the left. Once selected, the colour selected
from the choice on the right is immediately applied to the selection. This
allows the user to see how the colour will look on a particular line rather than
just in the window as the effect can sometimes be quite different.
Note that the background colour does not default to true white. The only
true white in the colour editor window is at the top of the grey-scale column,
highlighted in FIGURE 45.

Reference section.
8.2.11 Printing.
The print menu is available in both the Display and Processing windows
menu bar and consists of two options:
Print Page - Prints only the currently displayed image.
Print All - Prints all the images available in the display window, even if
they are not visible in the window.
Selecting either of the above options invokes the printer dialogue box,
depicted for the Processing window in FIGURE 46. The printer dialogue
box is common to the MS Windows environment and allows the user to
select the required printing options.
Having set the appropriate printing options the user can either press the
OK button to commence printing, or use the cancel button to quit the
printer dialogue box.
FIGURE 46. The printer dialogue box.

13 July 2009
Appendix
9.1. Points of Contact at Kratos

The point of contact for users will depend on the location of the instrument
and the type of information required.
9.1.1 USA, Canada and South America

Kratos Inc.
100 Red Schoolhouse Road,
Building A,
Chestnut Ridge,
New York 10977,
USA
Telephone (845) 426-6700 fax (845) 426-6192
Service: Duty Service Manager
Applications: Dr. Chris Moffitt (cmoffitt@kratos.com)
9.1.2 Europe and Far East

Kratos Analytical Ltd. in the UK is the registered head quarters for Kratos.
All Kratos instruments are designed, fabricated and tested in Manchester.
This office covers all areas outside the The Americas and Canada and
Japan.
319
Configuration File
Kratos Analytical Ltd.
Wharfside
Trafford Wharf Road,
Manchester, M17 1GP
UK
Telephone: +44 (0)161 8884400 Fax: +44(0)161 8884402
Service Manager : Mr. Mark Bowlas (mark.bowlas@kratos.co.uk)
Applications: Dr. Sarah Coultas, Dr. Simon Hutton, Dr. Gautam Mishra and
Dr. Adam Roberts
surface.applications@kratos.co.uk
9.1.3 Japan
Kratos XPS section, Analytical & Measuring Instruments Division
Shimadzu Corporation, 380-1, Horiyamashita,
Hadano, Kanagawa 259-1304, Japan
Telephone: 463-88-8502 Fax: 463-88-8507
Service: Mr. Uchida (dar@shimadzu.co.jp )
Applications: Mr. Yoshihide Yoshida (yoshi-da@shimadzu.co.jp )
9.2. Configuration File
The configuration file stores all of the instrument specific settings and
parameters. This includes lens values, stage parameters, detector settings
and electron transmission characteristics. It is vital that an up to date copy
of the instruments configuration file is kept separately from the instrument
computer in case of hard disk failure. The configuration file is called config-
uration.dset.
After any change in the configuration of the instrument, e.g. variation in neu-
traliser settings then the new configuration must be saved. In the tool bar of
the Manager window is an Edit command, FIGURE 1.
320 Appendix
Configuration File
edit menu option
FIGURE 1. Manager window.
Left click on the Edit command to open the pop up menu,FIGURE 2.
FIGURE 2. Edit menu.
Left click on save to up-date the current configuration file with the new set-
tings.
If the Vision 2 software is closed then the software will ask the user whether
or not the configuration file is to be saved,
FIGURE 3. Save configuration file.
It is usual to select Yes.
The configuration file is saved in the following directory:
C:\Program Files\Vision2\Instruments
Whenever a change to the instrument configuration is made it is good prac-

tice to make copy of the configuration file changing the name to:
config_todaysdate.dset
Appendix 321
Instrument Checks and First Line Maintenance
and save this file on to a floppy disk or CD.
9.3. Instrument Checks and First Line Maintenance
This section is intended to give the user some insight into the detailed work-
ing of Ultra. It is not intended to provide a comprehensive guide to servicing
and maintenance for engineers. Exercise of normal levels of instrument
care and use of simple checks and a routine maintenance schedule will
maintain performance and extend instrument life.
The Ultra have been designed to require minimal routine maintenance.

However, there are a number of useful checks which can be made to ensure
that the instrument is performing satisfactorily. More extensive routine main-
tenance and servicing is available as part of the optional Kratos Service
Contracts.
9.3.1 Chiller Servicing
Warning: Failure to carry out the service instructions for the chiller at the
specified intervals could lead to permanent damage to the instrument.
Interval Actions
Weekly Check fluid level.
Monthly Check the condenser (air intake) is free from obstruc-

tions or accumulations of debris. Cleaning may be
achieved with a domestic vacuum cleaner with brush
attachment. Caution: Never blow the condenser out
with compressed air.
Annually Change the fluid.

Check for fluid leaks throughout the whole system.
Check the condenser for fouling.
See the Chiller manual for further details.
9.3.2 Instrument Performance Checks
Kratos advise the use of a simple performance check at routine intervals. If

possible the test should be performed at least at two weekly intervals, and
preferably each week. In the event of a problem, a set of data will then be
available for the Kratos engineer to detect whether the fault was gradually
developing or is sudden in onset.
It is suggested that during (or soon after) installation the user should try to
reproduce the performance achieved by the installation engineer, for exam-
322 Appendix
ple using the largest selected area aperture as described below. This will
serve as a reference point.
The following procedure is suggested as a guide, although it may be modi-

fied where other site quality control procedures are implemented e.g. the
working procedures under NAMAS accreditation schemes, Good Labora-
tory Practice etc. The test is not designed to show ultimate performance;
merely that the instruments routine analysis is consistent.
1. Note approximate number of hours/days use since previous test.
2. Mount a piece of clean silver on the sample platen.
3. Introduce into the vacuum system.
4. Position sample in normal analysis position.
5. Select the 55 micron selected area aperture.
6. Sputter clean for 10 minutes, or until C1s and O1s intensities are mini-
mised.
7. Switch the X-rays on at 15kV 15mA.
8. Acquire Ag 3d spectra at PE 5, 10, 20, 40, 80 eV.
9. Acquire C1s, O1s spectra at PE 40eV.
10. Acquire Ag MNN XAES spectra at PE 10eV.
11. Acquire survey spectra at 160eV Pass Energy.
12. Record the analysis chamber pressure.
13. Record the sample current at current X-ray power.
14. Measure FWHM, Intensity for each of Ag 3d spectra.
15. Measure Signal/Background ratio for each spectrum.
16. Measure C1s/Ag3d ratio.
17. Measure Ag3d -- Ag MNN separation.
The tests can be repeated for smaller analysis areas, if required. The acqui-
sition parameters for each of the data objects can be created as an experi-
ment, using acquisition manager and then stored as a run specification and
Saved, e.g. with the name Routine_Check.dset. At the time of running the
test, all that will be necessary is to read in the run specification into an
acquisition and modify the data set name and Submit. Incorporating the
date of acquisition into the dataset name will help later identification. It is
advisable to copy the completed experiments (datasets) to a separate direc-
tory and maintain a backup.
9.3.3 Weekly Functional Checks.
Regular observation of the state of the base vacuum in both the STC and
SAC can indicate a need for a system bake. Depending on the gaseous
nature of the samples being introduced the main vacuum can be greatly
affected.
1. Before operation of any of the accessories requiring High Voltage a
check on the vacuum should be made. It is desirable that the vacuum is
always better than 1x10-7 torr before operation.
2. Check all safety covers are fitted.
Appendix 323
3. The main vacuum should usually be better than 5 x 10-8 torr after an
overnight pump and a value any higher than this might indicate that there
is a leak present on the system or serious deterioration due to water
vapour condensation etc. In the first instance the instrument should be
baked following the directions given in Chapter 3.
4. Inspect all water pipes for leaks.
5. Its a good idea to ensure all important data is backed up.
6. Make a note of the corrector coil, and charge neutraliser settings on the
instrument readout, Section 4.4.8 on page 88.
7. Check pressures of gas supplies, e.g. compressed air, vent gas, etc.
324 Appendix
Index
A E
Acquisition control 79 Edit 320
Active 81 Electron bombardment ionisation 128,
Adaptor lens 164 161
Add to processed data 300 Electrostatic Mode 75
Advanced Mode 201 Electrostatic mode 75
Alignment Plates 164 Element list (manager window) 203
Analyser mode 74 Engineer Mode 201
Analyser state 78 Entering values 70
Angle resolved XPS 241 Exhaust 14
Aperture 124 Extractor Current 141, 175
Area of analysis 76
ARXPS - Manual sample position 241 F
Atmospheric Pressure 14 Fast Entry Lock 99
Auto Scan Profile 116 Field of view 1 76
Auto Z 113 Field of view 2 76
Automatic stage control 108 Field of view 3 76
Automatic vacuum sequences 44 Field of view 4 76
Autostage 104 Float mode 164
AutoZ 233 Float voltage 168
Axis of rotation 244 Floating mode 167
Azimuthal Rotation 182 Focus Lens 164
Follow mode - manager 232
B
Backing the vacuum system 49 G
Brightness 133, 165 Gas on 252
Gases 38
C Grabbing an image 72
Calibrating the autosatge 105
Calibration - charging shift 286 H
Charge neutraliser 88, 211 Hemispherical analyser 75
Charge Transfer 132, 164 High resolution scan - large area 209
Chiller 322 Hybrid Mode 75
Close SEC-SAC valve 46
Compucentric Rotation 182 I
Condenser Lens 164 Image integration 78
Configuration file 320 Imaging aperture 77
Constant height bar 92 Imaging off 78
Imaging on 78
D Import position 222
Degas 135, 169 Instrument Manager window 197
De-ioniser cartridge 87 Integration time 78
Delay 232 Ion Beam Edge Effects 133, 166
Depth Profile - manager 248 Ion Beam Raster 166
Differential pumping 130, 160, 164 Ion energy 129, 162
Dual Anode 84 Ion Gun Alignment 142, 176
1
ion Gun Bend 164 Opening a Dataset 72
Ion Gun Condenser Lens 142, 175 Opening a dataset 73
Ion Gun Emission Current 137, 142, 170, Optical Images 71
176
Ion Gun Extraction Current 137, 170 P
Ion Gun Float 142, 175 Parallel image acquisition - manager 215
Ion Gun Focus 142, 176 Parallel photoelectron imaging 74
Ion gun gas on 46 Pass Energy 76
Ion Gun Interface 135, 168 Post gas on standby time 252
Ion gun table 137, 171 Pump SAC 47
Ion Induced Mixing 167 Pump SEC 45
Ion pump controller 41 R
Ion Source Extractor 141, 175 Radiation 14
Ion Source Grid 142, 175 Rapid Depth Profiling 165
Iongun gas off 46 Real-time display 201
Iris 124 Reset Row 240
Rotary Pump 14
K RSF relative sensitivity factor 287
KRAM debug 204 Running integral 78
L S
Large area (FOV1) spectra 205 Safety labels 11
Leakage current 86 Sample bar 92
Lens mode 75 Sample mounting 89
Line scan 82 Sample Transfer 117
Liquid Nitrogen 14 Save run (manager window) 200
Load position table 226 Save selection 73
Load run (manager window) 199 Saving objects 72
Loading sample bar 120 Scan deflection plates - theory 30
Loop Back - manager 228 Scanned Map 82
Selected area spectroscopy - Manager
M 219
Magazine 97 Shielding 14
Magnetic field (site requirement) 38 Single integration 78
Magnetic lens utilities 212 Site requirements 37
Manual stage control 106 Slot 77
Mode 70 Small spot spectrocopy 77
Mouse 63 Snap shot 113
Snapshot 82
N Source High Tension 136, 169
Narrow region scan - large area 209 Spectrum 80
Neutraliser - Manager window 214 Spherical mirror analyser 75
NICPU control unit 39 Sputter shield (pneumatic) 179
Stage control unit 39
O Start from raw data 300
Open SEC-SAC valve 46 State Change - ion gun gas control 249
2
Index
State Change - loop 247

State change - position table 226
State Change - time delay 233
Status window 204
Stubs 90
Switching X-ray on 85
T
Thoriated 15
Thoriated filament regulations 15
Toggle buttons 71
Transfer 120
Transfer lens 160
U
Undo all processing 300
Unload 120
Unloading sample bar 122
Update ion gun table 138, 171
User Mode 201
V
Vacuum conytrol unit 47
Vacuum Sequences 44
Vacuum System 14
Vibration 38
VME Initialisation 66
VME/Slave messages 204
W
WX-489 97
WX-523 99
X
X-ray parameters 85
X-ray source selection 83
X-rays off 85
Z
Zone Control 67

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Wharfside, Trafford Wharf Road,

Manchester, M17 1GP, UK

Latest Revision: rev. 4

All rights reserved.

KRATOS ANALYTICAL Ltd., Surface Analysis Product Group, Wharfside,

Trafford Wharf Road, MANCHESTER, M17 1GP, England.

Chapter 1 Safety Warnings .................................................. 9

Chapter 2 AXIS Technology as Applied to the AXIS Ultra DLD 21

Chapter 3 Overview of the AXIS Ultra DLD ............................. 37

3.2. Vacuum Control Unit ...................................47

Chapter 4 Basic Operation ..................63

4.4.5.1Analyser Mode ...................................................... 74

4.8. Operation of the Autostage ........................ 104

Chapter 5 Mini Beam I and III Ion sources .....................127

5.5.6Degas ................................................................ 143

Chapter 6 Floating Ion Gun ............................................. 159

6.2. Manual Software Interface ......................... 168

Chapter 7 Data Acquisition using the Instrument Manager 197

7.3 Defining an Experiment in the Manager Window 205

7.3.5Small Spot - Selected Area Spectra .................. 219

Chapter 8 Vision Processing Software ............................. 257

After acceptance of the instrument it is strongly recommended that the checks

1.1 European Union Directives Compliance

1.1.1 FCC Compliance

1.1.2 Electrical Supplies

Europe U.S.A and Japan

Mains supply voltage warning

HIGH VOLTAGE WARNING

1.1.3 Maintaining compliance with the electromagnetic compatibility and

The following is a list of precautions which must be observed to maintain

Service work must be carried out by Kratos trained engineers. Kratos

1.1.4 Sample records

10 Chapter 1 Safety Warnings

replacing. Any item returned for repair/replacement must be accompanied by

1.1.5 Safety labels

FIGURE 1.Mains voltage warning labels

FIGURE 2.High Voltage warning labels

Chapter 1 Safety Warnings 11

FIGURE 3.Earthing Labels

FIGURE 4.Mechanical safety warning labels

FIGURE 5.Ionising radiation warning label

12 Chapter 1 Safety Warnings

KRATOS ANALYTICAL LTD

PART No. REV DATE

FIGURE 6.Rating plate

1.1.6 Warning: Ionising Radiation Generator

regulation 7 - Prior risk assessment.

regulation 8 -Restriction of exposure.

regulation 10 -Maintenance and examination of engineering controls etc.

regulation 12 - Contingency plans.

regulation 13 - Radiation protection advisor.

regulation 14 - Information, Instruction and training.

regulation 17 - Local rules and radiation protection supervisors.

regulation 31 - Duties of manufacturers etc. of articles for use in work with

regulation 33 - Misuse or interference with sources of ionising radiation.

regulation 34 - Duties of employees.

The IRR99 and associated ACoP (L121) are available on-line at

1.1.7 Laser Light

Chapter 1 Safety Warnings 13

cause damage to the eye.

1.1.8 Handling Liquid Nitrogen

1.1.9Taking the Vacuum System to Atmospheric Pressure

1.1.10 Rotary Pump Exhaust

Name (Print): ___________ Job Title:

Organisation: ______ Phone number:

Signed: _____________________ Date:

b) Immunogenic yes: no:

c) Corrosive yes: no:

d) Reactive yes: no:

yes: no: