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Handbook of Physical Vapor Deposition (PVD) Processing

Handbook of Physical Vapor Deposition (PVD) Processing

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Handbook of Physical Vapor Deposition (PVD) Processing

Comprimento:
1,419 página
131 horas
Lançado em:
Apr 29, 2010
ISBN:
9780815520382
Formato:
Livro

Descrição

This updated version of the popular handbook further explains all aspects of physical vapor deposition (PVD) process technology from the characterizing and preparing the substrate material, through deposition processing and film characterization, to post-deposition processing. The emphasis of the new edition remains on the aspects of the process flow that are critical to economical deposition of films that can meet the required performance specifications, with additional information to support the original material.

The book covers subjects seldom treated in the literature: substrate characterization, adhesion, cleaning and the processing. The book also covers the widely discussed subjects of vacuum technology and the fundamentals of individual deposition processes. However, the author uniquely relates these topics to the practical issues that arise in PVD processing, such as contamination control and film growth effects, which are also rarely discussed in the literature. In bringing these subjects together in one book, the reader can understand the interrelationship between various aspects of the film deposition processing and the resulting film properties. The author draws upon his long experience with developing PVD processes and troubleshooting the processes in the manufacturing environment, to provide useful hints for not only avoiding problems, but also for solving problems when they arise. He uses actual experiences, called "war stories", to emphasize certain points. Special formatting of the text allows a reader who is already knowledgeable in the subject to scan through a section and find discussions that are of particular interest. The author has tried to make the subject index as useful as possible so that the reader can rapidly go to sections of particular interest. Extensive references allow the reader to pursue subjects in greater detail if desired.

The book is intended to be both an introduction for those who are new to the field and a valuable resource to those already in the field. The discussion of transferring technology between R&D and manufacturing provided in Appendix 1, will be of special interest to the manager or engineer responsible for moving a PVD product and process from R&D into production. Appendix 2 has an extensive listing of periodical publications and professional societies that relate to PVD processing. The extensive Glossary of Terms and Acronyms provided in Appendix 3 will be of particular use to students and to those not fully conversant with the terminology of PVD processing or with the English language.

  • Fully revised and updated to include the latest developments in PVD process technology
  • ‘War stories’ drawn from the author’s extensive experience emphasize important points in development and manufacturing
  • Appendices include listings of periodicals and professional societies, terms and acronyms, and material on transferring technology between R&D and manufacturing
Lançado em:
Apr 29, 2010
ISBN:
9780815520382
Formato:
Livro

Sobre o autor

Donald M. Mattox obtained his B.S degree in Physics from Eastern Kentucky State University. He served as a meteorologist and Air Weather Officer in the USAF during and after the Korean War. He then obtained a M.S. degree in Solid State Physics from the University of Kentucky in 1960. In 1961 he went to work at Sandia National Laboratories (SNL). Don was a manager and member of the Technical staff at SNL for 27 years and has been a consultant to the vacuum coating industry for over 28 years. In 1995 he was the recipient of the American Vacuum Society Albert Nerken Award "For his invention of the ion plating process and its continued development." In 2007 Don received the Society of Vacuum Coaters Nathaniel Sugerman Award “For his development of the ion plating process and long-term commitment to education in the vacuum coating community.” Don has published numerous papers and book chapters on the subject of Physical Vapor Deposition (PVD) processing and technology transfer from R&D to production. He is the author of Handbook of Physical Vapor Deposition (PVD) Processing (1st edition 1998, 2nd edition 2010) published by Elsevier and Foundations of Vacuum Coating Technology, published by William Andrew/Elsevier (1st edition 2003).


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Handbook of Physical Vapor Deposition (PVD) Processing - Donald M. Mattox

Handbook of Physical Vapor Deposition (PVD) Processing

Second Edition

Donald M. Mattox

Table of Contents

Cover image

Title page

Dedication To my wife Vivienne

Copyright

Preface to First Edition

Preface to Second Edition

Acknowledgements

Acronyms Used in Vacuum Coating and Surface Engineering

A

B

C

D

E

F

G

H

I

J

K

L

M

N

O

P

Q

R

S

T

U

V

W

X

Y

Z

Miscellaneous Symbols

Donald M. Mattox

Chapter 1. Introduction

Publisher Summary

1.1 Surface Engineering

1.2 Thin Film Processing

1.3 Process Documentation

1.4 Safety and Environmental Concerns

1.5 Units

1.6 Summary

References

Chapter 2. Substrate (Real) Surfaces and Surface Modification

Publisher Summary

2.1 Introduction

2.2 Materials and Fabrication

2.3 Atomic Structure and Atom–Particle Interactions

2.4 Characterization of Surfaces and Near-Surface Regions

2.5 Bulk Properties

2.6 Modification of Substrate Surfaces

2.7 Summary

References

Chapter 3. The Good Vacuum (Low Pressure) Processing Environment

Publisher Summary

3.1 Introduction

3.2 Gases and Vapors

3.3 Gas–Surface Interactions

3.4 Vacuum Environment

3.5 Vacuum Processing Systems

3.6 Vacuum pumping

3.7 Vacuum- and Plasma-Compatible Materials

3.8 Assembly

3.9 Evaluating Vacuum System Performance

3.10 Purchasing a Vacuum System for PVD Processing

3.11 Cleaning of Vacuum Surfaces

3.13 Process-Related Contamination

3.14 Safety Aspects of Vacuum Technology

3.15 Summary

References

Chapter 4. The Sub-Atmospheric Processing Environment

Publisher Summary

4.1 Introduction

4.2 Pressure Monitoring and Control

4.3 Mass Flow Meters (MFMs) and Mass Flow Controllers (MFCs)

4.4 Geometry of the Pumping Manifold

4.5 Conduction

4.6 Distribution Manifolds for Gas Flow Uniformity

4.8 Conclusion

References

Chapter 5. The Low Pressure Plasma Processing Environment

Publisher Summary

5.1 Introduction

5.2 The Plasma

5.3 Plasma–Surface Interactions

5.4 Configurations for Generating Plasmas

5.5 Ion and Plasma Sources

5.6 Plasma Processing Systems

5.7 Plasma-related Contamination

5.8 Some Safety Aspects of Plasma Processing

5.9 Summary

References

Chapter 6. Vacuum Evaporation and Vacuum Deposition

Publisher Summary

6.1 Introduction

6.2 Thermal Vaporization

6.3 Thermal Vaporization Sources

6.4 Transport of Vaporized Material

6.5 Condensation of Vaporized Material

6.6 Materials for Evaporation

6.7 Vacuum Deposition Configurations

6.8 Process Monitoring and Control

6.9 Contamination from the Processing

6.10 Advantages and Disadvantages of Vacuum Deposition

6.11 Some Applications of Vacuum Deposition

6.12 Gas Evaporation and Ultrafine (Nano) Particles

6.13 Other Processes

6.14 Summary

References

Chapter 7. Physical Sputtering and Sputter Deposition (Sputtering)

Publisher Summary

7.1 Introduction

7.2 Physical Sputtering

7.3 Sputtering Configurations

7.4 Transport of the Sputter-vaporized Species

7.5 Condensation of Sputtered Species

7.6 Sputter Deposition Geometries

7.7 Targets and Target Materials

7.8 Process Monitoring and Control

7.9 Contamination Due to Sputtering

7.10 Advantages and Disadvantages of Sputter Deposition

7.11 Some Applications of Sputter Deposition

7.12 Summary

References

Chapter 8. Arc Vapor Deposition

Publisher Summary

8.1 Introduction

8.2 Arcs

8.3 Arc Source Configurations

8.4 Reactive Arc Deposition

8.5 Arc Materials

8.6 Arc Vapor Deposition System

8.7 Process Monitoring and Control

8.8 Contamination Due to Arc Vaporization

8.9 Advantages and Disadvantages of Arc Vapor Deposition

8.10 Some Applications of Arc Vapor Deposition

8.11 Summary

References

Chapter 9. Ion Plating and Ion Beam-Assisted Deposition

Publisher Summary

9.1 Introduction

9.2 Stages of Ion Plating

9.3 Sources of Depositing and Reacting Species

9.4 Sources of Energetic Bombarding Species

9.5 Sources of Accelerating Potential

9.6 Some Plasma-Based Ion Plating Configurations

9.7 Ion Beam-Assisted Deposition (IBAD)

9.8 Process Monitoring and Control

9.9 Contamination in the Ion Plating Process

9.10 Advantages and Disadvantages of Ion Plating

9.11 Some Applications of Ion Plating

9.12 Summary

References

Chapter 10. Atomistic Film Growth and Some Growth-Related Film Properties

Publisher Summary

10.1 Introduction

10.2 Condensation and Nucleation

10.3 Interface Formation

10.4 Film Growth

10.5 Reactive and Quasi-Reactive Deposition of Films of Compound Materials

10.6 Post-Deposition Processing and Changes

10.7 Deposition of Unique Materials and Structures

10.8 Summary

References

Chapter 11. Film Characterization and Some Basic Film Properties

Publisher Summary

11.1 Introduction

11.2 Objectives of Characterization

11.3 Types of Characterization

11.4 Stages and Degree of Characterization

11.5 Some Film Properties

11.6 Summary

References

Chapter 12. Adhesion and Deadhesion

Publisher Summary

12.1 Introduction

12.2 Origin of Adhesion and Adhesion Failure (Deadhesion)

12.3 Adhesion of Atomistically Deposited Inorganic Films

12.4 Adhesion Failure (Deadhesion)

12.5 Adhesion Testing

12.6 Designing for Good Adhesion

12.7 Failure Analysis

12.8 Summary

References

Chapter 13. Cleaning

Publisher Summary

13.1 Introduction

13.2 Gross cleaning

13.3 Specific Cleaning

13.4 Application of Fluids

13.5 Removal of Particulate Contamination

13.6 Rinsing

13.7 Drying, outgassing, and outdiffusion

13.8 Cleaning lines

13.9 Handling and Storage/transportation

13.10 Evaluation and monitoring of cleaning

13.11 In Situ Cleaning

13.12 Contamination of the Film Surface

13.13 Safety

13.14 Summary

References

Chapter 14. The External Processing Environment

Publisher Summary

14.1 Introduction

14.2 Reduction of Contamination

14.3 Materials

14.4 Body Coverings

14.5 Processing Areas

14.6 Summary

References

Appendix. The Transfer of Technology from Research and Development to Manufacturing

A.1 Stages of Technology Transfer

A.2 Organization

A.3 Research and Development (R&D) and Manufacturing Environments

A.4 Communication

A.5 Styles of Thinking

A.6 Training

Index

Dedication To my wife Vivienne

Without Vivienne’s constant support, encouragement, and editorial assistance, this edition would not exist.

Copyright

William Andrew is an imprint of Elsevier

The Boulevard, Langford Lane, Kidlington, Oxford OX5 1GB, UK

30 Corporate Drive, Suite 400, Burlington, MA 01803, USA

First edition 1998

Second edition 2010

Copyright © 2010, Donald M. Mattox. Published by Elsevier Inc. All rights reserved

The right of Donald M. Mattox to be identified as the author of this work has been asserted in accordance with the Copyright, Designs and Patents Act 1988

No part of this publication may be reproduced, stored in a retrieval system or transmitted in any form or by any means electronic, mechanical, photocopying recording or otherwise without the prior written permission of the publisher

Permissions may be sought directly from Elsevier’s Science & Technology Rights Department in Oxford, UK: phone (+44) (0) 1865 843830; fax (+44) (0) 1865 853333; email: permissions@elsevier.com Alternatively you can submit your request online by visiting the Elsevier web site at http://elsevier.com/locate/permissions, and selecting Obtaining permission to use Elsevier material

Notice

No responsibility is assumed by the publisher for any injury and/or damage to persons or property as a matter of products liability, negligence or otherwise, or from any use or operation of any methods, products, instructions or ideas contained in the material herein. Because of rapid advances in the medical sciences, in particular, independent verification of diagnoses and drug dosages should be made

British Library Cataloguing-in-Publication Data

A catalogue record for this book is available from the British Library

Library of Congress Cataloging-in-Publication Data

A catalog record for this book is available from the Library of Congress

ISBN: 978-0-81-552037-5

For information on all Elsevier publications visit our web site at books.elsevier.com

Typeset by MPS Limited, a Macmillan Company, Chennai, India www.macmillansolutions.com

Printed and bound in The United States of America

10 11 12 13 14 15 10 9 8 7 6 5 4 3 2

Preface to First Edition

Donald M. Mattox, Albuquerque, NM

The motivation for writing this book is that there is no single source of information which covers all aspects of Physical Vapor Deposition (PVD) processing in a comprehensive manner. The properties of thin films deposited by PVD processes depend on a number of factors, and each must be considered when developing a reproducible process and obtaining a high product throughput and yield from the production line.

This book covers all aspects of Physical Vapor Deposition (PVD) process technology from the characterizing and preparing the substrate material, through deposition processing and film characterization, to post deposition processing. The emphasis of the book is on the aspects of the process flow that are critical to reproducible deposition of films that have the desired properties.

The book covers both neglected subjects such as film adhesion, substrate surface characterization, and the eternal processing environment, as well as widely discussed subjects such as vacuum technology, film properties, and the fundamentals of individual deposition processes. In this book the author relates these subjects to the practical issues that arise in PVD processing, such as contamination control and substrate property effects on film growth, which are often not discussed or even mentioned in the literature. By bringing these subjects together in one book, the author has made it possible for the reader to better understand the interrelationship between various aspects of the film deposition processing and the resulting film properties. The author draws upon his long experience with developing PVD processes, troubleshooting the processes in the manufacturing environment, and teaching short courses on PVD processing, to not only present the basics but to provide useful hints for avoiding problems, and solving problems when they arise. Some examples of actual problems and solutions (war stories) are provided as footnotes throughout the text. The organization of the text allows a reader who is already knowledgeable in the subject to scan through a section and find discussions that are of particular interest. The author has tried to make the subject index as useful as possible so that the reader can rapidly go to sections of particular interest. Extensive references allow the reader to pursue subjects in greater detail if desired.

An important aspect of the book is the useful reference material presented in the Appendices. A glossary of over 2500 terms and acronyms will be especially useful to those individuals that are just entering the field and those who are not fully conversant with the English language. Many of the terms are colloquialisms that are used in the field of Surface Engineering.

The author realizes that covering this subject is a formidable task, particularly for one person, and that this effort is incomplete at best. He would like to elicit comments, corrections, and additions, which may be incorporated in a later edition of the book. In particular, he would like to elicit war stories of actual problems and solutions. Credit will be given for those that are used.

Preface to Second Edition

Donald M. Mattox, Management Plus, Inc., Albuquerque, NM

The motivation and premise of the first edition is still applicable, but times have changed! Given a term (or an author) and any of the search engines, a vast amount of information is available to the reader on the Internet. In the second edition, I have taken particular care to have terms, synonyms, acronyms, antonyms, and related terms that can be searched for on the internet for more information. There have been some major changes in processing techniques in the last ten years, namely the introduction of HIPIMS and HIPIMS+, the increased use of chemical vapor precursors in reactive PVD processing, and the increased development of thick and nanolayered PVD coatings, particularly for tribological applications. The importance of gas/vapor flow and control in reactive PVD and PECVD processes has led to the addition of Chapter 4 on The Sub-Atmospheric Processing Environment and the change of the title of Chapter 3 from The Low-Pressure Gas and Vacuum Processing Environment to The Good Vacuum (Low Pressure) Processing Environment.

March 2010

Acknowledgements

The author would like to thank Sandia National Laboratories for supporting his work in PVD processing for many years. He would also like to thank the Society of Vacuum Coaters for permission to use many of the figures that were developed for the Education Guides to Vacuum Coating Processing (SVC Publications – 2009). These guides are one-page descriptions of various aspects of PVD processing written in order to chunk the information for easy learning.

Most of all, the author would like to thank his wife, Vivienne, for the encouragement and vast amount of help that have made this second edition possible.

Acronyms Used in Vacuum Coating and Surface Engineering

A

a (α) Amorphous (Example: a-Si), Optical adsorption coefficient (cm−1)

A Ampere

Å Ångstrom

AAS Atomic absorption spectroscopy

ABS Acrylonitrile butadiene styrene; Alky-benzene-sulfonate detergent

ABS™ Arc-bonded sputtering

ACGIH American Conference of Governmental Industrial Hygienists

a-C Amorphous carbon

a-C:H Amorphous hydrogen-containing carbon (one form of diamond-like carbon)

AC Alternating current

ACS American Chemical Society

AEM Analytical electron microscopy

AES Auger electron spectroscopy

AESF American Electroplaters and Surface Finishers

AF Audio frequency

AFM Atomic force microscope; Atomic force microscopy; Abrasive flow machining

AIMCAL Association of Industrial Metallizers, Coaters and Laminators, Inc.

AIP American Institute of Physics

ALD Atomic layer deposition

AMLCD Active-matrix liquid crystal display

AMR Anisotropic magnetoresistive

amu Atomic mass unit

ANSI American National Standards Institute

AO Atomic oxygen

APC Adaptive process control

APCVD Atmospheric pressure chemical vapor deposition

APGD Atmospheric pressure glow discharge

APIMS Atmospheric pressure ionization mass spectrometry

APP Atmospheric pressure plasma

APS American Physical Society

AR Antireflective

ARAS Antireflective/antistatic

ARC Antireflective coating

ARE Activated reactive evaporation

ARF Argon fluoride

ARIP Activated reactive ion plating

ARO After receipt of order

ASHRAE American Society of Heating, Refrigerating, and Air-Conditioning Engineers

ASIC Application-specific integrated circuit

ASM ASM International (previously American Society for Metals; now ASM International)

ASME American Society of Mechanical Engineers

ASNT American Society for Non-destructive Testing

ASQC American Society for Quality Control

ASTM American Society for Testing and Materials

atm Atmosphere (usually standard atmosphere)

at% Atomic per cent

AVEM Association of Vacuum Equipment Manufacturers (more correctly known as AVEM International)

AVS The society that used to be known as the American Vacuum Society

B

B Magnetic field (vector)

BAG Bayard–Alpert gauge

BARE Bias active reactive evaporation

BBAR Broad band antireflection

bcc Body-centered cubic (crystallography)

BOPP Biaxially oriented polypropylene

bp Boiling point

BP Bandpass (filter)

BPSG Borophosphosilicate glass

BRDF Bidirectional reflectance distribution function (light)

BSC Black sooty crap

C

c Velocity of light in a vacuum, crystalline

C Capacitance; Degrees centigrade; Coulomb; ceiling

CAD Computer-aided design

CAM Computer-aided manufacturing

CAPVD Cathodic arc physical vapor deposition

CAS Chemical abstract service

CASING Crosslinking by activated species of inert gas

CASS Copper-accelerated acetic acid salt spray

cc Cubic centimeter

CCAI Chemical Coaters Association International

CCC Chromate conversion coating

CCD Charged-coupled device

CCW Counterclockwise

cd Candela

CD Compact disc; Critical dimension; Cross direction

CDG Capacitance diaphragm gauge

CDMS Chlorodimethylsilane

CD-R Compact disc-recordable

CE Comformité européenne

CEVC Completely enclosed vapor cleaner

CF™ Conflat (vacuum flange)

CFC Chlorofluorocarbon

CFC-111 Trichloroethane

CFC-113 Trichlorotrifluoroethane

cfm Cubic feet per minute

cfs Cubic feet per second

CGA Compressed Gas Association

cgs Centimeter–gram–second system of measurement

CIE Commission International de l’Eclairage (International Commission on Illumination)

CIGS Copper–indium–gallium–diselenide

CLA Center line average

CLEO Conference on Laser and Electro-Optics

cm Centimeter

cmh Cubic meters per hour

CMM Converting machinery/materials

CMOS Complementary metal oxide semiconductor

CMP Chemical–mechanical polishing; Chemical–mechanical planarization

CN Coordination number

CNDP Cold neutron depth profile

COO (CoO) Cost of ownership

CNT Carbon nanotube

CPP Cast polypropylene

CPWR Coupled plasmon-waveguide resonance

CrP Chromium-rich oxide passivation

CRT Cathode ray tube

CSP Concentrated solar power (solar thermal)

CTE Coefficient of thermal expansion

CTMS Chlorotrimethylsilane

C-V Capacitance-voltage

CVD Chemical vapor deposition

CW Clockwise

D

d Day

dc Direct current (preferable to DC)

D-CVD Dielectric-chemical vapor deposition

DBD Dielectric barrier discharge

DCS Dichlorosilane

di- 2; Two

DI Deionized

Diff Diffusion pump

DIO Deionized and -ozonated (water)

DIW Deionized water

DLC Diamond-like carbon

DLF Diamond-like films

DMS Dual magnetron sputtering

DMSO Dimethyl sulfoxide

DOE Department of Energy (US); Design of experiments

DOI (Doi) Digital object identifier (intellectual property)

DOP Dioctyl phthalate

DOT Department of Transportation

DOVID Diffractive optically variable image device

DP Diffusion pump

DRAM Dynamic random access memory

DTIC Defense Technical Information Center (US)

DVD Directed vapor deposition

DUV Deep ultraviolet

DWDM Dense wavelength division multiplexing

dwt Pennyweight

E

E Emissivity; Electric field (vector); Elastic modulus

e Exponential

EB (eb) Electron beam

e-beam Electron beam

ECD Electrochemical deposition

ECM Electrochemical machining

ECR Electron cyclotron resonance

ECS Electrochemical Society

EDM Electrodischarge machining

EDX Energy-dispersive X-ray

EDTA Ethylene diamine tetraacetic acid

EELS Electron energy loss spectroscopy

EHC Electrolytic hard chrome

EIES Electron impact emission spectroscopy

EL Electroplated

ELD Electroluminescent display (flat panel)

EM Electromigration

emf Electromotive force

EMI Electromagnetic interference

EN Electroless nickel

EPA Environmental Protection Agency

epi Epitaxial

EPMA Electron probe X-ray microanalysis

ERA Evaporative rate analysis

ERD Elastic recoil detection

ES&H Environmental Safety and Health

ESCA Electron spectroscopy for chemical analysis

ESD Electrostatic discharge

EU European Union

EUV Extreme ultraviolet

eV electron volt

F

F Farad; Free machining (steel)

FC Fault classification

fcc Face centered cubic

FD Fault detection

FDD Floppy disc drive

FEC Field emission cathode

FED Field emission display; Field emission diode

FE-SEM Field emission-scanning electron microscopy

FET Field effect transistor

FF Fill factor

FIB Focused ion beam

FIFO First in first out

FIM Field ion microscopy

FLIR Forward-looking infrared (7.5 to 12 μm)

FPC Fixed process control; Flexible printed circuits

FPD Flat panel display

fpm Feet per minute

FTIR Fourier transform infrared

FTO Fluorine-doped tin oxide

G

g Unit of gravitational acceleration; Gram

G Giga (suffix for 10⁹); Unit of magnetic field strength (Gauss); Gallons; Unit of acceleration due to gravity

GANA Glass Association of North America

GDMS Glow discharge mass spectrometry

GDOES Glow discharge optical emission spectroscopy

GFCI Ground fault circuit interrupter

GLAD Glancing angle deposition

GPM Gallons per minute

gr Grain

GWP Global warming potential

H

h Planck’s constant; Hour; Hecto (10²)

H Henry (unit of inductance); Hardness

HAD Hollow cathode-assisted deposition

HAP Hazardous air pollutants

HAZ Heat-affected zone; Hazardous (material)

HCD Hollow cathode discharge

HCFC Hydrochlorofluorocarbon

HCL Hollow cathode lamp; Hydrochloric acid

hcp Hexagonal close-packed

HDD Hard disk drive

HDP-CVD High density plasma chemical vapor deposition

HEED High energy electron diffraction

HEPA High efficiency particle air (see also ULPA)

HF Hydrofluoric acid

HFCVD Hot filament chemical vapor deposition

HFE Hydrofluoroether

HIP Hot isostatic processing

HIPIMS High power impulse magnetron sputtering

HIPIMS+ Modulated pulse power (MPP) HIPIMS

HK Knoop hardness

HLB Hydrophilic–lipophilic balance

HMC Hybrid micro circuit

HMCTSO Hexamethylcyclotrisiloxane

HMDSO Hexamethyldisiloxane

hPa Hectopascals

HPPMS High power pulse magnetron sputtering

HRI High refractive index

HV Vickers hardness

HVOF High velocity oxygen fuel

HWOT Half wave optical thickness

Hz Hertz (cycles per second)

I

i Prefix used to indicate that the film was formed using beam-type film ion deposition. Examples: i-C; i-BN

IAD Ion-assisted deposition

IARC International Agency for Research on Cancer (establishes carcinogenicity of materials)

IBA Ion beam analysis

IBAD Ion beam-assisted deposition

IBAE Ion beam-assisted etching

IBED Ion beam-enhanced deposition

IBEST™ Ion beam surface treatment

IC Integrated circuit

ICB Ionized cluster beam (deposition)

ICP Inductively coupled plasma

ICP-MS Inductively coupled plasma mass spectrometer

ID Internal diameter

IDLH Immediately dangerous to life or health

IDM Integrated device manufacturing

IEEE Institute of Electrical and Electronic Engineers

IES Institute of Environmental Sciences

IG Ionization gauge

IGU Insulated glass unit (double glazing)

ILD Interlayer dielectric

IMD Intermetal dielectric

IMEMS Integrated microelectromechanical systems

Ioc Open circuit current (solar cell)

IP Intellectual property

IPA Isopropyl alcohol

IPC Institute for Interconnecting and Packaging Electronic Circuits; International patent classification

iPVD Ionized physical vapor deposition

I-PVD Ion-assisted physical vapor deposition

IR Infrared

Isc Short circuit current (solar cell)

ISCST International Society of Coating Science and Technology

ISHM International Society for Hybrid Microelectronics

ISO International Standards Organization

ISS Ion scattering spectroscopy

IT Information technology; Internet transactions

ITO Indium–tin oxide alloy (90 : 10)

I-V Current-voltage

IVD Ion vapor deposition

IWFA International Window Film Association

J

J Joule; Electric current (vector)

JVST Journal of Vacuum Science and Technology

K

K Dielectric constant; Karat (fineness of gold)

k Kilo (10³); Boltzmann’s constant; Portion of the complex index of refraction given by n-ik or n(1-ik)

κ (kappa) Optical extinction coefficient (κ550 – extinction at 550 nm)

kcal Kilocalorie

kGy KiloGray

KRF Krypton fluoride

kWH Kilowatt-hour

L

l Liter (not preferred)

L Low (carbon steel); Liter (preferred)

LAC Large-area coating

LAD Laser ablation deposition

LASER Light amplification by stimulated emission of radiation

LbL Layer by layer

LC50 Median lethal dose

LCD Liquid crystal display

LCM Laser confocal microscope

LCO2 Liquid CO2

LCVD Laser chemical vapor deposition

LDPE Low density polyethylene

LED Light-emitting diode

LEED Low energy electron diffraction

LEL Lower explosive limit

LEISS Low energy ion scattering spectroscopy

LFL Lower flammability limit

LIBS Laser-induced breakdown (plasma) spectrometry

LLDPE Linear low density polyethylene

LM Layer metallization

LOCOS Local oxidation of silicon

LPCVD Low pressure chemical vapor deposition (see also SACVD)

LPPS Low pressure plasma spray

LIMA Laser-induced mass analysis

LLS Linear least squares (statistical analysis)

LiPON Lithium phosphorous oxynitride

LN, LN2 Liquid nitrogen

low-e Low-emission; Low-emissivity

LPCVD Low pressure chemical vapor deposition

LRP Liquid ring pump

LSA Laser spike annealing

LTEL Long-term exposure limits

LTS Long-throw sputtering

LWP Long-wavelength pass filter

M

m Milli (suffix for 10−3); Meter; Molality

M Mega (prefix for 10⁶); Minute

MBE Molecular beam epitaxy

mc Microcrystalline

mcg Micrograms

MCrAlY Metal–chromium–aluminum–Yitterium

MD Movchan–Demchiskin; Machine direction

MDG Molecular drag gauge

Me Metal

Me-C:H Metal-containing hydrocarbons

MEC Methylene chloride

MEMS Microelectromechanical systems (also called MST)

MePIIID Metal plasma immersion ion implantation and deposition

MERESAN™ Measurement and evaluation of surfaces by evaporative rate analysis

MERIE Magnetically enhanced reactive ion etcher

MF Mid-frequency

MFC Mass flow controller

MFM Mass flow meter

MFSA Metal Finishing Suppliers' Association

Mil Specs Military standards and specifications

min Minute

mks, MKS Meter–kilogram–second system of measurement

ML Monolayer

MLAR Multilayer antireflection coating

MLS Monolayers per second

MMIC Monolithic microwave integrated circuits

MNS Metal–nitride–silicon

MO Magneto-optical

MOCVD Metalorganic chemical vapor deposition

MOMBE Metalorganic molecular beam epitaxy

mono- 1; One

MOS Metal oxide semiconductor

MoS2M Metal-containing MoS2

MPI Manufacturing process instruction

MPP Modulated pulse power (see also HIPIMS+)

MR Magnetoresistive

MRS Materials Research Society

MSDS Materials safety data sheet

MST Microsystems technology (also called MEMS)

MT-CVD Medium temperature chemical vapor deposition

MTJ Magnetic tunnel junction

MTMOS Methyltrimethoxysilane

MTR Material test report; Moisture transmission rate

MVTR Moisture vapor transmission rate

N

n Index of refraction; Portion of the complex index of refraction given by n-ik

N Newton (SI unit)

N Normal (solution strength – chemistry)

NACE National Association of Corrosion Engineers

NAMF National Association of Metal Finishers

NASF National Association for Surface Finishing

NBS National Bureau of Standards, which has been renamed NIST

nc Nanocrystalline; Nanocomposite

NC Normally closed

NDE Non-destructive evaluation

NDT Non-destructive testing

NEG Non-evaporable getter

NESHAP National emission standards for hazardous air pollutants

NFPA National Fire Protection Association

NIR Near-infrared

NIST National Institute of Standards and Technology (US)

nm Nanometer

NMR Nuclear magnetic resonance

NO Normally open

NPB N-propyl bromide

NRA Nuclear reaction analysis

NREL National renewable energy laboratory

NST Nanoscience and technology

NTIS National Technical Information Service (US)

NVR Non-volatile residues

O

OD Optical density; Outside diameter

ODP Ozone-depletion potential

ODS Ozone-depleting substance

OEM Original equipment manufacturer; Optical emission monitor

OES Optical emission spectroscopy

OLED Organic light-emitting devices; Organic luminescent devices

OMS Optical mass spectrometer

OPP Oriented polypropylene

OS Ozone-safe

OSEE Optically stimulated electron emission

OSHA Occupational Safety and Health Administration (US)

OTFT Organic thin film transistor

OTR Oxygen transmission rate

OVD Optically variable device

OVID Optically variable image display

OXTR Oxygen transmission rate

oza or oz(a) Avoirdupois ounce

ozt or oz(t) Troy ounce

P

p Parallel (Example: p wave)

P Suffix used to denote plasma-deposited material (Example: P-TEOS)

Pa Pascal

PA Polyamide

PACVD Plasma-assisted chemical vapor deposition

PAPVD Plasma-assisted physical vapor deposition

PAVD Plasma-assisted vapor deposition

PBIID Plasma-based ion implantation and deposition

PC Polycarbonate

PCE Perchloroethylene; Photothermal conversion efficiency

PD Plasma doping

PDP Plasma display panel

PDMS Polydimethylsiloxane

PE Polyethylene

PECVD Plasma-enhanced chemical vapor deposition

PEEK Polyetheretherketone

PEI Polyetherimide

PEL Permissible exposure limit

PEM Plasma emission monitor

PEMS Plasma-enhanced magnetron sputtering

PERC Perchloroethylene

PET Polyethylene terephthalate (polyester)

penta- 5; Five

PF Packing fraction

PFC Perfluorocompounds

PFD Process flow diagram

PFPE Perfluorinated polyether

pH Pouvoir hydrogene (hydrogen ion content)

ph Precipation hardening (steel)

PICVD Plasma impulse chemical vapor deposition

PIID Plasma immersion ion deposition

PIII Plasma immersion ion implantation

PLD Pulsed laser deposition

PM Preventive maintenance; Powder metallurgy

PML Polymer multilayer

PMS Pulsed magnetron sputtering

PO Purchase order

poly Polycrystalline

POU Point of use

PP Polypropylene; Plasma polymerization

ppm Parts per million

ppmbv Parts per million by volume

PSG Phosphosilicate glass; Phosphrous+silicon oxides

psi Pounds per square inch

psia Pounds per square inch – absolute

psig Pounds per square inch – gauge

PSII Plasma source ion implantation

PV Photovoltaic

PVA Polyvinyl alcohol

PVC Polyvinyl chloride

PVD Physical vapor deposition

PVDC Polyvinylidene chloride

PWB Printed wiring board

PWR Plasmon-waveguide resonance

PZT Lead zirconate titanate (PbZrTiO3)

Q

Q Charge in coulombs

QA Quality assurance

QC Quality control

QCM Quartz crystal microbalance; Quartz crystal monitor

QMS Quadrupole mass spectrometer

0D (zeroD) Quantum dot (structure)

QWOT Quarter wavelength optical thickness

R

R Resistance; Organic radical in chemical nomenclature

Ra Roughness (average)

Rmax Roughness (maximum)

Rs Sheet resistance; Spreading resistance

R2R Roll to roll

RAM Random access memory

RBS Rutherford backscattering spectrometry

RED Reflection electron diffraction

rf Radio frequency (preferable to RF)

RFI Radio frequency interference

RFID Radio frequency identification

RFQ Request for quote

RGA Residual gas analyzer

RH Relative humidity

RHEED Reflection high energy electron diffraction

RIBE Reactive ion beam etching

RIE Reactive ion etching

RMOS Refractory metal oxide semiconductor

rms Root mean square

RO Reverse osmosis

ROI Return on investment

ROM Read-only memory

ROW Rest of world

RPE Reactive plasma etching

rpm Revolutions per minute

rps Revolutions per second

RT Room temperature

RTA Rapid thermal annealing

RTCVD Rapid thermal chemical vapor deposition

RTN Rapid thermal nitridation

RTP Rapid thermal processing

RTSPC Real time statistical process control

S

S Reciprocal ohm; mho; Siemen

s Second; Perpendicular (as in s-wave); Standard deviation

SACVD Sub-atmospheric chemical vapor deposition

SAD Selected area diffraction; Spotless arc-activated deposition

SAE Society of Automotive Engineers

SAM Scanning Auger spectroscopy

SAMPE Society for the Advancement of Materials and Processing Engineering

SAW Surface acoustic wave

SCBA Self-contained breathing apparatus

sccm Standard cubic centimeters per minute

sccs Standard cubic centimeters per second

scf Standard cubic feet

SCF Supercritical fluid

sclm Standard cubic liters per minute

scls Standard cubic liters per second

scm Standard cubic meters

SCM Scanning capacitance microscope

SCR Silicon-controlled rectifier

SCSI Small computer systems interface

SEAM Scanning electron acoustic microscope

SEI Secondary electron image

SEM Scanning electron microscope; Scanning electron microscopy

SEMI Semiconductor Equipment and Materials International

SFM Scanning force microscope

sg Specific gravity

SI Système International d’Unités (International System of Units)

SIAM Scanning interferometric aperatureless microscope

SIMOX Separation by implanted oxygen

SIMS Secondary ion mass spectroscopy

SION Silicon oxynitride

SIP Sputter ion plating; Self-ionized plasma

SIS Semiconductor-insulator-semiconductor

SK Stranski–Krastanov

SLAM Scanning laser acoustic microscope; Scanning laser acoustic microscopy

SLAR Single layer antireflection

slm Standard liters per minute

SMART Self-monitoring analysis and reporting technology

SME Society of Manufacturing Engineers

SMIF Standard mechanical interface

SMT Surface mount technology

SNMS Secondary neutral mass spectrometry

SOD Spin-on-dielectric

SOG Spin-on-glass

SOI Silicon-on-insulator

SPC Statistical process control

SPE Solid phase epitaxy

SPIE International Society for Optical Engineering

SPM Scanning probe microscope

SQUID Superconducting quantum interference device

sr Steradian

SRAM Static random access memory

SRG Spinning rotor gauge

SRM Standard reference material

SS (SST) Stainless steel

SSIS Surface scanning inspection systems

SSMS Spark source mass spectrometry

std Standard

STEL Short-term exposure limit

STEM Scanning transmission electron microscopy

SThM Scanning thermal microscopy

STI Shallow trench isolation

STM Scanning tunneling microscope; Scanning tunneling microscopy

STP Standard temperature (0°C) and pressure (760 Torr)

SVC Society of Vacuum Coaters

SWP Short-wavelength pass filter

SZM Structure-zone-model

T

TA Thermal analysis

TAB Tape-automated bonding

t:a-C Tetrahedral amorphous carbon

ta-C:H Tetrahedral-bonded carbon (no hydrogen) (one form of diamond-like carbon)

TA-MS Thermal analysis with mass spectrometry

TBAH Tetrabutylammonium hydroxide

TC Thermocouple; Thermocompression; Time constant

TCA 1,1,1-trichloroethane (or methyl chloroform)

TCC Transparent conductive coating

TCE Trichloroethylene (CHCl : CCl2); Thermal coefficient of expansion

TCLP Toxicity characteristic leaching procedure

TCO Transparent conductive oxide

TCP Transformer-coupled plasma

TCR Temperature coefficient of resistivity

TD Transverse direction

TDMS Thermal desorption mass spectrometry

TEM Transmission electron microscope; Transmission electron microscopy

TEOS Tetraethoxysilane

tetra- 4; Four

TFI Thin-film inductive

TFT Thin-film transistor

TGA Thermogravimetric analysis

TGA-MS Thermogravimetric analysis with mass spectrometry

TIBA Triisobutylaluminum

TIS Total integrated scatter

TiW (W : 10 wt%Ti) or (W : 30at% Ti) (alloy)

TLV Threshold limit values

Trademark

TMDSO Tetramethyldisiloxane

TMMOS Trimethylmethoxysilane

TMP Turbomolecular pump

TMS Tetramethyldisiloxane (TMDSO preferred)

TPD Temperature-programmed-desorption

tri- 3; Three

TSHT Total solar heat transmittance

TTT Tritium tracer technique

TWA Time-weighted average

TWM Thermal wave microscopy

TZM Alloy of titanium, zirconium, and molybdenum

U

u Unified atomic mass unit

UBM Unbalanced magnetron

UBS Unbalanced magnetron sputtering

UCHF Ultraclean high flow

UEL Upper explosive limit

UF Ultra-filtration

UHP Ultrahigh purity

UHV Ultrahigh vacuum

ULPA Ultralow-permeation air

ULSI Ultralarge scale integration

uPE Unplasticized PE

uPVC Unplasticized polyvinyl chloride

UPW Ultrapure water

USPTO US Patent and Trademark Office

UTS Ultimate tensile strength

UV Ultraviolet

V

v Velocity

V Volt; Voltage (as in capacitance-voltage measurements)

VAR Vacuum arc remelting

VCR Voltage coefficient of resistance

VD Vacuum degassing

VEPA Very high efficiency particulate air (filter)

VHV Very high vacuum

VIM Vacuum induction melting

VLP- Very low pressure (-PECVD)

VLR Visible light reflection

VLT Visible light transmission

VOC Volatile organic compound

Voc Open circuit voltage (solar cell)

VOD Vacuum oxygen decarburization

VPE Vapor phase epitaxy

VPS Vacuum plasma spray

VUHV Very ultrahigh vacuum

VUV Vacuum ultraviolet

W

W Watt (power)

Wp Peak power (watts)

WCC Tungsten carbide plus carbon, also CrCC, etc. Also WC-C and WC : C

WDS Wavelength dispersive spectrometry

WDM Wavelength division multiplexing

WDX Wavelength-dispersive X-ray

WLP Wafer-level packaging

WORM Write once read many

Wp Watt peak

wt% Weight per cent

WVTR Water vapor transmission rate

X

XES X-ray energy spectroscopy

XPS X-ray photoelectron spectroscopy

XRD X-ray diffraction

XRF X-ray fluorescence

XRM X-ray microanalysis

XRT X-ray topography

XUHV Extra ultrahigh vacuum

Y

Y Young’s modulus

YAG Yttrium aluminum garnet

Z

Z Atomic number of an element

ZAO Aluminum-doped zinc oxide

ZD Zero defects

Miscellaneous Symbols

2D Two-dimensional

3D Three-dimensional

α Amorphous

σ Standard deviation

ø Diameter

Ω Ohm

μ Micron

μc Microcrystalline

μm Micrometer

n Frequency

λ Wavelength

Donald M. Mattox

Don Mattox obtained his B.S. degree in Physics from Eastern Kentucky State University in 1953. He served as a Lieutenant in the USAF during and after the Korean War. During the war he obtained a Meteorology degree from MIT. After being discharged from the service he obtained his M.S. degree in Solid State Physics from the University of Kentucky in 1959 and went to work for Sandia Corporation (later Sandia National Laboratories) in 1961. Don retired from Sandia National Laboratories in 1989 after 28 years as a Member of the Technical Staff and then as a Technical Supervisor. At retirement he was Supervisor of the Surface and Interface Technology Division. He has had more than 45 years' experience in research, development, application, and production of thin films and coatings prepared by PVD processes as well as other techniques such as electrodeposition, CVD and thermal spraying. In addition he has had extensive experience in many other phases of material science in that he has supervised persons involved in the research, development, and application of organic materials, adhesive bonding, ceramic and glass fabrication, ceramic metallizing, surface chemical analytical techniques, tribology, and failure analysis. He has had extensive experience in transferring technology from R&D into production, instructing engineering and production personnel, and in troubleshooting production problems. Don was President of the American Vacuum Society (now AVS: Science and Technology of Materials, Interfaces, and Processing) in 1985. In 1988, the 9th International Congress on Vacuum Metallurgy presented him with an award for outstanding contributions to metallurgical coating technology for the period 1961–1988 and in 1995 he was the recipient of the AVS Albert Nerken Award for his work in the development of the ion plating process. From 1989 to 2006 Don was the Technical Director of the Society of Vacuum Coaters as well as being a consultant to industry on PVD processing. In 2007 Don received the Nathaniel H. Sugerman Award from the Society of Vacuum Coaters. At present he is a consultant in the field of PVD processing with Management Plus, Inc. of Albuquerque, NM. Don has taught courses on PVD processing and vacuum technology to the Sandia National Laboratories, AVS, MRS, SVC, and at numerous industry venues.

Don has published more than 100 papers and book chapters on the subject of PVD processing and other coating processes as well as the first technical paper on the PVD process, called Ion Plating. Don is the author of the book Handbook of Physical Vapor Deposition (PVD) Processing (1998) and The Foundations of Vacuum Coating Technologies (2003), both published by Elsevier (William Andrew Publishing/Noyes Publications), and Education Guides to Vacuum Coating Processing, published by the Society of Vacuum Coaters (2009). Don is the co-editor of Adhesion in Solids, Vol. 119, MRS Symposium Proceedings (1988) and, along with Vivienne Harwood Mattox, edited the book 50 Years of Vacuum Coating Technology and the Growth of the Society of Vacuum Coaters published by the Society of Vacuum Coaters (2007). Don is the editor of the Proceedings of the Annual Technical Conference, Society of Vacuum Coaters and the Bulletin, Society of Vacuum Coaters.

Chapter 1

Introduction

Publisher Summary

A surface modification process changes the properties of the surface, but the substrate material is still present on the surface. One of such processes is physical vapor deposition (PVD) processes that are atomistic deposition processes in which material is vaporized from a solid or liquid source in the form of atoms or molecules and transported in the form of a vapor through a vacuum or low pressure gaseous (or plasma) environment to the substrate, where it condenses. The main categories of PVD processing are vacuum deposition (evaporation), sputter deposition, arc vapor deposition, and ion plating. There are a number of other thin film deposition processes that should be considered for certain applications, for example, a TiN hard coating can be deposited by PVD or chemical vapor deposition (CVD). The ability to scale-up (up-scale) a deposition process and associated equipment to provide a quality product at an attractive price is essential in the commercialization of any process. It is important that the development work be done on representative substrate material and with processes and equipment that can be scaled to production requirements. An important factor in manufacturability is the deposition fixturing, which holds the substrates in the deposition chamber.

1.1 Surface Engineering

Surface engineering involves changing the properties of the surface and near-surface region in a desirable way. Surface engineering can involve an overlay process or a surface modification process. In overlay processes a material is added to the surface and the underlying material (substrate) is covered and not detectable on the surface. A surface modification process changes the properties of the surface but the substrate material is still present on the surface. For example, in aluminum anodization, oxygen reacts with the anodic aluminum electrode of an electrolysis cell to produce a thick oxide layer on the aluminum surface. Table 1.1 shows a number of overlay and surface modification processes that can be used for surface engineering.

Table 1.1

Each process has its advantages, disadvantages, and applications. In some cases surface modification processes can be used to modify the substrate surface prior to depositing a film or coating. For example, a steel surface can be hardened by plasma nitriding (ionitriding) prior to the deposition of a hard coating by a physical vapor deposition (PVD) process. In other cases, a surface modification process can be used to change the properties of an overlay coating. For example, a sputter-deposited coating on an aircraft turbine blade can be shot peened to densify the coating and place it into compressive stress.

An atomistic deposition process is one in which the overlay material is deposited atom-by-atom. The resulting film can range from single crystal to amorphous, fully dense to less than fully dense, pure to impure, and thin to thick. Generally the term thin film is applied to layers which have thicknesses on the order of a micron or less (1 micron = 10−6 meters) and may be as thin as a few atomic layers. Thicker deposits are called coatings. The term thick film is usually not used for thick atomistically deposited vacuum deposits as that term is used for paint-on, fire-on types of deposition.

Often the properties of thin films are affected by the properties of the underlying material (substrate) and can vary through the thickness of the film. Thicker layers are generally called coatings. An atomistic deposition process can be done in a vacuum, plasma, gaseous, or electrolytic environment.

1.1.1 Physical Vapor Deposition (PVD) Processes

Physical vapor deposition processes (often just called thin film processes) are atomistic deposition processes in which material is vaporized from a solid or liquid source in the form of atoms or molecules and transported in the form of a vapor through a vacuum or low pressure gaseous (or plasma) environment to the substrate, where it condenses. Typically, PVD processes are used to deposit films with thicknesses in the range of a few nanometers to thousands of nanometers; however, they can also be used to form multilayer coatings, graded composition deposits, very thick deposits, and freestanding structures. The substrates can range in size from very small to very large, for example the 10′ × 12′ glass panels used for architectural glass. The substrates can range in shape from flat to complex geometries such as watchbands and tool bits. Typical PVD deposition rates are 10–100Å (1–10 nanometers) per second.

Physical vapor deposition processes can be used to deposit films of elements and alloys as well as compounds using reactive deposition processes. In reactive deposition processes, compounds are formed by the reaction of the depositing material with the ambient gas environment such as nitrogen (e.g. titanium nitride, TiN) or with a co-depositing material (e.g. titanium carbide, TiC). Quasi-reactive deposition is the deposition of films of a compound material from a compound source where loss of the more volatile species or less reactive species during the transport and condensation process is compensated for by having a partial pressure of reactive gas in the deposition environment; for example, the quasi-reactive sputter deposition of ITO (indium–tin oxide) from an ITO sputtering target using a partial pressure of oxygen in the plasma.

The main categories of PVD processing are vacuum deposition (evaporation), sputter deposition, arc vapor deposition, and ion plating, as depicted in Figure 1.1.

Figure 1.1 PVD Processing Techniques: (a) Vacuum Evaporation, (b) and (c) Sputter Deposition in a Plasma Environment, (d) Sputter Deposition in a Vacuum, (e) Ion Plating in a Plasma Environment with a Thermal Evaporation Source, (f) Ion Plating with a Sputtering Source, (g) Ion Plating with an arc Vaporization Source, and (h) Ion Beam-Assisted Deposition (IBAD) with a Thermal Evaporation Source and Ion Bombardment from an Ion Gun

Vacuum Deposition (Vacuum Evaporation)

Vacuum deposition (Ch. 6), which is sometimes called vacuum evaporation, is a PVD process in which material from a thermal vaporization source reaches the substrate with little or no collision with gas molecules in the space between the source and substrate. The trajectory of the vaporized material is line of sight. The vacuum environment also provides the ability to reduce gaseous contamination in the deposition system to a low level. Typically, vacuum deposition takes place in the gas pressure range of 10−5 Torr to 10−9 Torr, depending on the level of gaseous contamination that can be tolerated in the deposition system. The thermal vaporization rate can be very high compared to other vaporization methods. The material vaporized from the source has a composition which is in proportion to the relative vapor pressures of the material in the molten source material. Thermal evaporation is generally done using thermally heated sources such as tungsten wire coils or by high energy electron beam (e-beam) heating of the source material itself. Generally, the substrates are mounted at an appreciable distance away from the evaporation source to reduce radiant heating of the substrate by the vaporization source.

Vacuum deposition is used to form optical interference coatings, mirror coatings, decorative coatings, permeation barrier films on flexible packaging materials, electrically conducting films, wear resistant coatings, and corrosion protective coatings.

Sputter Deposition

Sputter deposition (Ch. 7) is the deposition of particles vaporized from a surface (target) by the physical sputtering process. Physical sputtering is a non-thermal vaporization process where surface atoms are physically ejected from a solid surface by momentum transfer from an atomic-sized energetic bombarding particle, which is usually a gaseous ion, accelerated from a plasma. This PVD process is sometimes just called sputtering, i.e. sputtered films of —, which is an improper term in that the film is not being sputtered. Generally the source-to-substrate distance is short compared to vacuum deposition. Sputter deposition can be performed by energetic ion bombardment of a solid surface (sputtering target) in a vacuum using an ion gun or low pressure plasma (< 5 mTorr) (Ch. 5) where the sputtered particles suffer few or no gas phase collisions in the space between the target and the substrate.

Sputtering can also be done in a higher plasma pressure (5–30 mTorr) where energetic particles sputtered or reflected from the sputtering target are thermalized by gas phase collisions before they reach the substrate surface. The plasma used in sputtering can be confined near the sputtering surface or may fill the region between the source and the substrate. The sputtering source can be an element, alloy, mixture, or a compound and the material is vaporized with the bulk composition of the target. The sputtering target provides a long-lived vaporization source that can be mounted so as to vaporize in any direction. Compound materials such as TiN and zirconium nitride (ZrN) are commonly reactively sputter deposited by using a reactive gas in the plasma. The presence of the plasma activates the reactive gas (plasma activation), making it more chemically reactive.

Sputter deposition is widely used to deposit thin film metallization on semiconductor material, coatings on architectural glass, and reflective coatings on compact discs (CDs), and for magnetic films, dry film lubricants, hard coatings (tools, engine parts), and decorative coatings.

Arc Vapor Deposition

Arc vapor deposition (Ch. 8) uses a high current, low voltage arc to vaporize a cathodic electrode (cathodic arc) or anodic electrode (anodic arc) and deposit the vaporized material on a substrate. The vaporized material is highly ionized and usually the substrate is biased so as to accelerate the ions (film ions) to the substrate surface.

Arc vapor deposition is used to deposit hard and decorative coatings. The ions (film ions) that are formed in arc vaporization are useful in the ion plating process.

Ion Plating

Ion plating (Ch. 9), which is sometimes called ion-assisted deposition (IAD) or ion vapor deposition (IVD), utilizes concurrent or periodic bombardment of the depositing film by atomic-sized energetic particles to modify and control the properties of the depositing film. In ion plating the energy, flux, and mass of the bombarding species along with the ratio of bombarding particles to depositing particles are important processing variables. The depositing material may be vaporized either by evaporation, sputtering, arc erosion, or by decomposition of a chemical vapor precursor.

The energetic particles used for bombardment are usually ions of an inert or reactive gas, or, in some cases, ions of the condensing film material (film ions). Ion plating may be done in a plasma environment where ions for bombardment are extracted from the plasma or it may be done in a vacuum environment where ions for bombardment are formed in a separate ion gun. The latter ion plating configuration is often called ion beam-assisted deposition (IBAD). By using a reactive gas in the plasma, films of compound materials can be deposited. Ion plating can provide dense coatings at relatively high gas pressures where gas scattering can enhance surface coverage.

Ion plating is used to deposit hard coatings of compound materials, adherent metal coatings, optical coatings with high densities, and conformal coatings on complex surfaces.

1.1.2 Non-PVD Thin Film Atomistic Deposition Processes

There are a number of other thin film deposition processes that should be considered for certain applications. For example, a TiN hard coating can be deposited by PVD or chemical vapor deposition (CVD).

Chemical Vapor Deposition (CVD) and PECVD

Thermal CVD (or vapor plating) is the deposition of atoms or molecules by the high temperature reduction or decomposition of a chemical vapor precursor species, which contains the material to be deposited. Reduction is normally accomplished by hydrogen at an elevated temperature. Decomposition is accomplished by thermal activation. The deposited material may react with other gaseous species in the system to give compounds (e.g. oxides, nitrides). Chemical vapor deposition processing is generally accompanied by volatile reaction byproducts and unused precursor species. Chemical vapor deposition has numerous other names and adjectives associated with it such as vapor phase epitaxy (VPE) when CVD is used to deposit single crystal films, metalorganic CVD (MOCVD) when the precursor gas is a metalorganic species, plasma-enhanced CVD (PECVD) when a plasma is used to induce or enhance decomposition and reaction, and low pressure CVD (LPCVD) when the pressure is less than ambient.

Plasmas may be used in CVD reactors to activate and partially decompose the precursor species. This allows deposition at a temperature lower than thermal CVD and the process is called plasma-enhanced CVD (PECVD) or plasma-assisted CVD (PACVD). The plasmas are typically generated by radio frequency (rf) techniques. Figure 1.2 shows a parallel plate CVD reactor that uses rf power to generate the plasma. This type of PECVD reactor is in common use in the semiconductor industry to deposit silicon nitride (Si3N4) and phosphosilicate glass (PSG), encapsulating layers a few microns thick with deposition rates of 5–100 nm/min. At low pressures, concurrent energetic particle bombardment during deposition can affect the properties of films deposited by PECVD.

Figure 1.2 Parallel Plate Plasma-enhanced Chemical Vapor Deposition (PECVD) Reactor. Typical Parameters are: Radio Frequency (rf) – 50 kHz to 13.56 MHz; Temperature – 25 to 700°C; Pressure – 100 mTorr to 2 Torr; Gas Flowrate – 200 sccm

Plasma-based CVD may also be used to deposit polymer films (plasma polymerization). In this case the precursor vapor is a monomer that becomes crosslinked in the plasma and on the surface to form an organic or inorganic polymer film. These films have very low porosity and excellent surface coverage. When plasma depositing films from organo-silane precursors, oxygen can be added to the plasma to oxidize some of the silicon in the film.

Electroplating, Electroless Plating, and Displacement Plating

Electroplating is the deposition on the cathode of metallic ions from the electrolyte of an electrolysis cell. Only about 10 elements (Cr, Ni, Zn, Sn, In, Ag, Cd, Au, Pb, and Rh) are commercially deposited from aqueous solutions. Some alloy compositions such as Cu–Zn, Cu–Sn, Pb–Sn, Au–Co, Sn–Ni, Ni–Fe, Ni–P and Co–P are commercially deposited. Conductive oxides such as PbO2 and Cr2O3 can also be deposited by electroplating. A thin film of material deposited by electroplating is often called a flash and is on the order of 40 millionths of an inch thick. Typically, the anode of the electrolytic cell is of the material being deposited and is consumed in the deposition process. In some cases, the anode material is not consumed and the material to be deposited comes only from the solution, which must be continually replenished. For example, lead oxide, PbO2, can be electrodeposited from a lead nitrate plating bath using carbon anodes. Stainless steel and platinum are also often used as non-consumable anode materials.

In electroless or autocatalytic plating, no external voltage/current source is required. The voltage/current is supplied by the chemical reduction of an agent at the deposit surface. The reduction reaction is catalyzed by a material, which is often boron or phosphorous. Materials that are commonly deposited by electroless deposition are: Ni, Cu, Au, Pd, Pt, Ag, Co, and Ni–Fe alloys. Displacement plating is the deposition of ions in solution on a surface and results from the difference in electronegativity of the surface and the ions. The relative electronegativities (electromotive series) of some elements are shown in Table 1.2. For example, gold in solution will displacement plate-out on copper and lead will displacement plate-out on aluminum.

Table 1.2

Electrophoresis is the migration of charged particles in an electric field. Electrophoretic deposition, or electrocoating, is the electrodeposition of large charged particles from a solution.[1] The particles may be charged dielectric particles (glass particles, organic molecules, paint globules, etc.) that are non-soluble in the aqueous electrolyte. Alternatively, some of the components can be treated so that they are soluble in water but will chemically react in the vicinity of an electrode so their solubility is decreased. Particles are usually deposited on the anode but sometimes on the cathode (cataphoresis).

Chemical Reduction

Some thin films can be deposited from chemical solutions at low temperatures by immersion in a two-part solution that gives a reduction reaction. Chemical silvering of mirrors and vacuum flasks is a common example.[2,³] The glass surface to be silvered is cleaned very thoroughly then nucleated using a hot acidic stannous chloride solution or by vigorous swabbing with a saturated solution of SnCl2. The surface is then immediately immersed in the silvering solution where a catalyzed chemical reduction causes silver to be deposited on the glass surface. Copper oxide (Cu2O) films can be deposited from mixing solutions of CuSO4 + Na2S2O3 (sodium thiosulfate) and NaOH.

Elemental materials such as platinum, gold, tin, and indium can be deposited by the thermal decomposition of a chemical solution. For example, platinum can be deposited by the thermal decomposition of platinum chloride solution on the surface.

1.1.3 Applications of Vacuum-deposited Materials

Some of the most utilized applications of thin film deposition processes include:

• Single and multilayer films and coatings

• Nanolayered materials

• Optical films for transmission and reflection

• Decorative films

• Decorative and wear-resistant (decorative/functional) coatings

• Permeation barriers for moisture and gases

• Corrosion-resistant films

• Electrically insulating layers for microelectronics

• Coating of engine turbine blades

• Coating of high strength steels to avoid hydrogen embrittlement

• Diffusion barrier layers for semiconductor metallization

• Magnetic films for recording media

• Transparent electrical conductors and antistatic coatings

• Wear and erosion-resistant (hard) coatings (tool coatings)

• Dry film lubricants

• Composite and phase-dispersed films and coatings

• Nanocomposite materials

• Thin-walled freestanding structures and foils

Some materials deposited by PVD processes are as follows.

Some elements:

• Gold – electrical conductor, anticorrosion surface, surface replication, bondable surface, infrared (IR) reflectance

• Silver – electrical conductor, heat reflector, optical mirrors, low shear solid film lubricant

• Aluminum – electrical conductor, optical reflectance, corrosion resistance, permeation barrier

• Copper – electrical conductor, solderability

• Cadmium – corrosion resistance (being phased out)

• Zinc – corrosion resistance

• Titanium – glue layer to oxides

• Chromium – glue layer to oxides, corrosion resistance, hard coating

• Palladium – galvanic corrosion layer between Ti and Au

• Molybdenum – glue layer to oxides

• Tantalum – corrosion and erosion resistance

• Beryllium – freestanding X-ray windows

• Carbon (DLC) – hard coat, chemically resistant, low friction

• Nickel – glue layer to metals, basecoat on brass

• Silicon – semiconductor devices

• Selenium – photosensitive material

Some mixtures (physical mixtures or above solubility limits):

• Silicon + dopants – semiconductor devices

• Nanophase composites – hard coatings

Some glasses:

• Amorphous silicon (a–Si) – semiconductor, photovoltaic

• Phosphorus + silicon oxides (PSGs) – encapsulant

Some alloys:

• Zinc + aluminum – corrosion protection

• Aluminum + copper + silicon – semiconductor metallization

• Indium + tin/oxide – transparent electrical conductor, IR reflection

• Nickel + chromium – glue layer to oxides, electrical resistance

• Tungsten + titanium – semiconductor metallization, diffusion barrier (W:Ti [90:10 wt%; 70:30 at %])

Some compounds:

• Titanium nitride – diffusion barrier coating, tool coating, decorative coating

• Titanium/Carbon nitride – tool coating, decorative coating

• Titanium/Aluminum nitride – wear coating

• Chromium nitride – hard coating, low friction

• Aluminum oxide – permeation barrier, diffusion barrier

• Titanium oxide – high index optical coating

• Silicon dioxide – low index optical coating

• Magnesium fluoride – low index optical coating

• Molybdenum disulfide – solid film lubricant

• Molybdenum diselenide – solid film lubricant (electrical conductor)

• Tantalum oxide – high index optical coating

• Zinc sulfide – high index optical coating

Some layered systems:

• Ti/Au, Ti/Pd/Cu/Au, Ti/Ag, Ti/Pd/Ag – electrical conductor electrodes on oxides

• Cr/Au, Cr/Pd/Au – oxide metallization

• Mo/Au – oxide metallization

• TiN/Al – silicon metallization

• Ni/Cr – basecoat on brass

• Nanolayered composites – hard/wear coatings

• ZnOx : Ag : Zn (thin): ZnOx : TiOx – low-e (low emission) glass coating

• SnOx : Ag : NiCr (thin) : SnOx – low-e glass coating on glass

1.2 Thin Film Processing

1.2.1 Stages of Fabrication

The production of useful and commercially attractive engineered surfaces using PVD deposition processes involves a number of stages that are interdependent. The stages are:

• Choice of the substrate (real surfaceCh. 2).

• Defining and specifying critical properties of the substrate surface and how these can be determined.

• Development of an appropriate surface preparation process which includes cleaning and may involve changing the surface morphology or chemistry (surface modification).

• Selection of the film material(s) and film structure to produce the film adhesion and film properties required.

• Choice of the fabrication process to provide reproducible coating properties and long-term stability.

• Development of production equipment that will give the necessary product throughput.

• Development of the fabrication equipment, process parameters, parameter limits, and monitoring/control techniques to give a good product yield.

• Development of appropriate characterization techniques to determine the properties and stability of the product.

• Possibly the development of techniques for the reprocessing or repair of parts with defective coatings.

• Creation of written specifications and manufacturing process instructions (MPIs) for all stages of the processing.

1.2.2 Factors that Affect Film Properties

Deposited thin films and coatings generally have unique properties compared to the material in bulk form and there are no handbook values for such properties. There have been many books and articles on film deposition and film properties but generally these treatments do not emphasize the importance of the substrate surface and deposition conditions on the film properties. The properties of a film of a specific material formed by any atomistic deposition process depend on five factors, namely:

• Substrate surface condition before and after cleaning and surface modification – e.g. surface morphology (roughness, inclusions, particulate contamination), surface chemistry (surface composition, contaminants), mechanical properties, surface flaws, outgassing, preferential nucleation sites, and the stability of the surface.

• Details of the deposition process and system geometry – e.g. the deposition process used, angle-of-incidence distribution of the depositing adatom flux, substrate temperature, deposition rate, gaseous contamination, concurrent energetic particle bombardment (flux, particle mass, energy).

• Details of film growth on the substrate surface – e.g. condensation and nucleation of the arriving atoms (adatoms), interface formation, interfacial flaw generation, energy input to the growing film, surface mobility of the depositing adatoms, growth morphology of the film, gas entrapment, reaction with deposition ambient (including reactive deposition processes), changes in the film properties during deposition.

• Intermediate processing – e.g. periodic ion bombardment, oxidation between layers, wiping or burnishing between layers.

• Post-deposition processing and reactions – e.g. chemical reaction of the film surface with the ambient, subsequent processing, thermal or mechanical cycling, corrosion, interfacial degradation; surface treatments such as burnishing of soft surfaces, shot peening, overcoating (topcoat), or chemical modification such as chromate conversion. Changes due to service environment.

In order to have reproducible film properties, each of these factors must be reproducible. When problems occur in manufacturing, each of these factors should be considered as a possible source of the problem.

Chapter 2 discusses the real surface (substrate) on which the film must be deposited. The real surface never has the same composition as the bulk material. With some materials, such as polymers, the surface and bulk material are affected by its history.

Characterization of the elemental, phase, microstructural, morphological, and physical properties of real surfaces is important in establishing criteria for the reproducible surface necessary to produce reproducible film properties. The substrate surface morphology can have a large effect on the film morphology and properties, as discussed in Ch. 10. The physical and mechanical properties of the substrate surface can affect the performance of the film structure and the apparent adhesion of the film to the surface (Ch. 12). The real surface can be modified in desirable ways prior to the deposition of the film structure.

A contaminant can be defined as any material in the ambient or on the surface that interferes with the film formation process, affects the film properties, or influences the film stability in an undesirable way. In most cases the concern is with both the type and amount of the contaminant. Contaminants can cover the whole surface, as with oxide reaction layers or an adsorbed hydrocarbon layer, or they can be limited to restricted areas such as particulates or fingerprints. A major concern in processing is the variability of the contamination in such a manner as to affect product and process reproducibility.

Cleaning is the reduction of the type and amount of contamination to an acceptable level of the substrate surface; it is an important step in PVD processing and is discussed in Ch. 13. In PVD processing this cleaning can be done external to the deposition system (external cleaning) and internal to the deposition system (in situ cleaning). The manner in which a surface can be cleaned is often controlled, to some extent, by government regulations on pollution control (US EPA (Environmental Protection Agency)) and workplace safety (US OSHA (Occupational Safety and Health Administration)).

Contamination encountered in PVD processes can be categorized as:

• Substrate surface-related – e.g. oxide layers on metals, embedded particulates.

• Ambient (external) process-related – e.g. chemical residues, water stains.

• Ambient (external) environment-related – e.g. settled airborne particulates, adsorbed water vapor and hydrocarbons.

• Deposition environment-related – e.g. residual gases in the vacuum/plasma environment, water desorbed from vacuum surfaces, particulates and vapors in the deposition system.

• Deposition process-related – e.g. contaminant vapors and particulates from vaporization sources, fixtures and tooling.

• Post-deposition contamination – e.g. oxides formed on the free surfaces of the deposited film, adsorbed hydrocarbons.

Chapters 3, 4 and 5 discuss the environment in the deposition chamber and how this environment can contribute to contamination that affects film properties. The properties of the deposition environment are determined by contamination in the vacuum or plasma environment and contamination released by the processing. Often these sources of contamination can change with time due to changes in the internal surface area of the deposition system as film material builds up on fixtures and vacuum surfaces, degradation of the vacuum integrity of the system, degradation of the vacuum pumping system, buildup of contamination from all sources, catastrophic changes due to a lack of fail-safe design of the deposition system, and/or improper operating procedures. These changes can be reflected in product yield. Where very clean processing, as is used in the semiconductor industry, is required, contamination in the deposition ambient may be the controlling factor in product yield.

Chapter 14 discusses the external processing

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