Status of ALD MCP Program at Argonne

Anil Mane, Qing Peng, Joe Libera, Jeff Elam

LAPPD Project Second Microchannel Plate Godparent Review October 4, 2010

Outline

New hardware Resistive coatings Emissive coatings Scale-up

MCP Godparent Review Meeting 10-4-2010

Work Plan and Deliverables

Year 1 Emissive coatings Resistive coatings Begin scale-up Year 2 Stripe coating (Dynode Chain) Continue scale-up Year 3 Produce tiles

MCP Godparent Review Meeting 10-4-2010

New Hardware: Measurement and Testing

Mercury probe conductance of thin films in air, computer controlled

Shadow mask measure lateral resistance of thin films

MCP Godparent Review Meeting 10-4-2010

Vacuum setup HV conductance and thermal coefficient of MCPs

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New Hardware: MCP Gain Testing Setup

~10-7mbar vacuum

quartz window for UV

Next: MCP mount, electronics, safety plan

MCP Godparent Review Meeting 10-4-2010

New Hardware: Electroding and Fixtures

Fixture 1 - Clausing Fixture 2 - Fermilab

Frame with MCP

frame in rotary fixture

frame in rotary fixture

MCP Godparent Review Meeting 10-4-2010

New Hardware: Process Development and Scale-up

Large area reactor: substrate size 12 x 18, single 8 tile

Beneq TFS500 Multiple 8 tiles (up to 40)

MCP Godparent Review Meeting 10-4-2010

Resistive Coatings: Al2O3/ZnO (AZO)

Good: existing process Bad: hard to control (etching of ZnO by trimethyl aluminum precursor) Bad: big slope (105 resistance change over 10% composition change)

etching

MCP Godparent Review Meeting 10-4-2010

Cross-Sectional Image of ALD Film in MCP

Glass ALD Film

100 nm ALD film visible in middle of MCP 6 samples to testing group Testing: gain, then sparks
MCP Godparent Review Meeting 10-4-2010

Temperature Coefficient

10

12

Resistance (Ohms)

10

11

Standard Glass MCP: T=-0.02 Micromachined silica MCP: T=-0.036 20% AZO MCP: T=-0.06

10

10

10

20

30

40

50

60

70

80

T(C)

MCP Godparent Review Meeting 10-4-2010

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Resistive coatings: MgO/ZnO (MZO)

Quartz Microbalance Data: Thickness (Angstroms)

No etching in MZO Resistance is tunable MgO is candidate for SEY layer No MCPs made yet with MZO

MCP Godparent Review Meeting 10-4-2010

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Patterned electrodes for testing ALD films: in-plane versus thru-film resistance
Electrode Pad ALD film

glass

MCP Godparent Review Meeting 10-4-2010

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Resistance of ALD AZO and MgZnO

AZO Thru-film

AZO

In plane

2.64e5 ohmcm

26 ohmcm

Thru-film MgZnO

MgZnO

In plane

2.29e2 ohmcm

0.20ohmcm

In plane resistivity ~x103-104 higher than thru-film (preliminary)

MCP Godparent Review Meeting 10-4-2010

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Resistive Coatings: Chemistry 1

No etching Resistance is tunable, small slope (102 over 10%) T=-0.027 Very reproducible (different locations, different batches) MCPs work: (20 micron, 60 L/D, 1x106 gain at 1200V) 11 MCPs to testing group

MCP Godparent Review Meeting 10-4-2010

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Photographs of bare MCP(a), After ALD chemisty-1 coating (b) and after ALD chemisty-1 coating + 200nm Cr electrode (c).
a) Bare MCP b) After ALD c) After ALD + Cr electrode

SEM analysis of chemisty-1 coated MCP (d) Top surface low magnification, (e) top surface high magnification and (f) Cross-section of MCP.
(d) (e) (f)

Image taken from middle of MCP

MCP Godparent Review Meeting 10-4-2010

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ALD resistive coating on MCP: Chemistry 1

Resistivity vs. % W in Al2O3 on MCP 1.E+14
Resistivity (ohm-cm)
AFM on planer substrate (Courtesy: Hau Wang)

1.E+12 1.E+10
1.E+08 1.E+06

10% Roughness 0.506nm

20% 0.889nm

30% 1.41nm

Maximum RMS roughness < 3% Workable resistivity range for 33mm MCP

10

15

20

25

30
I(A)

35
MCP

30% W in Al2O3
2.E-07 y = 1E-08x - 2E-09 1.E-07

% of metal ALD cycles doping in oxide

W % in Al2O3

Uniform and smooth ALD coating pores of MCP

-1.E-21

-10

-5
-1.E-07

10

-2.E-07 V(V)

Linear I-V on MCP

MCP Godparent Review Meeting 10-4-2010

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Reproducibility: ALD Chemistry 1

Thickness on Si(100)
660 Thickness
Thickness [A]

Resistance
1.E+14
Resistance (ohm)

650 640 630

Composition A Composition B

1.E+12 1.E+10 1.E+08 1.E+06 0

Composition A Composition B

On Glass On MCP

620 0 5 10 # of MCP 15 20

10 # of MCP

15

20

Excellent reproducible thickness and resistance on Glass Resistance variation on MCP cause by electrode variations (end spoiling not controlled)

MCP Godparent Review Meeting 10-4-2010

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MCP resistance stability (air vs. vacuum) Chemistry 1

MCP# 122 Photonis electrode first + + ALD resistive chem-1 + SEE coating

Vacuum break I-V measured after 4 days

R=150M at RT

Stable I-V response in vacuum

MCP Godparent Review Meeting 10-4-2010

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ALD coated MCP resistance stability in vacuum Chemistry 1

MCP# 122 Photonis electrode first + ALD resistive chem-1 + SEE coating

200 180 160

R=150 M

Resistance variation <5%

MCP resistance (M)

140 120 100 80 60 40 20 0 0 2 4 6 8 10

Data collected at constant 100V condition (heating of MCP?)

Time (days)

Very stable resistance performance with less than 5% resistance variation I-V set-up upgrade in progress, will allow I-V testing for ~1.5kV

MCP Godparent Review Meeting 10-4-2010

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Resistivity of ALD coating on Glass: Chemistry #2

1.E+15

Data on Glass
Workable resistivity range for 33mm MCP

Resistivity (ohm-cm)

1.E+12
1.E+09 1.E+06 1.E+03 1.E+00 0

Linear I-V on Glass

5 10 Mo % in Al2O3 % of metal ALD cycles doping in oxide

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Better control process than chemistry 1: uniform and smooth ALD coating
Similar resistivity range (like chemisty 1) T=-0.033 Process tested on large substrates capable ALD reactor
MCP Godparent Review Meeting 10-4-2010

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Phosphor image of ALD functionalized MCP with chemistry 2 and Al2O3 SEE layer

@1200V

(Ossy)

MPC works

MCP Godparent Review Meeting 10-4-2010

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Spacers resistance tuning by ALD

Tune spacer resistance using ALD resistive coatings

MCP Godparent Review Meeting 10-4-2010

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Spacers resistance tuning by ALD (used Chemistry 1)

In-situ resistance monitoring
Spacer 1 Spacer 2 Spacer 3 Total R = R1+R2+R3

Total Resistance (R1+R2+R3, )

Chem -1 Compositon-2

Chem -1 Compositon-1

Can tune spacer resistance using thickness and composition

MCP Godparent Review Meeting 10-4-2010

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Emissive Coatings
Substrates: Si(100) - conductive, smooth, flat, cheap Photonis MCPs ALD MCPs Films: Al2O3, MgO, SiO2, ZnO/Al2O3 Diamond (UNCD) film awaiting test 1-100 nm ~60 samples to characterization group

No ALD

ALD (Ossy)

MCP Godparent Review Meeting 10-4-2010

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Process scale-up: Chemistry 2 in large area coater

12x12 Glass For initial test, used same pressures and timings as small reactor

300mm Si wafer
MCP Godparent Review Meeting 10-4-2010

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Large substrate testing: ALD Chemistry #2

Location across substrate
150

Thickness
794.0 791.6

150

Index of refraction
1.773 1.766

100

100

50

789.3 786.9

50

1.759 1.751

Y(mm)

Y(mm)

784.5 782.1

1.744 1.737

-50

-50

1.730 1.722

779.8
-100

777.4 775.0

-100

1.715

-150 -150

-100

-50

50

100

150

-150 -150

-100

-50

50

100

150

X (mm)

X (mm)

Location across substrate Item

Minimum Maximum

Thickness [A]
775 794

Index of refraction (n)

1.72 1.77

Average
% STDV (1)

785
0.57

1.73
0.84

MCP Godparent Review Meeting 10-4-2010

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Scale-up

8x8MCP

First test: Al2O3 on 8x8 capillary glass array

MCP Godparent Review Meeting 10-4-2010

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