CENTER FOR NANOSCALE SCIENCE AND ENGINEERING
Standard Operating Procedures
Edwards Thermal Evaporator
Matt Deye and Brian Wajdyk
Version 1.1
Page 1 of 13
Important
•
•
•
•
•
•
•
Gloves should be worn while handling substrate and deposition material to reduce
contamination.
Do not press “Stop” or “Start” buttons. They should be covered by a glass slide and labeled with
a warning.
Please return chamber to a vacuum when done with ma
machine.
chine. This ensures no atmospheric
contamination.
You can only use CeNSE laboratories and equipment if you have been approved by Brian or
Chuck, reserved the tool on the calendar, and filled out a form. No Exceptions!
If the equipment is acting unusual SSTOP!
TOP! Please discuss with Brian or Chuck before proceeding
and leave a note on the machine.
Any accidental damage must be reported immediately.
All CeNSE laboratories are protected by video surveillance.
Version 1.1
Page 2 of 13
Machine exterior and chamber
Device controls
Version 1.1
Page 3 of 13
Machine exterior and chamber
Device controls
Version 1.1
Page 4 of 13
Operating Procedure
1. Preparation
1.1. Before beginning, be sure to wear gloves to reduce contamination.
2. Pressurize chamber
2.1. Press vent on chamber pressure controller (Fig 2a) – system will slowly pressurize to
atmospheric pressure. This will take approximately 3 to 5 minutes.
2.2. Once atmospheric pressure has been reached (~760 torr) the chamber door will
release.
2.3. A hissing sound will be observed coming from the machine. This is nitrogen gas
purging the system. After several seconds, press “seal” on chamber pressure
controller (Fig 2a) to stop purge.
3. Load Chamber
3.1. This evaporator is capable of accepting two deposition materials at once. The
evaporator has an upper and lower electrode.
3.2. Clip sample onto stage at top of chamber.
3.3. Select a tungsten filament or boat with appropriate deposition material. Using a hex
wrench, tighten filament onto desired electrode.
4. Closing Chamber
4.1. Ensure that all samples, deposition materials are loaded and secured.
4.2. Close and lock chamber door
4.3. Hit “Cycle” on chamber pressure controller (Fig 2a) be begin vacuum cycle.
4.4. Proceed to next step once a chamber pressure range of 10-5 torr has been reached.
5. Set thickness gauge
5.1. Using the thickness gauge (Fig 2c), press the “Data” button until the “Layer” LED is
lit. This thickness gauge is capable of measuring two different films.
5.2. Using the “Data” button, select the “Density” LED. Use the “Up” and “Down”
buttons to enter the density of your first deposition material from appendix A,
provided at the end of this document.
5.3. Using the “Data” button, select either the nm or µm LED. Use the “Up” or “Down”
buttons to select your desired thickness.
5.4. Proceed to the next step.
6. Evaporating the deposition material.
6.1. With the shutter in the “closed” position (Fig 1a), and with the chamber pressure in
the 10-5 torr range, choose the deposition source material on the amperage control
(Fig 2d).
6.2. With the shutter still closed, slowly turn up the amperage on the power supply
while monitoring chamber vacuum. Continue until a change in vacuum pressure
Version 1.1
Page 5 of 13
occurs or tungsten boat begins to glow. Once this occurs, leave the machine for 5
minutes.
6.3. After 5 minutes, increase amperage on power supply until thermal evaporation of
source material occurs.
6.3.1. Ensure vacuum does not go beyond the 10-3 torr range
6.3.2. Adjust amperage to achieve desired deposition rate. Once
achieved, open shutter and press the “Run” button on the
thickness monitor.
6.4. Monitor thickness gauge until desired thickness is achieved.
6.4.1. Thickness gauge will dim the LED displaying “shutter open”. This
indicates that the desired thickness has been achieved.
6.4.2. Once target thickness is achieved, close shutter and slowly turn
down power supply amperage. Turn power supply back to zero.
6.5. For second material, repeat steps 6.1 through 6.4
7. Opening chamber
7.1. Once deposition procedure is complete, wait 10 minutes for boat to cool. Failure to
do so can oxidize boat and deposition material.
7.2. After 10 minutes, press “vent” on the chamber pressure controller (Fig 2a). The
chamber will now begin to pressurize. It will take approximately 3 to 5 minutes to
reach atmospheric pressure. The chamber pressure controller will display “Sealed”
when this occurs.
7.3. Remove deposition material and sample.
7.4. Return chamber to vacuum by pressing “cycle” on the chamber pressure controller
(Fig 2a).
Version 1.1
Page 6 of 13
Appendix A: Deposition Material
Properties
Deposition material properties:1
Formula
Ag
AgBr
AgCl
Al
Al2O3
Al4C3
AlF3
AlN
AlSb
As
As2Se3
Au
B
B2O3
B4C
BN
Ba
BaF2
BaN2O6
BaO
BaTiO3
BaTiO3
Be
BeF2
BeO
Bi
Bi2O3
Bi2S3
Bi2Se3
1
Density
10.5
6.47
5.56
2.70
3.97
2.36
3.07
3.26
4.36
5.73
4.75
19.3
2.37
1.82
2.37
1.86
3.5
4.886
3.244
5.72
5.999
6.035
1.85
1.99
3.01
9.8
8.9
7.39
6.82
Z-Ratio
0.529
1.18
1.32
1.08
0.336
?
?
?
0.743
0.966
?
0.381
0.389
?
?
?
2.1
0.793
1.261
?
0.464
0.412
0.543
?
?
0.79
?
?
?
Acoustic
Impedance
16.69
7.48
6.69
8.18
26.28
11.88
9.14
23.18
22.70
4.20
11.13
7.00
19.03
21.43
16.26
11.18
SQM-160 User’s Guide, Version 4.06. Sigma Instruments, Inc. 2000-2008.
Version 1.1
Page 7 of 13
Material Name
Silver
Silver Bromide
Silver Chloride
Aluminum
Aluminum Oxide
Aluminum Carbide
Aluminum Fluoride
Aluminum Nitride
Aluminum Antimonide
Arsenic
Arsenic Selenide
Gold
Boron
Boron Oxide
Boron Carbide
Boron Nitride
Barium
Barium Fluoride
Barium Nitrate
Barium Oxide
Barium Titanate (Tetr)
Barium Titanate (Cubic)
Beryllium
Beryllium Fluoride
Beryllium Oxide
Bismuth
Bismuth Oxide
Bismuth Trisuiphide
Bismuth Selenide
Formula
Bi2Te3
BiF3
C
C
C8H8
Ca
CaF2
CaO
CaO-SiO2
CaSO4
CaTiO3
CaWO4
Cd
CdF2
CdO
CdS
CdSe
CdTe
Ce
CeF3
CeO2
Co
CoO
Cr
Cr2O3
Cr3C2
CrB
Cs
Cs2SO4
CsBr
CsCl
CsI
Cu
Cu2O
Cu2S
Cu2S
CuS
Dy
Dy2O3
Er
Version 1.1
Density
7.7
5.32
2.25
3.52
1.1
1.55
3.18
3.35
2.9
2.962
4.1
6.06
8.64
6.64
8.15
4.83
5.81
6.2
6.78
6.16
7.13
8.9
6.44
7.2
5.21
6.68
6.17
1.87
4.243
4.456
3.988
4.516
8.93
6
Cu2S
Cu2S
CuS
Dy
Dy2O3
Er
Z-Ratio
?
?
3.26
0.22
?
2.62
0.775
?
?
0.955
?
?
0.682
?
?
1.02
?
0.98
?
?
?
0.343
0.412
0.305
?
?
?
?
1.212
1.41
1.399
1.542
0.437
?
5.6
5.8
4.6
8.55
7.81
9.05
Acoustic
Impedance
2.71
40.14
3.37
11.39
9.25
12.95
8.66
9.01
25.74
21.43
28.95
7.29
6.26
6.31
5.73
20.21
1.58
1.52
1.92
1.03
1.13
0.98
Page 8 of 13
Material Name
Bismuth Telluride
Bismuth Fluoride
Carbon (Graphite)
Carbon (Diamond)
Parlyene (Union Carbide)
Calcium
Calcium Fluoride
Calcium Oxide
Calcium Silicate (3)
Calcium Sulfate
Calcium Titanate
Calcium Tungstate
Cadmium
Cadmium Fluoride
Cadmium Oxide
Cadmium Sulfide
Cadmium Selenide,
Cadmium Telluride
Cerium
Cerium (III) Fluoride
Cerium (IV) Dioxide
Cobalt
Cobalt Oxide
Chromium
Chromium (III) Oxide
Chromium Carbide
Chromium Boride
Cesium
Cesium Sulfate
Cesium Bromide
Cesium Chloride
Cesium Iodide
Copper
Copper Oxide
Copper (I) Sulfide (Alpha)
Copper (I) Sulfide (Beta)
Copper (II) Sulfide
Dysprosium
Dysprosium Oxide
Erbium
Formula
Er2O3
Eu
EuF2
Fe
Fe2O3
FeO
FeS
Ga
Ga2O3
GaAs
GaN
GaP
GaSb
Gd
Gd2O3
Ge
Ge3N2
GeO2
GeTe
Hf
HfB2
HfC
HfN
HfO2
HfSi2
Hg
Ho
Ho2O3
In
In2O3
In2Se3
In2Te3
InAs
InP
InSb
Ir
K
KBr
KCl
KF
Version 1.1
Density
Er2O3
Eu
EuF2
7.86
5.24
5.7
4.84
5.93
5.88
5.31
6.1
4.1
5.6
7.89
7.41
5.35
5.2
6.24
6.2
13.09
10.5
12.2
13.8
9.68
7.2
13.46
8.8
8.41
7.3
7.18
5.7
5.8
5.7
4.8
5.76
22.4
0.86
2.75
1.98
2.48
Z-Ratio
8.64
5.26
6.5
0.349
?
?
?
0.593
?
1.59
?
?
?
0.67
?
0.516
?
?
?
0.36
?
?
?
?
?
0.74
0.58
?
0.841
?
?
?
?
?
0.769
0.129
10.189
1.893
2.05
?
Acoustic
Impedance
1.02
1.68
1.36
25.30
14.89
5.55
13.18
17.11
24.53
11.93
15.22
10.50
11.48
68.45
0.87
4.66
4.31
Page 9 of 13
Material Name
Erbium Oxide
Europium
Europium Fluoride
Iron
Iron Oxide
Iron Oxide
Iron Sulphide
Gallium
Gallium Oxide (B)
Gallium Arsenide
Gallium Nitride
Gallium Phosphide
Gallium Antimonide
Gadolinium
Gadolinium Oxide
Germanium
Germanium Nitride
Germanium Oxide
Germanium Telluride
Hafnium
Hafnium Boride,
Hafnium Carbide
Hafnium Nitride
Hafnium Oxide
Hafnium Silicide
Mercury
Holminum
Holminum Oxide
Indium
Indium Sesquioxide
Indium Selenide
Indium Telluride
Indium Arsenide
Indium Phosphide
Indium Antimonide
Iridium
Potassium
Potassium Bromide
Potassium Chloride
Potassium Fluoride
Formula
KI
La
La2O3
LaB6
LaF3
Li
LiBr
LiF
LiNbO3
Lu
Mg
MgAl2O4
MgAl2O6
MgF2
MgO
Mn
MnO
MnS
Mo
Mo2C
MoB2
MoO3
MoS2
Na
Na3AlF6
Na5AL3F14
NaBr
NaCl
NaClO3
NaF
NaNO3
Nb
Nb2O3
Nb2O5
NbB2
NbC
NbN
Nd
Nd2O3
NdF3
Version 1.1
Density
3.128
6.17
6.51
2.61
5.94
0.53
3.47
2.638
4.7
9.84
1.74
3.6
8
3.18
3.58
7.2
5.39
3.99
10.2
9.18
7.12
4.7
4.8
0.97
2.9
2.9
3.2
2.17
2.164
2.558
2.27
8.578
7.5
4.47
6.97
7.82
8.4
7
7.24
6.506
Z-Ratio
2.077
0.92
?
?
?
5.9
1.23
0.778
0.463
?
1.61
?
?
0.637
0.411
0.377
0.467
0.94
0.257
?
?
?
?
4.8
?
?
?
1.57
1.565
0.949
1.194
0.492
?
?
?
?
?
?
?
?
Acoustic
Impedance
4.25
9.60
1.50
7.18
11.35
19.07
5.48
13.86
21.48
23.42
18.91
9.39
34.36
1.84
5.62
5.64
9.30
7.40
17.95
Page 10 of 13
Material Name
Potassium Iodide
Lanthanum
Lanthanum Oxide
Lanthanum Boride
Lanthanum Fluoride
Lithium
Lithium Bromide
Lithium Fluoride
Lithium Niobate
Lutetium
Magnesium
Magnesium Aluminate
Spinel
Magnesium Fluoride
Magnesium Oxide
Manganese
Manganese Oxide
Manganese (II) Sulfide
Molybdenum
Molybdenum Carbide
Molybdenum Boride
Molybdenum Trioxdide
Molybdenum Disulfide
Sodium
Cryolite
Chiolite
Sodium Bromide
Sodium Chloride
Sodium Chlorate
Sodium Fluoride
Sodium Nitrate
Niobium (Columbium)
Niobium Trioxide
Niobium (V) Oxide
Niobium Boride
Niobium Carbide
Niobium Nitride
Neodynium
Neodynium Oxide
Neodynium Fluoride
Formula
Ni
NiCr
NiCrFe
NiFe
NiFeMo
NiO
P3N5
Pb
PbCl2
PbF2
PbO
PbS
PbSe
PbSnO3
PbTe
Pd
PdO
Po
Pr
Pr2O3
Pt
PtO2
Ra
Rb
Rbl
Re
Rh
Ru
S8
Sb
Sb2O3
Sb2S3
Sc
Sc2O3
Se
Si
Si3N4
SiC
SiO
SiO2
Version 1.1
Density
8.91
8.5
8.5
8.7
8.9
7.45
2.51
11.3
5.85
8.24
9.53
7.5
8.1
8.1
8.16
12.038
8.31
9.4
6.78
6.88
21.4
10.2
5
1.53
3.55
21.04
12.41
12.362
2.07
6.62
5.2
4.64
3
3.86
4.81
2.32
3.44
3.22
2.13
2.648
Z-Ratio
0.331
?
?
?
?
?
?
1.13
?
0.661
?
0.566
?
?
0.651
0.357
?
?
?
?
0.245
?
?
2.54
?
0.15
0.21
0.182
2.29
0.768
?
?
0.91
?
0.864
0.712
*1000
?
0.87
1
Acoustic
Impedance
26.68
7.81
13.36
15.60
13.56
24.73
36.04
3.48
58.87
42.05
48.52
3.86
11.50
9.70
10.22
12.40
10.15
8.83
Page 11 of 13
Material Name
Nickel
Nichrome
Inconel
Permalloy
Supermalloy
Nickel Oxide
Phosphorus Nitride
Lead
Lead Chloride
Lead Fluoride
Lead Oxide
Lead Sulfide
Lead Selenide
Lead Stannate
Lead Telluride
Palladium
Palladium Oxide
Polonium
Praseodymium
Praseodymium Oxide
Platinum
Platinum Oxide
Radium
Rubidium
Rubidium Iodide
Rhenium
Rhodium
Ruthenium
Sulphur
Antimony
Antimony Trioxide
Antimony Trisulfide
Scandium
Scandium Oxide
Selenium
Silicon
Silicon Nitride
Silicon Carbide
Silicon (II) Oxide
Silicon Dioxide
Formula
Sm
Sm2O3
Sn
SnO2
SnS
SnSe
SnTe
Sr
SrF2
SrO
Ta
Ta2O5
TaB2
TaC
TaN
Tb
Tc
Te
TeO2
Th
ThF4
ThO2
ThOF2
Ti
Ti2O3
TiB2
TiC
TiN
TiO
TiO2
Tl
TlBr
TlCl
TlI
U
U3O8
U4O9
UO2
V
V2O5
Version 1.1
Density
7.54
7.43
7.3
6.95
5.08
6.18
6.44
2.6
4.277
4.99
16.6
8.2
11.15
13.9
16.3
8.27
11.5
6.25
5.99
11.694
6.32
9.86
9.1
4.5
4.6
4.5
4.93
5.43
4.9
4.26
11.85
7.56
7
7.09
19.05
8.3
10.969
10.97
5.96
3.36
Z-Ratio
0.89
?
0.724
?
?
?
?
?
0.727
0.517
0.262
0.3
?
?
?
0.66
?
0.9
0.862
0.484
?
0.284
?
0.628
?
?
?
?
?
0.4
1.55
?
?
?
0.238
?
0.348
0.286
0.53
?
Acoustic
Impedance
9.92
12.20
12.15
17.08
33.70
29.43
13.38
9.81
10.24
18.24
31.09
14.06
22.08
5.70
37.10
25.37
30.87
16.66
Page 12 of 13
Material Name
Samarium
Samarium Oxide
Tin
Tin Oxide
Tin Sulfide
Tin Selenide
Tin Telluride
Strontium
Strontium Fluroide
Strontium Oxide
Tantalum
Tantalum (V) Oxide
Tantalum Boride
Tantalum Carbide
Tantalum Nitride
Terbium
Technetium
Tellurium
Tellurium Oxide
Thorium
Thorium (IV) Fluoride
Thorium Dioxide
Thorium Oxyfluoride
Titanium
Titanium Sesquioxide
Titanium Boride
Titanium Carbide
Titanium Nitride
Titanium Oxide
Titanium (IV) Oxide
Thallium
Thallium Bromide
Thallium Chloride
Thallium Iodide (B)
Uranium
Tri Uranium Octoxide
Uranium Oxide
Uranium Dioxide
Vanadium
Vanadium Pentoxide
Formula
VB2
VC
VN
VO2
W
WB2
WC
WO3
WS2
WSi2
Y
Y2O3
Yb
Yb2O3
Zn
Zn3Sb2
ZnF2
ZnO
ZnS
ZnSe
ZnTe
Zr
ZrB2
ZrC
ZrN
ZrO2
Version 1.1
Density
5.1
5.77
6.13
4.34
19.3
10.77
15.6
7.16
7.5
9.4
4.34
5.01
6.98
9.17
7.04
6.3
4.95
5.61
4.09
5.26
6.34
6.49
6.08
6.73
7.09
5.6
Z-Ratio
?
?
?
?
0.163
?
0.151
?
?
?
0.835
?
1.13
?
0.514
?
?
0.556
0.775
0.722
0.77
0.6
?
0.264
?
?
Acoustic
Impedance
54.17
58.48
10.57
7.81
17.18
15.88
11.39
12.23
11.47
14.72
33.45
Page 13 of 13
Material Name
Vanadium Boride
Vanadium Carbide
Vanadium Nitride
Vanadium Dioxide
Tungsten
Tungsten Boride
Tungsten Carbide
Tungsten Trioxide
Tungsten Disulphide
Tungsten Suicide
Yttrium
Yttrium Oxide
Ytterbium
Ytterbium Oxide
Zinc
Zinc Antimonide
Zinc Fluoride
Zinc Oxide
Zinc Sulfide
Zinc Selenide
Zinc Telluride
Zirconium
Zirconium Boride
Zirconium Carbide
Zirconium Nitride
Zirconium Oxide