CENTER FOR NANOSCALE SCIENCE AND ENGINEERING
Standard Operating Procedures
Bell-Jar Thermal Evaporator
Brian Wajdyk
With revisions by:
Ross Levine
Rui Zhu
Version 1.1
Page 1 of 15
Important
•
•
•
•
•
•
Gloves should be worn while handling substrate and deposition to reduce contamination.
It is of utmost importance that the foreline and roughing valves never be opened at the same
time. If both are ever open simultaneously, the machine will be ruined.
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 STOP! Please discuss with Brian or Chuck before
bef
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 15
Machine exterior and chamber
Version 1.1
Page 3 of 15
Device controls
Version 1.1
Page 4 of 15
Operating Procedure
1. Preparation
1.1. Before beginning, be sure to wear gloves to reduce contamination and to protect the hands.
2. Warm up the diffusion pump
2.1. Open the foreline valve by turning the knob counter clockwise as far as it will turn.
2.2. Turn on the foreline pump, using the powerstrip on the back of the unit. This is important to do
before turning on the diffusion pump because the outlet of the diffusion pump (the foreline)
needs a lower pressure to operate.
2.3. If it is not already zeroed, Press the zero button on the deposition panel (figure 2a). This will
keep track of the amount of time the diffusion pump has been warming up.
2.4. Turn the pressure sensor switch to position 1, which monitors the foreline pressure with a
thermocouple (figure 2a). The markings on the top of the gauge in are the readings of this
gauge, in mTorr. The pressure should begin to drop.
2.5. When the foreline pressure reads below 50 mTorr, turn on the diffusion pump toggle switch
(figure 2d). Care must be taken here to observe the TC1 pressure while switching the diffusion
pump on. If there is too much air pressure in the inlet to the diffusion pump, the foreline
pressure (the outlet) may rise too quickly. If the foreline pressure ever rises above 200 mTorr
while the diffusion pump is running, oil may be forced back up towards the bell jar, ruining
the system. Do not allow this to happen.
3. Load the bell jar
3.1. Open the air inlet and wait for several minutes until the bell jar returns to atmospheric
pressure.
3.2. Close the air inlet and slowly lift the bell jar upwards.
3.3. Place the boat with the deposition materials between the electrodes (figure 1a).
3.4. Mount the sample on the stage, facing downwards (figure 1a).
3.5. Ensure that the shutter is between the sample and the boat (figure 1a).
3.6. Slowly pull the bell jar down until it rests on the machine.
4. Configure the deposition
4.1. Press the “program” button on the deposition panel (figure 2b).
4.2. Using the dial on the film controls, select the film number that corresponds to the deposition
material in the table in Appendix A (figure 2b).
4.3. Press the “next” button. This will load the material parameters into memory. Ensure that the
material parameters match those listed in Appendix A (figure 2b).
4.4. Press the “program” button again to save the selection (figure 2b).
Version 1.1
Page 5 of 15
Operating Procedure, continued
5. Pump down the chamber
5.1. Wait until the deposition panel shows that 30 minutes have passed. This is important because
if the oil is not thoroughly heated, backflow may occur which will destroy the system.
5.2. Confirm that the chrome isolation valve is closed.
5.3. Flip on the roughing pump toggle switch (figure 2d).
5.4. Open the roughing valve all the way. Also, make sure the air inlet is closed.
5.5. Turn the pressure gauge to position 2 (figure 2a).
5.6. Wait until the foreline pressure is below 50 mTorr (figure 2a).
5.7. Close the roughing valve completely.
5.8. Open the isolation valve slowly. After turning it 5 to 7 turns, you may open it more rapidly.
Ensure that there is not a sudden change in pressure; this may signify that something is wrong.
5.9. After opening the isolation valve, wait 20-30 minutes until the pressure is around 10-6 Torr.
6. Begin deposition
6.1. Turn on the ion gauge by flipping the power switch on (figure 2c).
6.2. Flip the filament switch on the ion gauge (not the one on the main machine) for a second or
two (figure 2c). Look behind the machine to ensure the filament stays on for several seconds.
If it turns off, flip the switch again. This may take several tries.
6.3. Turn on the filament toggle switch on the machine (figure 2d).
6.4. Turn the dial on the power regulator until you can see a glow through the window (figure 1b).
6.5. Wait a few minutes until the vacuum stabilizes on the ion gauge (figure 2c).
6.6. Press the zero button on the deposition panel (figure 2b).
6.7. Open the shutter (figure 1b).
7. End Deposition
7.1.
7.2.
7.3.
7.4.
7.5.
7.6.
When the desired thickness has been achieved, close the shutter (figure 1b).
Slowly turn the power regulator to zero (figure 1b).
Turn off the filament toggle switch on the machine (figure 2d).
Close the isolation valve completely.
Turn off the diffusion pump toggle switch (figure 2d).
Wait 30 minutes for the chamber to cool.
8. Unload the sample
8.1. Close the foreline valve.
8.2. Use the air inlet valve on the left of the machine to vent the bell jar.
8.3. Raise the bell jar, unload the samples, and lower the bell jar.
Version 1.1
Page 6 of 15
Operating Procedure, continued
9. When you are done with the machine
9.1. Rough the bell jar:
9.1.1. Open the roughing valve.
9.1.2. Wait until the pressure gauge reads 100 mTorr (figure 2a).
9.1.3. Close the roughing valve.
9.2. Turn off the roughing pump toggle switch (figure 2d).
9.3. Switch off the powerstrip in the back of the unit.
Version 1.1
Page 7 of 15
Appendix A: Film selection
This table is used in step 4.2 to determine which film to select.
Film Number
Film 1
Film 2
Film 3
Film 4
Film 5
Film 6
Film 7
Film 8
Film 9
Deposition Material
Density
Z-Ratio
Aluminum
Titanium
Copper
Gold
Silicon
Nickel
Platinum
Silicon Dioxide
Custom
2.70
4.50
8.93
19.3
2.32
8.91
21.4
2.648
1.08
0.628
0.437
0.381
0.712
0.331
0.245
1.00
See below
Using film 9 to set your own deposition material:
1. Refer to the next pages for material properties for your deposition material.
2. Use only film 9 for custom settings. Never change the settings for films 1-8.
3. When setting the film number as per step 4.2 in the operating procedure, turn the dial on the film
controls until “Film 9” is displayed.
4. Press the “next” button.
5. Rotate the dial to set the density to the appropriate value.
6. Use the “next” and “previous” buttons to cycle through density, tooling factor, z-ratio, and desired
final thickness. If you make a mistake, press the “clear” button.
7. Press the “program” button when done to save your settings. Proceed to step 4 of the operating
procedures.
Version 1.1
Page 8 of 15
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
Bi2Te3
BiF3
C
C
C8H8
Ca
CaF2
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
7.7
5.32
2.25
3.52
1.1
1.55
3.18
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
?
?
?
?
?
3.26
0.22
?
2.62
0.775
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
2.71
40.14
3.37
11.39
SQM-160 User’s Guide, Version 4.06. Sigma Instruments, Inc. 2000-2008.
Version 1.1
Page 9 of 15
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
Bismuth Telluride
Bismuth Fluoride
Carbon (Graphite)
Carbon (Diamond)
Parlyene (Union Carbide)
Calcium
Calcium Fluoride
Formula
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
Er2O3
Eu
EuF2
Fe
Fe2O3
FeO
FeS
Version 1.1
Density
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
Er2O3
Eu
EuF2
7.86
5.24
5.7
4.84
Z-Ratio
?
?
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
8.64
5.26
6.5
0.349
?
?
?
Acoustic
Impedance
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
1.02
1.68
1.36
25.30
Page 10 of 15
Material Name
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
Erbium Oxide
Europium
Europium Fluoride
Iron
Iron Oxide
Iron Oxide
Iron Sulphide
Formula
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
KI
La
La2O3
LaB6
LaF3
Li
LiBr
Version 1.1
Density
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
3.128
6.17
6.51
2.61
5.94
0.53
3.47
Z-Ratio
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
?
2.077
0.92
?
?
?
5.9
1.23
Acoustic
Impedance
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
4.25
9.60
1.50
7.18
Page 11 of 15
Material Name
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
Potassium Iodide
Lanthanum
Lanthanum Oxide
Lanthanum Boride
Lanthanum Fluoride
Lithium
Lithium Bromide
Formula
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
Ni
NiCr
NiCrFe
NiFe
NiFeMo
NiO
P3N5
Version 1.1
Density
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
8.91
8.5
8.5
8.7
8.9
7.45
2.51
Z-Ratio
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
?
?
?
?
?
?
?
?
0.331
?
?
?
?
?
?
Acoustic
Impedance
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
26.68
Page 12 of 15
Material Name
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
Nickel
Nichrome
Inconel
Permalloy
Supermalloy
Nickel Oxide
Phosphorus Nitride
Formula
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
Sm
Sm2O3
Sn
SnO2
SnS
SnSe
SnTe
Version 1.1
Density
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
7.54
7.43
7.3
6.95
5.08
6.18
6.44
Z-Ratio
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
0.89
?
0.724
?
?
?
?
Acoustic
Impedance
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
9.92
12.20
Page 13 of 15
Material Name
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
Samarium
Samarium Oxide
Tin
Tin Oxide
Tin Sulfide
Tin Selenide
Tin Telluride
Formula
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
VB2
VC
VN
VO2
W
WB2
WC
Version 1.1
Density
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
5.1
5.77
6.13
4.34
19.3
10.77
15.6
Z-Ratio
?
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
?
?
?
?
?
0.163
?
0.151
Acoustic
Impedance
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
54.17
58.48
Page 14 of 15
Material Name
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
Vanadium Boride
Vanadium Carbide
Vanadium Nitride
Vanadium Dioxide
Tungsten
Tungsten Boride
Tungsten Carbide
Formula
WO3
WS2
WSi2
Y
Y2O3
Yb
Yb2O3
Zn
Zn3Sb2
ZnF2
ZnO
ZnS
ZnSe
ZnTe
Zr
ZrB2
ZrC
ZrN
ZrO2
Version 1.1
Density
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
?
?
?
0.835
?
1.13
?
0.514
?
?
0.556
0.775
0.722
0.77
0.6
?
0.264
?
?
Acoustic
Impedance
10.57
7.81
17.18
15.88
11.39
12.23
11.47
14.72
33.45
Page 15 of 15
Material Name
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