Ar Sputtering
1. Flushing Ar gas line
(1) When TMP-1 (V150) is running , V1 close, V2 close.
(2) If TMP-4 (V50) is not running, run it.
(3) Close V12. V8 , V10 , V13 should be close.
(4) Slowly open the V14, pull the Ar gas line with TMP4. Ensure that the reading of TC2 does not exceed 2V.
(5) When the reading of TC2 is close to 7.3V, close V14.
(6) Open V15 (value of Ar gas cylinder), set Ar gas line to 1 atm, close V14.
(7) Open V14 carefully while read TC2. In this case, the reading of TC2 should never be less than 2V. When TC2 is close to 7.3V, close V14.
(8) repeat (6) and (7) about 3 times.
(9) when TMP-1 is running and TC2 is 7.3V, open V2. When the vacuum level of TC2 deteriorates and becomes 7.3V again, open V1.
2. Ar sputtering
(1) Open V15. When Ar gas line is 2 atm, close V15.
(2) Cool the Ar gas line in LN2 of a dewar bottle (fix it with an Aluminum plate).
(3) Ion gun holder electrode (H) to GND, sample electrode (S) to tester (20 mA range).
(4) Place the sample holder on the annealing base and place the annealing base in front of the annealing base (it is advisable to tilt it slightly in the direction in which the beam will be easily hit).
(5) Close GV2.
(6) Open VLV1 gradually while looking at the vacuum level of the Chamber. Set it to 5×10-5 Torr (6.43V).
(7) Turn on the power of Ion gun controller.
(8) Turn the Filament knob to the right and inject IF = 25 mA.
(9) The acceleration voltage is set to 1kV.
(10) Turn on the switch Remote (this starts sputtering).
(11) Adjust the FOCUS, position, and Angle of the sample to maximize the sample current. It usually has a current 2 mA.
(12) Turn off Remote, Fila turn to 0 mA.
(13) Close VLV1, it turns back about 2.8 until see a black marker.
(14) The vacuum level should be better to 1×10-9 Torr (2V) in 1-2 min. Open GV2.
(15) In another 10 min, the vacuum level should improve to less than 5×10-10 Torr.
Note: The order (1) and (2) must never be reversed. Ar liquefies at LN2 temp, so when LN2 is gone, the pressure in the gas line increases and is very dangerous.
Annealing
(1) Change cable from “Supttering” to “Annealing” (attached Figure).
(2) Open GV2 (connected TSP)
(3) Control Filment HV
An invertal time to open the “Power”, “Set”, “OUTPUT”
(4) Control DC power supply
(5) Take note (5min/15 min): IF, VF, IE, Pp;
(6) Close
(7) Open TSP(B) 25 waiting ~2min
(8) it is not necassrtay to plug out cable if you don’t perform the STM test.
(2) Make sure that the Imax knob on the control panel is left (Imax = 0) and the switch is Imax.
Also, confirm that the terminal of C.C. OUTPUT on control panel 1 is connected to a DC power supply (it should be normally connected).
(2) Adjust dI/dV knob on the control panel 1 (this is the speed at which the current is dropped at the end of the annealing). It is usually set to 0.5×10-2 A/s. The actual speed of the current drop is different from the display of control panel 1.
(3) Place the sample holder on the annealing base and check that the current transfer terminal of the annealing base is in contact with the sample holder by the tester. At this point, the resistance value is from Pt(111) (10-5 Ω・cm).
(4) Connnect the DC power supply to the current introduction terminal of the annealing base with a cable. Verify that no current draw pin is connected to the sputtering pin.
(5) Fix the radiation thermometer with a stand where the center of the sample is visible.
(6) Connect the radiation thermometer and the control panel 1 with a cable. Turn on the TM switch.
TM OUTPUT D-OUT
TM INPUT A-OUT
(7) Gradually turn the knob of Imax to the right while looking at the value of the radiation thermometer, and raise it up to the target Temp. For the sample with a large resistivity. it is recommended to use a power supply with a higher maximum voltage and raise the temp slightly, then turn off the power supply and switch to the original power supply.
(8) The temp may vary from 10 to 20 in the progress of annealing. Turn the Imax knob to adjust the temp appropariately.
(9) Switch control panel 1 from Imax to START, after annealing.
(10) Turn off the direct current, when the current is 0.
(11) Turn the Imax Knob to the left. Switch back to Imax.
Deposition Methods
(1) Make sure that the vacuum level (UHV2 reading) is good (usually around 1×10-10 Torr).
(2) The sample holder attached the tip of the transfer rod and the surface is directed upward. Place the thinnest part of the transfer rod directly above the deposited part so that the deposited part is fully visible from the Membrane Pressure Gauge.
(3) Wire as follows
- Connect the membrane pressure gauge and the membrane pressure controller.
- Connect the output of the high voltage power supply to the crucible through the tester (200 mA range) (Ag-Ta crucible, Au-W crucible).
- Connect the DC power supply (KIKUSUI PAD35-20L) to the fila and drop one side to GND.
(4) Turn on the power of the MPG controller and set up MPG parameter (density, Zvalue) depending on the vapor deposition source material. The distance between the vapor deposiiton and MPG is twice the root of the vapor deposition and the sample distance. Set up density value as a half of real value.
(5) Make sure the toggle switch on control panel 1 is Imax and the Imax knob is full to the left.
(6) Turn on KIKUSUI PAD35-20L power supply.
(7) Looking at the value of UHV2 and PAD35-20L, turn the Imax knob to the right gradually and draw 5A current, at this time, the voltage is about 5V.
(8) Until the UHV2 is good enough (usually around 3×10-10 Torr), degas continues. it usually lasts about 5 min.
(9) Make sure the HV power supply porality is positive. Set the current limit (normally 30 mA is fine).
(10) Reading UHV2, MPG controller, and tester, the deposition speed is got by applying the HV gradually. The evaporation rate of 0.1A/sec can be got by regulate I and V.
(11) Once the melting pot has warmed uniformly and the evaporation rate has stabilized, the sample is directed downward and brought directly above the evaporator. Once teh required amount has been deposited, the sample is quickly moved and pointed upward.
(12) Set the high voltage power supply to 0V. Turn off the power supply.
(13) Turn the Imax knob of the Control panel 1 to the left, Imax =0.
(14) Turn off the power (KIKUSUI PAD35-20L).
(15) Turn off the Membrane Pressure Meter.
Low Energy Electron Diffraction
1. Ensuring preparation pressure (Pp) < 2×10-9 Torr.
2. Insert sample holder in Manipulator; the position of Manipulator is neighbour to (10, 15, 15).
3. Assembly line: ULVAC LEED-AES Controller terminal
LEED mode selected; Manipulator V2–Control Panel 1 LEED V2; Manipulatro C—ULVAC LEED/AES controller LEED C; monitor Is with tester (~20 uA).
4. U2 off
5. close light
6. lip open
4. Controller power is On
5. Filaments trun on to right, 6.9. IE should not exceed 2 mA.
6. Turn on “Lower”, Acceleration Voltage of electron gun is 90-115 eV.
7. Turn on “Screen” to kV.
8. Emission turn, It change to best, stop.
9. When It change to lagest, regulate Emission, Accelaration Voltage and Contrast, focus, (x, y, z).
10. When you can see LEED patterns and sports is clearly, regulate Emission, Accelaration Voltage and Contrast, focus, (x, y, z).
close power
open GV2
TSP open-close
Note:
1. At RT, the filament can be exposed to atomspheric pressure repeatedly without impairing its emission characteristic.
QING SHI 