The following 5400 LS operating procedures provide details of many aspects of how to operate a 5000 LS XPS system. PHI did not make very many of the 5400 LS (large sample) systems but the ones that are still in operation are real work horses.
On a side note, I found this procedure in our database and know that it is from 2008, but I do not know who wrote it. It is very detailed and well written but I can not take the credit. If I find out who wrote it I will update this post. Enjoy!
5400 LS System Operating Procedures
Daily System Turn ON
1) Turn on the computer.
2) Turn on the Model 147, in the rack above the x-ray cooler console.
3) Turn on the Card Rack Power. The button islocated to the left ofthe keyboard just under the countertop.
4) Run the 5000 LS system control program.
5) Turn on the image monitor and the camera. Turn on the lamp.
6) You are now prepared to do something. Seethe appropriate section for operation of a particular component.
Daily System Turn OFF
1) Turn off the ion gun.
a) Turn off the argon gas.
b) Turn down the beam voltage to zero. c) Turn down the emission to zero.
d) Turn off the ion gun.
e) Close the manual differential pumping butterfly valve, located just above the turbo behind the system.
f) Close valve V4 with the “Diff Pump Ion Gun” button on the AVC remote. If it doesn’t work, close V4 manually on the front of the AVC. Caution! – Be careful not to press the wrong button.
2) Turn off the x-ray source.
a) Turn down the power to zero.
b) Turn down the high voltage adjust knob to zero. Press the high voltage button to turn it off.
c) Turn off the 32-095 X-Ray Source Control power.
3) Turn off the UV source.
a) Shut the He gas leak valve mounted on the source. b) Close the pumping stage P1 valve.
c) Close valve V4 with the “Diff Pump Ion Gun” button on the AVC remote.
4) Turn off the image monitor and (optional) camera. Turn off the lamp.
5) Turn off the “Card Rack Power” if you won’t be using the system for a couple of days or more. The button is located to the left of the keyboard just under the counter top.
6) Turn off the Model 147 if you also turned off the Card Rack Power in the step above.
7) Turn off the computer if you also turned off the Model 147 in the step above and you don’t need it again soon.
Loading in samples
NOTE: Before you actually introduce the sample into the chamber, make sure that the X- ray source; ion gun and neutralizer filaments are all OFF. Make sure that the ion gun/UV source is not being pumped (V4 closed on AVC). If the Card Rack Power was off, turn it on and let it warm up for15 minutes before operation. Some of the motor controls don’t work well until they warm up.
CAUTION!: Any aberration in this procedure could easily result in damage to the stage, ribbon, and/or platen. The only way to fix it involves venting the vacuum chamber. BE CAREFUL and watch the platen movement at all times!
1. Back-fill the intro by pressing the “BACK FILL INTRO” button on the AVC remote box.
2. Load sample platen and press “PUMP INTRO” button on AVC remote. The mechanical pump will rough out intro chamber to 2 bars on the AVC remote box. Then, V3 will open automatically and the turbo will pump out the intro chamber. After 4 bars are present on the AVC remote box, the cold cathode gauge on the
20-180 Intro Pump Control will activate and indicate the vacuum in the intro chamber.
3. Continue to pump the intro chamber until you have at least less than 1 X 10-6Torr indicated on the 20-180 Intro Pump Control (Varian 860A cold cathode gauge). This takes at least 30 minutes. The longer you pump, the lower the pressure burst is when you finally load the sample platen.
4. In the AugerScan program, go to System, Stage Control. This is the stage dialog box. Press the “DOCK”button. The stage will go to the proper coordinates (see stage table for more information).
5. Press “INTRO SAMPLE” on the AVC remote box. The V1 valve will open automatically.
6. Turn the Intro Ribbon feed through CW until it docks with the stage platen.
CAUTION! Watch the platen movement carefully the entire time. You will feel a indent when it is in the right position. The front and back edges of the sample platen will be about ¼ inch beyond the edges of the stage. You can see this through the 4.5” windows. If it is not moving smoothly or is not going back far enough, retract the platen and make sure that you are in the “DOCK” position. The “LOAD” position will not work.If you push it in too far,past the indent, the platen may get stuck. You would then have to readjust the Z-axis slightly, using the adjust button the up/down arrows, until you can latch it long enough to pull it back out and try again.
7. Once the platen is in position, click on the “LOAD” button.This will increase the Z-axis up by 2mm(other parameters should stay the same. This allows the ribbon to be retracted without bringing the platen with it. CAUTION! Do not change any other settings in the position or the ribbon/stage could be damaged. If the ribbon does not retract, increase the Z axis slightly by selecting the “Adjust” button next to “Z Axis” and scrolling the up/down arrows slightly, until the ribbon withdraws. You may want to “Se tLoad Position” with the modified Z
8. Remove the intro ribbon by turning the Intro ribbon Feed CCW until it stops at the end and V1 closes automatically. IfV1 does not close automatically, you can switch the AVC to “Manual” mode and toggle the V1 valve shut – be very careful not to press the button next to it by accident or you will back-fill the chamber accidentally (bad news!).
Removing Samples
NOTE:Before you actually remove the sample from the chamber, make sure that the X- ray source; ion gun and neutralizer filaments are all OFF. Make sure that the ion gun/UV source is not being pumped (V4 closed on AVC). If V4 doesn’t close by pressing the “DIFF PUMP ION GUN” button on the AVC remote. If the Card Rack Power was off, turn it on and let it warm up for 15 minutes before operation. Some of the motor controls don’t work well until they warm up.
CAUTION!: Any aberration in this procedure could easily result in damage to the stage, ribbon, and/or platen. The only way to fix it is to vent the whole chamber and know what you’re doing. BE CAREFUL and watch the platen movement at all times!
1. If the intro is up-to-air: Press the“PUMP INTRO” button on AVC remote. The mechanical pump will rough out intro chamber to 2 bars on the AVC remote box. Then, V3 will open automatically and the turbo will pump out the intro chamber. After 4 bars are present on the AVC remote box, the cold cathode gauge on the 20-180 Intro Pump Control will activate and indicate the vacuum in the intro chamber.
2. Continue to pump the intro chamber until you have at least less than 1 X 10-6
Torr indicated on the 20-180 Intro Pump Control (Varian 860A cold cathode gauge). This takes at least 30 minutes. The longer you pump, the lower the pressure burst is when you finally load the sample platen.
3. In the AugerScan program, go to System, Stage Control. This is the stage dialog box. Press the “DOCK”button. The stage will go to the proper coordinates (see stage table for more information). You should be able to see that the platen will raise slightly upward just as the stage completes the movement to this position.
4. Press the “INTRO SAMPLE” button on the AVC remote box. The V1 valve will open automatically.
5. Turn the Intro Ribbon feedthrough CW until it docks with the stage platen.
CAUTION! Do not move more that necessary to make contact with the platen.
6. Remove the sample platen by turning the Intro ribbon Feed through CCW until it stops at the end and V1 closes automatically. Caution! Watch the platen movement carefully the entire time. If it is not latching to the platen or it is not moving smoothly, detach and then retract the platen and make sure that you are in the “DOCK” position. You may have to increase the Z by 2 mm in order to unlatch the ribbon.The “LOAD” position will not work. You may need to readjust some of the parameters for smoother loading/unloading of the platen.
Use the “Adjust” button activation along with the up/down arrows, next to each coordinate number, to make the small adjustments. Be very careful not to take too large of a step or the ribbon/stage may be damaged. See the manual for the 30-520 Large Sample Stage for more detailed information on alignment.
XPS Analysis Procedure
1) Position your sample in position.
2) Select the x-ray source(Standard or Mono).
a) Use the Standard Source – Mg for high counts.
b) Use the Monochromator Source (Al) for better FWHM.
c) The Standard Source – Al is typically not used on this system due to the presence of the monochromator.
3) For the Standard Source,lower the nose closer to the sample. a) Normally this will block half of the video view.
b) Keep in mind that the Mg side of the anode is closest to the computer (this knowledge will help you align the source to achieve maximum counts).
4) Turn on the x-ray source and set to full power.
5) Set the source type in AugerScan (Hardware Properties).
6) Set the analyzer aperture and check the corresponding aperture in AugerScan
(Hardware Properties).
7) Set up the analysis parameters ( survey sweeps, pass energy, etc.)
8) Go.
X-ray Source Operation
There are two x-ray sources. The standard source is the 04-548 Dual Anode (Mg/Al) large spot located between the two V1 solenoids. The monochromator source also has a dual anode, completely coated with Al.
1) Set the x-ray source switch.
a) Standard: Set to “STANDARD”. b) Monochromator: Set to “MONO”.
2) Turn on the 32-095 x-ray source control.
3) Filament energize. Press the appropriate button just to the right of the blue
“Out/Act.” button. The blue button should not be lit. a) Standard: Select Mg or Al.
b) Monochromator: Select 1 or 2.
4) Select the corresponding button for the “Parameter Display” on the right just to the left of the red “High Voltage” button.
5) High voltage turn-on
a) Make sure that the large “Raise Voltage” knob on the 22-040 DC Power Supply is turned all the way down(counterclockwise).
b) Press the red“High Voltage” button so that it is lit (blinking).
c) Turn up the voltage slowly with the large knob to 14.5 kV. Take about 20 seconds to do this.
d) Note: both sources are brought up to voltage at this time,but only one can have the filaments energized at a time.
6) Power increase.
a) With the “Parameter Adjust” buttons, increase the power to about 100 watts. This is a good warm-up setting. You will have to readjust the high voltage knob to bring the voltage back up to 14.5 kV. Let it there for about 10 minutes.
b) Increase the power to 300 watts. Again, increase the high voltage to 14.5 kV.
Ion Gun Operation = sputtering
The 04-300 Differentially Pumped 4kV Ion Gun is controlled by the 77-067 Ion Gun Control boards (4). The differential pumping capability allows the base vacuum in the chamber to equalize at a factor of ten better than without the differential pumping. Although this ion gun is spec’d at 4 kV, it can only be safely run at 3 kV (above at which it will likely arc). Note that if you do not click on the “Set” key each time that you change a setting, it will not actually be at that value. Also, note that the emission current is an indirect reading of the filament current.
1) Turn on the differential pumping (press the “DIFF PUMP IOIN GUN” button to open V4). Of course, the turbo behind the vacuum chamber must be on and at full speed (all LEDs lit) before you can or should do this.
2) Close the butterfly valve from the differential turbo to the UV source and open the butterfly valve from the differential turbo to the ion gun.
3) Open the “Ion Gun Control” dialog box under the System menu in AugerScan.
4) Set the “Emission” to 25 mA and the “Beam Voltage” to 0 V. The “Objective” setting should be approximately 80% – this value is set by imaging on the phosphor, where you can see the best focus point.
5) Click on the “ON” button. The emission current will automatically ramp slowly to 25 mA.
6) The pressure reading at the bottom of the ion gun control window should be under 1 mPa.
7) Open the argon bottle on the ion gun until you achieve about 8 mPa of pressure on the readout. Note that the pressure will typically drift up after warming up, so keep an eye on it and turn it down if necessary. Try to maintain about 10 mPa. Normal operation is at 10 mPa to 15 mPa.
8) When you want to turn on the ion gun, set the Beam Voltageto the desired value and click on the set key.
9) Note that there is no warning box in the main AugerScan program window letting you know that the ion gun is on, once you close this dialog box without turning off the ion gun. Take care to remember to turn it off when you aren’t using it, as well as closing the gas bottle.
Neutralizer Operation
The 04-090 Neutralizer is controlled by the72-030 Neutralizer Control board. The purpose of the neutralizer is to cancel the positive charging effects of the sample bombardment of x-ray photon. The neutralizer floods the sample surface with electrons to compensate for the electrons the photons eject.
1) Open the “Neutralizer Control” dialog box under the System menu in AugerScan.
2) The “Emission Control” may be set to any value from0 to 25 mA. Typical operation is in the 15 to 22 mA range. Don’t run it any higher than you need to in order to extend the filament life.
3) The “Electron Energy” may be set from0 to 100 %. This corresponds to a 0 to -170
Vdc bias applied to the extractor lens to accelerate the electrons toward the sample. Set this parameter to obtain the best performance.
4) Click the “On” button to turn it on, obviously.
5) Again, like the ion gun control, remember to turn it off when you are not using it since there is no indication that it ison in the main AugerScan program.
Analyzer Operation
The 10-360 Spherical Capacitor Energy Analyzer is controlled by the 80-360 Analyzer
Control boards (5).
1) There are four apertures to select from, providing various analysis areas.Consider the trade-off between signal strength and resolution when selecting the appropriate aperture.# 4 provides the best signal and # 1 provides the best FWHM. If you have size (area) restrictions, thatmay restrict the decision.
a) Aperture analysis area
i) Aperture 4 –4 x 10 mm slit
ii) Aperture 3 – 0.80 mm diameter iii)Aperture 2 – 0.40 mmdiameter iv)Aperture 1 – 0.15 mm diameter
b) Software Aperture setting (AugerScan – Hardware Properties – XPS)
i) Once you reset the aperture on the analyzer, you must select the corresponding aperture size in the Hardware Properties menu. The control uses different lens voltages for different apertures.
c) The aperture selection is on the knob on the neck of the analyzer. To see the setting, go behind the system in order to look at it.
2) Software Area setting (AugerScan – Hardware Properties – XPS)
a) Aperture 4 –select “Large” area
b) Apertures 1-3 – select “Small” area
3) Software Source setting (AugerScan–HardwareProperties–XPS)
a) You must specify whether you are usingthe Mg or Al x-ray anode, or the UV source. Otherwise the energies will be shifted dramatically.
UV Source Operation
The UVS 10/35 UV Source is controlled by the UVS 20-A UV Source Control.
1) Pump the intro chamber and wait until the cold cathode gauge (20-180 meter) reads in the 10-5Torr range or less.
2) Differentially pump the UV source P2 (port 2). Press “DIFF PUMP ION GUN” on the AVC remote, close the butterfly valvefromthe differential turbo to the ion gun, and open the butterfly valve fromthe differential turbo to the UV source.
3) Open the valve on the He bottle (1 turn CCW).
4) Open the small butterfly valve between the intro chamber and the UV source P1 port.
Rotate 90 degrees CCW to open.
5) At this point, the base pressure in the vacuum chamber should remain unaffected.
6) Turn on the power to the UVS 20A power supply & control, for the UV source. The meter should indicate 1500 V applied to the UV source anode.
7) With the leak valve on the UV source, open the valve until you read about 9*10-6
Torr on the cold cathode vacuum gauge. This is enough to ignite.The base pressure should remain in the low eights/high nines.
8) Press the “Start” button on the UV control. The “Current” knot should be in a middle position. If the UV source fired, the “Voltage” LED will go out and the “Current” LED will go on. The voltage indication on the meter will drop to approximately 400
9) The lamp (look inside the UV source hood) should glow pale yellow to white. This is also visible in the end of the capillary tube inside the chamber.
10)By switching the UV control meter switch to “Current” the discharge current can be controlled. The UV discharge will extinguish below about 20 mA.
11)The alignment of the capillary tube may be adjusted with the three turn knobs.
Venting the system (backfilling the vacuum chamber)
1) Connect a bottle of dry nitrogen to the N2input on the back of the vacuum chamber.
It must be regulated to 4 PSI maximum.
2) Remove the platen from the vacuum chamber. It can stay in the introduction chamber. The introduction chamber pumping must be left on for at least 10 minutes before actually venting the vacuum chamber,as the difference in pressure between the introduction chamber and the main chamber must not be too large.
3) Put the stage in the “Bakeout” position. Note that if you vent with nitrogen and can prevent water vapor from entering the system, then you may not have to bake..
4) Turn off all x-ray sources, ion guns, etceteras.
5) Turn off the Digital Ion Gage by first pressing the “I/T” button, then turning off the main power knob on the left.
6) Shut off the ion pump control by rotating the “Mode” knob to “Off”.
7) Wait for at least 10 minutes for the filaments to cool.
8) Press the “Backfill Chamber” button on the Automatic Valve Control.
9) Turn off the pumps
a) Turn off the differential pump turbo (behind the vacuum chamber) by pressing the right-most button on the control.
b) Turn off the intro pump turbo by toggling the “Stop” switch on the 20-180 Intro
Pump Control.
c) Turn off the intro rough pump by unplugging it from the 220 Vac power outlet behind the vacuum chamber.
Pumping the System after up-to-air
1) With the pumps still off,press the “ROUGH CHAMBER” button on the Automatic
Valve Control (AVC) front panel. This will prepare the system for pumping, so the AVC knows how to open the valves in the right sequence, when you turn on the pumps. It is crucial, that the “ROUGH CHAMBER” button is pressed before any pumps are turned on.
2) Start the differential turbo pump (by pressing the right-most button) on the front panel of the Balzers TCP121 turbo controller and plug in the intro rough pump (220 Vac outlet) at approximately the same time. Valves V1, V4, and V6 should open when you do this. The differential pump pumps through a small hole, which explains why it can pump at such a high pressure.
3) Turn on the Power toggle on the 20-180 Intro Pump Control but do not start it yet.
4) Observe the valve settings on the AVC remote. When V6 closes and V3 and V7 open, start the intro turbo pump by toggling the “Start” switch on the 20-180. This might take about 10 minutes. This is done automatically so that the intro rough pump alone can pump out the bulk of the air before the turbo pump is engaged in the pumping.
5) The LED bars on the AVC remote should light up to four bars in a half hour approximately. Once they do, the cold cathode gauge will start and the pressure will be indicated on the meter on the 20-180 Intro Pump Control.Note that it may take considerably longer for the four LEDs to light in actuality. You can also use the thermocouple gauge to get a reading of the pressure while it is pumping. This is a good indicator if everything is pumping down okay or not. If it is sticking at some point above 1 mTorr, then there is likely a leak.Check all recently sealed flanges.
6) Let it pump with just the turbo pumps for about 1 hour.
7) Once the 20-180 Intro Pump Control meter (cold cathode gauge) indicates in the 10^-5
Torr range, you can turn on the Digital Ion Gauge III (DIGIII) to check the pressure. Turn the main power knob on the DIGIII to“UHV” and press the “I/T 3” button. This will activate the ion gauge and will show a reading if the pressure is in the 10^-3 Torr range or less.
a) If it won’t start, do not press the button again or you may damage the filament if the pressure is above the10^-3 Torr range. In this case, get a reading from the thermocouple or cold cathode gauge to verify that the pressure is low enough.
b) If the pressure is low enough and the DIGIII won’t read a pressure, you may have an open filament. The symptom of the DIGIII that will indicate this is that the pressure reading will scroll from10^-3 to 10^-10Torr as it is auto ranging,then will beep and shut off. See service personnel to check ion gauge status.
8) Assuming that the pressure is in the 10^-4 or 10^-5 Torr range, now it is time to outgas the Titanium Sublimator Pump (TSP) filaments into the turbos. They will outgas considerably if the system has been up-to-air, so we want to do this while we are still pumping with the turbo pumps as opposed to the ion pumps (which would just shut down under the pressure bursts).
a) Shut off the DIGIII filament by pressing the “I/T 3” button again.The gauge will shut off and the readout will show “0.0 x10 -3”.
b) Starting with filament 2, going around until filament 1, run each at 40 amps initially for one minute. The actual amps will decrease from 40 as it heats up, but that is okay (it is more important to maintain the current at the normal operating point – in the next step). Using a timer with an alarm helps with this task. Do not walk away from the system while doing this since it is easy to forget about it for a few minutes (too long). Turn the current down between cycles and use either “Continuous” or “Cycle” turn on the filaments.
c) Starting with filament 2, going around until filament 1, run each at 50-55 amps for one minute. Adjust the filament current to maintain this setting. It will decrease as the filament heats otherwise. Once you finish with filament 1, leave it there since you will now use this filament for normal operation until it expires.
d) Turn on the DIGIII filament by pressing the “I/T 3” button again.The gage will turn on and the pressure should be in the 10^-4 or 10^-5 Torr range. If you wait for about 10, while the TSP cools down, the pressure should drop into the low
10^-5 Torr range. This is a good point to start the ion pumps.
9) Starting the ion pumps
a) The pressure must be in the 10^-5 Torr range before starting the ion pumps. Keep in mind that the ion pumps cannot be run continuously unless the pressure is in the 10^-6 Torr range or less, but they can be run for a little while in the high 10^-
6 or low 10^-5 Torr range to help them heat and outgas in preparation for continuous operation.
b) Note that “START” mode on the “Ion Pump Control” is not current protected, whereas “RUN” mode is. We will start the pumps in “START” mode since the load is heavy but it must not be left there continuously, without observation, or a thermal runaway condition could occur during this process and destroy the pumps and control.
c) Turn the “RANGE” knob on the Ion Pump Control to “10 kV” for observation of the applied voltage to the ion pumps. Full power is 5 kV, half way on the meter. Once it reached 5 kV, we will know that we have successfully started the ion pumps.
d) Turn the “MODE” knob on the Ion Pump Control to “START”. This immediately turns on the ion pumps. Watch the pressure on the DIGIII while watching the voltage indication on the Ion Pump Control. The pressure should drop into the 10^-6 Torr range.
e) Let it run for maybe 10-15 minutes while observing it. If the pressure starts to increase again, which it probably will, shut off the ion pumps when it gets to the 9
X 10^-6 Torr range. The ion pumps are heating and outgassing since there is much water vapor in the system still.Let the pumps cool for 15-20 minutes, cycle the TSP for a minute, and try again.
f) Once the pressure is maintained in the mid 10^-6 Torr range or less with the Ion Pump Control on, press the “ROUGH CHAMBER” button on the AVC. This will close the valves using for rough pumping the chamber. Now the system is in its normal pumping mode, and at least 12 hours of operation will be required to reduce the pressure adequately in preparation for a bakeout.
g) Set the “MODE” knob on the Ion Pump Control to “RUN”. Make sure that the pressure is being maintained no higher than the mid 10^-6 Torr range.
h) You will need to run the TSP periodically, for a minute at a time, to help pump the water vapor in the system. I would do it maybe 2-3 times in the first hour of pumping, then less often as time goes on. If you don’t, the water vapor will cause the pressure to increase slowly, until perhaps the ion pumps shut off.
i) You don’t need to babysit the system anymore as long as the pressure is below the
10^-6 Torr range and dropping. I usually run the TSP just before I leave and then again the first thing after being away for a few hours.
j) You should be able to just get it into the high 10^-8 Torr range, just after shutting off the TSP. It will most likely maintain in the low 10^-7 Torr range though, unless you pump on it for days and/or give it a 24 hour bake.
i) If you can’t get this low, then there is a leak. Check all flange seals on recently replaced flanges. Use methanol or isopropanol, looking for bursts of pressure on the DIGIII readout. Are the flange bolts tightened properly?
System Bakeout
1) Remove the sample platen from vacuum chamber:
a) See the procedure above for removing the platen from the vacuum chamber.
2) Next, set sample stage to Bakeout position.NOTE: It is CRITICAL that the stage is always put into the bake out position BEFORE the motors are removed or the stage alignment will be lost and the stage could be damaged.
3) Remove the motors from the stage; be careful to keep the motor drive wires
- The small spring-loaded metal tabs next to the feedthroughs (on the motor assemblies) must be pulled up to remove the motors. The trick is to push on the metal lock while holding it against the spring with the slotted screw. You’ll need twofingers to do this.
4) Exit Auger Scan and turn off the Card Rack Power and RBD147 Interface Unit. This will shut off power to the electronics so that you can safely disconnect the cables. Leave the Electronics Power button on so that the main power is still available for a couple of components that we still need.
5) Standard x-ray source preparation
Caution! While you are working on this source, always make sure that the positioning knobs are tight (do it by tightening two opposite nuts at a time). They tend to work loose easily and then the source moves around too much and may damage the source or bellows.
a) Make sure that the 32-095 X-Ray Source Control is OFF.
b) Remove the front panel of the curved x-ray shield in order to get access to the internal water lines. Remove the Teflon sheet that is curled around the inside of the shield.
c) Disconnect the high voltage cable.
d) On the very top, disconnect the “IN” water line. Now unscrew the quick disconnect connector from the end of the protruding “IN” water line (on the x-ray source). Either side of the adapter will do. The idea here is to let air into the line so that most of the water can drain out through the “OUT” water line via gravity. Looking at the Teflon tubing in the shields, you should see the water, then the water bubbles, flowing through and out ofthe source into the “OUT” line. Wait until the water drains out of the monochromator source as well. When it looks like you’ve gotten as much out as possible, reattach the quick disconnect connector to the “IN” line. Disconnect the other water line (OUT) so both water lines from the cooling unit are disconnected.
e) Connect the water lines to each other to avoid having one of the lines blow up in case the x-ray source control is turned on before the water lines are reconnected later.
f) Disconnect the high voltage wire from the anode by removing the small screw.
g) Disconnect the Teflon tubes (the two long see-through pipes) from the top of the anode (at the bottom of the tubes). Use opposing wrenches to avoid stressing the metal water lines.
h) Remove the second half of the curved x-ray source shield and set the whole assembly aside. Remember the orientation of this piece so that it will be easier to replace later.
i) Remove the round thick Teflon piece from the back end of the anode.
j) The compressed air makes the pneumatic valves work. To get the compressed air- hose available, turn off the AVC if the V4 and V1-valves are already closed. Otherwise shut off the differential pumping (close V4) and make sure V1 is closed first (do so manually on the front panel of the AVC if you must).
k) Use the compressed air and paper towels to blowout the remaining water from
the anode. Use enough pressure to blow droplets of water out and no more – don’t blast it with high pressure.
l) Wrap foil over the exposed water lines and also around the main ceramic.
6) Monochromator x-ray source prep
a) Disconnect the water lines.Apply opposing pressure on the opposite side of the block when pushing on the water line connectors to disconnect them. Failure to do so will likely strip part of the x alignment mechanism, causing excessive movement from now on.
b) Remove the X-ray source shield (three screws).
c) Remove the small screw fastening the green grounding wire to the water jacket (white Teflon block).
d) Remove the two Bristol spline head bolts fastening the water jacket, which is the big, white Teflon block. Remove the water jacket by pulling and twisting it until it slides off.
e) Carefully remove the three O-rings from the back end of the anode. Do not use a sharp instrument or they will be damaged. Use your fingers only.
f) Remove the high voltage cable from the source.
g) Use the compressed air and paper towels to blowout the remaining water from
the anode. Use enough pressure to blow droplets of water out and no more – don’t blast it with high pressure.
h) Close the shutter to help keep the crystals clean during the bakeout. Turn the shutter knob counterclockwise to do so. Move the knob counterclockwise to the limit to close the shutter.
7) Reattach the air hose to the back of the system, apply pressure, and turn the AVC control panel back on.
8) Microscope and camera removal
a) Unplug the camera video cable – it is the connector closest to the power cord on the camera. Unplug the power cord also.
b) There are three twist rings on the column of the microscope. The top one fastens the whole microscope/camera assembly to the lower section. The middle ring is the focus. The bottom ring locks the focus ring. Loosen the top ring only while holding the bottom two rings still. This will allow you to remove the unbakeable microscope and camera while leaving the bakeable lower section in place.The advantage is that you won’t have to refocus the microscope when you put it back on after the bakeout.
9) Remove UV source cover (three screws). It is fairly difficult to reach these screw heads with a standard screwdriver.It pays to get a long skinny screwdriver for this task.
10) Remove the analyzer filter box (attached to the underside of the hemispherical analyzer). This is fastened with two bolts under the hemispherical analyzer.
11)Remove the PSD electronics box (mounted just under the analyzer).
12)Remove all cables from the main system above the table top (the only exception is the
Digital Ion gauge cable.
a) Do not remove the DIG cable (it is bakeable).
b) Do not remove the white cables attached to the side of the vacuum console.
These are the bakeout thermostats that are necessary for the bakeout.
c) Remove the UV source cover (in the previous step) before removing the HV feedthrough box for the analyzer.It is difficult to get the feedthrough box out with the UV source cover in place.
13)Remove the vacuum console table tops (2 sections). First, slide the large electronics console tabletop (with the computer on top) 2 inches to the right in order to move it away from the actual heating elements a bit.
14)Wipe the system with isoproponal (to remove fingerprints).
15)Cover all windows and feedthrus with aluminum foil.
a) Heavy duty foil works much better than the standard stuff. Double it up to make sure that it’s doing an adequate job of evening the heat.
b) Wrap it around the back of the windows to hold it in place.
c) Don’t forget the small window on the monochromator, or the small windows for the lamp and the microscope.
16)The knots controlling the valve on the sputter gun should not be over tightened. Just turn them clockwise until they reach the limit, then back off slightly (~10 degrees).
17)Make sure that the two tabletop switches are in the up position or the bake out ovens will not turn on. You have to pull them up by hand so that they stick above the tabletop.
18)Place the bakeout blanket over the system.
a) Note that there is a cross-shaped slot that lines up with the intro chamber and an entire extra piece that snaps over the monochromator. The intro chamber along with the V1 valve must be outside the blanket since they are not bakeable.
b) Be careful moving the blankets around the UV source and the standard x-ray source. Both of these sources must be inside the blanket. You will need extra foil to block holes since the blanket is difficult to move completely around the intro chamber. Also, there is an extra rectangular blanket piece in the drawer that could be used to insulate the standard x-raysource from the intro solenoids. If you don’t use this, the standard source may not get hot enough.
c) The vacuum lines from the turbo in back of the system to the ion gun prevent you from seating the bottom of the blanket on the tabletop. Use foil to block this large hole. You can crimp it on the edge of the blanket to hold it in place.
d) Snap all buttons and seal any holes with aluminum foil.
19)Set the bake out time (24 hours is recommended for this system)
20)Press the Bake out power button. You should hear a click. Make sure that the ovens are heating before you leave.
a) If the heaters aren’t coming on, check the bakeout circuit breaker on the back of the console. Also, setpoint 4 on the DIGIII must be activated(set to 5 x 10^-6). Also recheck the tabletop switches to make sure that they are still pulled up.
21)Place a fan at low speed on top of the intro chamber, directed at the V1 valve solenoids (two large can-shaped solenoids above the V1 opening itself). These solenoids could be damaged if they overheat,so they need to be cooled. Note that this is why it is important to place that extra blanket piece between the standard x-ray source and the solenoids– the insulate is required to keep the fan from cooling the standard x-ray source during the bake.
After the Bakeout
CAUTION! When making the connections required in this procedure, triple-check all connections. It is a dangerous practice to proceed to turn on the power without checking beyond the initial connection, even for experienced operators. Never guess at a connection – always make a positive identification, or get advice first. The Card Rack Power and 32-095 X-Ray Source Control must be off throughout this entire procedure.
1) Do not remove the blanket until at least two hours after the ovens shut off, to avoid thermal shock to the vacuum chamber. Besides, it harder to remove when it is so hot.
2) If the system is still very warm when the blanket is removed (feel along the main flanges which bear the heat the longest) leave the foil on for a couple more hours until the system cools more.
3) Remove the foil from the system.
a) Be careful not to pull off the heat sink fins from the UPS source when removing the foil.
4) Put the round Teflon piece back on the standard source anode. Since it barely fits over the water lines ends and is very tight, take care not to scrape off bits of Teflon into the water line itself.
5) Install the half of the standard x-ray source shell with the Teflon water lines. Tighten the Teflon water lines on the anode using two9/16 inch wrenches. Be careful not to over tighten these – the seals are Teflon, not metal. Connect the high voltage wire to the anode with the small screw.
6) Install the Teflon water block on the monochromator source. a) Slip the three seals on first with your fingers.
b) If the seals are dry, wet them first with a small amount of distilled water so that the Teflon block slips on better. If you have Apiezon grease, use that instead.
c) Fasten the green grounding wire.
7) Connect the water coolant lines to both the standard x-ray source and the monochromator x-ray source. The coolant should flow to the monochromator first, then to the standard source, then back to the coolant chiller. CAUTION! It is extremely important that you do not leave one end of the water lines disconnected. The water line will blow up in a subsequent step and one or both sources may be damaged.
a) Check the water level in the 16-020 X-Ray Heat Exchanger/Deionizer. Add common distilled water from the local grocer to fill it adequately.
8) Connect the filament and high voltage cables to both the standard x-ray source and the monochromator x-ray source.
9) Turn on the 32-095 X-Ray Source Control so that the coolant chiller will turn on and start pumping water through the system.
10)Carefully observe the water line connections on the standard source anode and on both sources in general. There must be no leaks. If there is even a partial drop anywhere on the connector (look especially on the shaft where it contacts the nut), tighten the nut, dry the water, and check it again in 15 more minutes.
11)Once it has satisfactorily passed the leak test, you can reassemble both sources completely.
12)Attach the UPS shield in place over the UPS source (naturally!).
a) This is where the super-long skinny screwdriver really comes in handy. Good luck getting this part on without it. Maybe you can do it.
b) Connect the high voltage and fan power cables to this shield.
13)To reattach the analyzer high voltage feedthrough box (under the hemispherical part):
a) The feedthrough box slides back into the connector from the side towards the intro chamber.There are two large bolts that restrain the movement that the box must slide past.
b) CAUTION! You must hold the differential turbo high vacuum flex line that runs to the adjacent UPS source out of the way. It rests against the side of the feedthrough box with considerable pressure. If you allow it to slide along the feedthrough box while you slide it in, it will eventually wear a hole in it and spring a leak – that will drive you mad some time in the future!
14)Connect the ion gun and neutralizer cables.
15)Install the stage motors
Caution! The stage must be cooled for at least 8 hours after the bakeout. Operation while the stage is warm can severely damage it.
a) Make sure that you put the right one in the right place. Any mixup will likely damage the stage and make everybody cry.
b) Note any misalignment in the motor shaft position with the shaft position on the corresponding stage port. A slight variation is normal and the motor will still engage easily. A rotational difference of 180 degrees indicates that there was some misalignment, so be cautious when using the stage, especially when loading/unloading samples. Some adjustment may be necessary. See the 30-520 Stage manual for detailed information.
c) Note that it is also very important that the computer still indicates the “Bakeout” position (X=0, Y=-8, Z=0, Tilt=45, Rotate=-185). If it isn’t, don’t put the motors on the stage until you turn on the electronics later and reset the stage position electronically to “Bakeout”. After that then, install the motors.
16)Position Sensitive Detector (PSD) electronics
a) Mount the Position Sensitive Detector (PSD) electronics boxin place under the hemispherical analyzer.It is important that this unit is grounded well, so use at least three bolts with the perforated lock washers and fasten the grounding strap (from the intro chamber valve bolt).
b) Connect the Preamp A &B connectors to the analyzer.
17)Connect the PSD high voltage cables.Note the connector label on the very end of the cable where it attaches to the analyzer, not next to the filter box in each cable. Check these connections carefully because the PSD is not something nice to fry by connecting the voltage in reverse.
18)Put the camera/microscope back in place.Be careful and hold the focus ring in place while only tightening down the top lock ring. Connect the video output to the monitor “Video”.
19)Connect all other cables not yet connected.
a) Analyzer Forward Lens (FWD LENS) cable – on the “neck” ofthe analyzer. b) Analyzer Control Lens (CTL LENS) cable – on the “neck” ofthe analyzer. c) Stage “Target” to the electrometer input.
d) Stage “Ion” should have a shorting cap on it.
Outgassing and High Voltage Conditioning Procedures
Note that the ion gun may be outgassed simultaneously with one of the x-ray sources. The normal routine is to outgas the filaments first (x-ray source: 1 hour, ion gun: 2-3 hours), then do the high voltage conditioning with the filaments off (x-ray source: 4-5 hours, ion gun: 4-5 hours), then start to operate them, first at low power, then increasing it slowly to full power (over a couple of hours). If you do not follow through with these
procedures fully, the sources will likely arc, perhaps damaging themand their controllers. Arcs will feed back and scramble the digital logic in other components, like the DIGIII
(which will beep until you reset it). Also, once an arc occurs,you will have to back off on the high voltage by about 20% and then increment it upward at half the previous rate. Arcs tend to occur again in the same spot once initiated. It is best to not hurry the initial outgassing since the crime doesn’t pay. If service work was done on any particular source, you will have to take extra care whileoutgassing it since it will take longer and is more likely to arc.
1) Turn on the computer, start the 5000LS program, turn on the Model 147, and turn on the Card Rack Power.
2) X-Ray Sources. Both x-ray sources outgas identically. The filaments and final power conditioning must be done separatelysince both sets (of filaments) cannot be run at the same time. The X-Ray Source Switch must be set to the source that you want to outgas. When you outgas the high voltage, it is applied to both sources simultaneously. Start with the Standard Source. Turn the X-Ray Source Switch to ‘Standard’. When you finish this procedure, switch the “X-Ray Source” switch the “Mono” and run through this procedure again. a) Filament Outgassing
i) Both filaments should be outgassedsimultaneously (Mg and Al for the standard source, Mono1 and Mono2 for the monochromator.
ii) Set the “Int/Ext” mode switch on the 32-095 to “Int”, for internal (manual)
iii)Press the blue “Out/Act” button to energize the filaments. Select “Both” under the “Filament Energize” section to turn on both filaments. The small red LED should lightnextto the button. Initially, the current will be 0.0 amps in each, as indicated on the display.
iv)The key indicator for how much the filaments are outgassing is the pressure reading on the DIGIII when you ramp the filament up. Outgassing typically occurs mostly beyond 3.0 amps, and will be noted by some pressure bursting on the DIGIII readout. Wait until the pressure lowers and stabilizes before increasing the current further.
v) The goal is to ramp each filament current to a target of 4.5 amps. Ramp the current for each filament in 1.0 amp increments to 3.0 amps, then in 0.5 amp increments to 4.5 amps, over the course of approximately 1 hour. Then hold it at 4.5 amps for about 25 minutes.
vi)Ramp each filament to 0.0 amps to turn themoff. Press the “Out/Act” button again to turnit off.
b) High Voltage Conditioning
i) Turn down the “Raise Voltage” dial on the 22-040 DC PowerSupply
(completely counterclockwise – CCW).
ii) Press the red “High Voltage” button on the 32-095 X-Ray Source Control. It will blink once it is on. It blinks when the voltage is under 8 kV, and it steady when over that.This is because thissource should never be operated below that voltage, since the filaments would then be overdriven to maintain power with low voltage. You can operate the source between 11 kV and 14.5 kV, but you should always use 14.5 kV under normal conditions (once it is outgassed).
iii)If you press the “HV” button to the rightof the red “High Voltage” button, the meter will indicate the voltage.
iv)Slowly turn up the voltage to 10 kV using the “Raise Voltage” knob. You can read the voltage either on the analog meter on the 22-040or on the digital meter on the 32-095. You can do this in about 15 seconds since this source rarely will arc below 10 kV. It is stillpreferable to go slow since the severity of an arc will be reducedif the power isn’t being driven well above the critical point.
v) The goal is to slowly, over the course of 4-5 hours, bring the voltage up to 16 kV. We go to 16 kV since the HV should be outgassed slightly above the normal operating point for best performance. The higher you are in voltage, the smaller the increment you should increase it by.
(1)Between 10 kV and 13 kV, raise the voltage 500 V every 15 minutes. (2)Between 13 kV and 16 kV, raise the voltage 300 V every 15 minutes.
vi)Ifan arc occurs, the 22-040 will shut itselfdown. Turn down the “Raise Voltage” knob and press the “Reset” button to restart it. Increase the voltage to about 2 kVbelow where it arced, and proceed with the HV conditioning. If it arcs again,do the same, except increment the voltage every30 minutes instead of 15.
c) Initial turn-on (normal power mode)
i) Select the filament on the 32-095 under “Parameter Display/Control”. Note that this filament will also have to be activated under “Filament Energize”.
ii) Turn on the High Voltage and set to about 13 kV. There will be a pressure burst the first time power is applied tothe anode, which is why we start at 13 kV instead of full power at 14.5 kV.
iii)Using the “Parameter Adjust” arrowson the 32-095, increase the power to 10 watts. You should see a pressure burst on the DIGIII readout. This indicated that everything is normal.
(1)If no pressure burst is noted, look inthe chamber for the filament light in the end of the x-ray source (standard source only). If there is no light, did you energize that filament in the“Filament Energize”section of the 32-095?
iv)Once the pressure drops downnearly to where it was before you turned on the source, increase the power to about 50 watts. Again, wait until the pressure drops down to the nominal level. Remember to compensate the high voltage adjustment as you increase the power since it will drop under the applied load. You may increase the voltage if arcing has not been a problem, otherwise let it condition longer.
v) Eventually, after an hour or two, you may increase the power and voltage to 300 watts and 14.5 kV, respectively.
3) Ion Source
a) Filament outgassing
Note that if you do not click on the “Set” key each time that you change a setting, it will not actually be at that value. If you did not do this, don’t suddenly click on it when you’ve been ramping it for some timewith no affect. Bring the current back down first to make sure that you don’t overdrive the filament before it’s outgassed. Also, note that the emission current is an indirect reading of the filament current.
i) Turn on the differential pumping (press the “DIFF PUMP” button to open V4). Of course, the turbo behind the vacuumchamber must be on and at full speed (all LEDs lit) before you can or should dothis.
ii) In the “Ion Pump Control” in AugerScan, set the “Emission” and “Beam
Voltage” values to zero. The raster does not matter for outgassing. iii)Click on the “ON” button.
iv)What we want to do now is slowly rampthe emission current from0 mA to 25 mA (full power) while we wait for thepressure to drop before incrementing upward. The pressure readout at thebottomof the window should be kept below 10 mPa at all times.Increase the emission current, hitting the “Set” button each time that you change it so that it takes affect. Increase it until you get a reading of about 7 mPa on the pressure. You will note the outgassing on the DIGIII readout also by pressure bursts when you increase the current.
v) Hold this setting for awhile (~25 minutes), since the ionization chamber and ion gun in general will start to heat up,and the pressure will actually increase over this time even though the emissioncurrent is the same. The tendency is that the pressure may raise above 10 mPa, so you will need todecrease the emission current until thepressure drops down further.
vi)Continue incrementing the emission currentuntil you reach 25 mA. Once there, leave it on until the pressure drops below 1 mPa. This may take a couple of hours.
vii)Set the emission current to zero inpreparation for the HV conditioning. b) High Voltage Conditioning
i) With the emission current off, set the BeamVoltage to 500 volts.
ii) The goal is to bring the voltage up to 4000 V. Normal operating voltage for this gun (04-300) is 3000 V. The ion gun is more likely to arc, typically, than the x-ray sources, so go slowly.
(1)Between 500V and 2 kV, raise the voltage 300 V every 20 minutes. (2)Between 2 kV and 3 kV, raise the voltage 200 V every 20 minutes. (3)Between 3 kV and 4 kV, raise the voltage 100 V every 15 minutes.
iii)If an arc occurs, you will usually heara “snap” in the vicinity of the 04-300 ion gun. You may have to reset the Card Rack Power toreinitialize the control in case the logic was scrambled. Increase the voltage to about 1 kV below where it arced, and proceed with the HV conditioning. If it arcs again, do the same, except increment the voltage at halfthe rate (twice the time between steps).
c) Initial turn-on (normal mode)
i) Set up a test sample, or just a part of the platen, to run the ion gun on. You could use phosphor to see the beam, and can also read the current on the electrometer (Target current).
ii) Turn on the differential pumping.
iii)Set the emission current to 25 mA andthe beamvoltage to zero. Set the
Objective to about 80%, or whatever you normally have it set to for focus. iv)Open the argon bottle on the ion gun until you achieve about 8 mPa of
pressure on the readout. Note that the pressure will typically drift up after warming up, so keep an eye on it and turn it down if necessary. Try to maintain about 10 mPa. Normal operation is at 10 mPa to 15 mPa.
v) Set the beam voltage to 1000 V. Look for a beam on the phospor or ion current (positive) at the target with the electrometer.
vi)Increase the voltage to 2000 V.Run it at this beam voltage for about 20 minutes before you increase it. Then you may run it at 3 kV unless you had problems with arcing. In that case, increase the voltage in smaller steps and allow more time for conditioning the source.
4) Position Sensitive Detector (PSD)
The objective here is to slowly increase the voltage on the PSD plates to provide conditioning.The typical full operating voltageis in the 2000 to 2400 V range. We start the conditioning at 1500 V.
a) Once the x-ray sources have been outgassed, and the sample platen has been loaded into the system, the PSD (multiplier plates) must be conditioned before full voltage can be applied.
b) Put a sample into position and turn on the standard x-ray source to half power. c) Select the “Multiplier Properties” menu in AugerScan, then select “XPS”
d) Type “1500” in the Multiplier “V” box.
e) Set up a XPS survey from 1000 eV to 0 eV an set the sweeps to 10.
f) Start the survey. You should see zero for the counts (no data). There may be an occasional small noise spike, but there shouldn’t be many.
g) Upon completion, increase the voltage to1600 V. Restart the same survey.
h) Continue to do this cycle until you reach 2000 V.At this point, increase by only
50 V per cycle. You will likely see data once you exceed 1900 V. Ifyou see significant noise spiking, take more sweepsat that voltage rather than increasing it. You may even want to decrease the voltage to take more sweeps if the noise spikes are excessive, and MUCH higher than the background counts.
i) Stop after you have taken the surveys with a PSD voltage of 2200V. At this point, the PSD plates are conditioned.
High Vacuum Pumping Operation
The high vacuumpumping systems on this instrument are comprised of two turbo/rough pumps, an ion pump, and the titanium sublimator pump.
1) Introduction chamber turbo/rough pump
a) This pumps directly on the introduction chamber. The turbo is mounted on the side of the intro chamber and therough pump is on the floor below.
b) The rough pump has an oil sorption filter toprevent the backflow of oil fromthe pump to the turbo. An oil filter is also installed onthe exit port to reduce the expulsion ofoil vapor into the lab.
c) The turbo and rough pumps are turned on/off separately. The turbo is controlled via the 20-180 “Intro Pump Control”, and the rough pump is turned on/off by plugging or unplugging the power cord(located behind the console).
d) The AVC controls the pumping sequence through valves V3, V6, and V7.
Typically, when the introor main chamber is up-to-air, the rough pump will evacuate it first by the AVC closing V7 and V3 and opening V6. Once two LEDs are lit on the AVC remote, the turbo gets into the pumping action by the AVC closing V6 and opening V7 and V3.
e) When you want to shut down these pumps, you must first close V3, V6, and V1. i) It is usually a good idea to “Backfill Intro” first,sothatthere is no risk of oil
being sucked into the intro chamber ifthe intro chamber is opened to the turbo when it is off.
ii) Toggle the “Stop” switch on the 20-180 control to halt theturbo. Unplug the rough pump to halt it. Note that the turbo blades will still be spinning at high speed.It is a good idea to vent the intro turbo by “cracking” the high vacuum line between the rough pump and the intro. Just undo one of the wingnuts on the flange for the flex line directly under the turbo, letting the air leak slowly in to slow the turbo blades and bring the intro pump systemup to air. This should be done to prevent the possibilityof oil being sucked fromthe rough pump into the turbo.
2) Differential pump
a) This pumps the differential ports on theion gun and UV source. It is located directly behind the vacuum console.
b) The turbo/rough pump combination is controlled by the Balzers TCP121 controller.Press the rightmostbutton to start or stop the pump.
c) The AVC controls the differential pumping valve V4. The turbo must be up to full speed before any attempt should be made to open V4.
d) Two butterfly valves located just above the turbo and V4 provide control over the differential pumping function – whether to differentiallypump the ion gun or the UV source.
i) This prevents gases used in the ion gun (argon) fromentering the UV source, and vice versa (He for the UV source fromentering the ion gun).
ii) The ion gun and UV source should never be operated together, but you can leave both butterfly valves open during normal operation if you’re not using the ion gun or UV source.
iii)When you are using the ion gun, close the butterfly valve to the UV source. iv)When you are using the UV source, closethe butterfly valve to the ion gun.
Replacing the Argon or Helium bottles
1) Argon bottle
a) Time to replace/refill?
i) It is difficult to tell when the argon isrunning out since there is no pressure gage on the bottle. The biggest symptomis that the sputter rates will drop off fromthe normal rates. One way to tell for sure, though a pain, is to remove the bottle (with the leak valve closed)and check for pressure in the bottle by sealing some foil over the opening with your hand and opening the bottle momentarily. If it sucks your hand into the bottle, thenit was indeed empty. There should be considerable pressure left in it at this point to make it worth re-installing. These bottles can be refilled for part of the cost of complete replacement.
ii) Since the bottle is quite small, it may need replacing/refilling every couple of years, depending on how much the ion gun is used. Systems with Auger capability that do a lot ofdepth profiling are more likely to need to replacethe bottle frequently.
iii)Some operators elect to puta high vacuumflex line and a larger bottle on the systemso there isn’t a concern about running out. Note that the bottle pressure should not exceed 275 PSI.
Alignment and Calibration Procedures
1) Camera and Sample Alignment.
2) XPS Calibration
3) Ion Gun Alignment
Regular Maintenance
1) Cleaning the air filters under the console.
2) X-Ray sources
a) Standard Source
b) Monochromator source