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2015/5/21 1 Y. Harada
2015/5/21
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Y. Harada
Outline
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1. Starting up the XPS
2. Sample Setting
3. Intro Sample
4. X-ray Source Setting
5. Sample Positioning
6. Z Alignment
7. Measurement
1. Survey Survey scan
2. Multiplex Narrow scan
3. Profile Depth profile
8. X-ray Shutdown Procedure
9. Removing Samples
10. Daily Shutdown Procedure
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Starting up the XPS
1. Turn on the ISA Busbridge.
2. Press on the switch on the Picoammeter.
3. Turn on the PC.
4. Press on the power switch on the Card Rack Power. (Green indicate light will
turn light on.)
5. Double click the PC-ACCESS icon.
ISA Busbridge CARD Rack Power Picoammeter
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Sample Setting
1. Place samples on the sample holder.
Maximum sample size: 10 mm × 10 mm × 3 mm.
2. Hold samples on the sample holder with metal mask, spring clips, screws,
conductive tape and conducting pastes.
Metal mask Spring clips screws Conductive tape
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Intro Sample 1
1. Open the N2 gas valve.
2. Press on the “Backfill Intro switch” on the “Auto Valve Control” console.
3. It is safe to open the introduction chamber cap “Intro cap”, if the Intro chamber
pressure reaches 760 Torr.
“Auto Valve Control”
console
Intro cap
Intro chamber
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Intro Sample 2
1. Slide the sample holder onto the Intro arm of the Introduction rod.
2. Replace the intro cap.
3. Press on the “Pump Intro” switch on the “Auto Valve Control” console.
Sample holder
Intro arm
“Auto Valve Control”
console
“Pump Intro” switch
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Intro Sample 3
1. After 15 minutes, check the “High VAC” light is lit.
2. Press the “Intro Sample” switch on the “Auto Valve Control” console.
3. V1 valve will open, then the V1 lamp turns on green.
4. Slide the Introduction rod assembly to its fully extended position.
stage
rod holder
Intro arm
V1 lamp
“Intro Sample”
switch
“Auto Valve Control”
console
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Intro Sample 4
1. Check the red marking on the X, Y micrometer.
2. Moving up the stage using Z axis micrometer.
3. Place the sample holder on the stage.
4. Slide the Introduction rod assembly to check the position the sample holder on
the stage.
5. Retract the Introduction rod assembly to its fully intended position. V1 valve
will automatically close.
X Y
Z
Tilt
stage
Rod
Holder
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X-ray Setting 1 1. Power on the “X-ray Source Control” X-ray source controller panel.
2. If not, then toggle switch from “EXT” to “INT” position, make sure the toggle
switch is in the “INT” position.
3. Check the “High Voltage Control” knob is at zero (off) position on the “X-ray
supply” controller.
4. Power on the X-ray power supply “X-ray Supply” panel.
5. Select the X-ray source. ( 1 : Mg or Al conventional, 2: monochromated Al)
“X-ray Source Control”
X-ray source controller
panel
“X-ray Supply”
X-ray Power Supply
panel
“INT/EXT”
toggle switch
“High Voltage
Control” Knob
X-ray source toggle switch
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X-ray Setting 2 1. Push on the “HV” and “High Voltage” switches on the “X-ray Source
Control” panel.
2. Turn on the “High Voltage” switch on the “X-ray Supply”.
3. Using the “High Voltage Control” knob set it to 14 kV on the “X-ray Supply”.
“X-ray Source Control” panel
HV
High Voltage
High Voltage
“X-ray Supply” panel
High Voltage
Control knob
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X-ray Setting 3 1. Select the X-ray source. If you use Mg X-ray, press on the two Mg button.
2. “Parameter Display Control” changes from “kV” to “watts”.
3. Press the “Parameter adjust” button. Set the X-ray power to the 400W(Mg) or
200W(Al) each 10W per cycles.
4. Hold for the 15 minutes (X-ray aging process)
5. Toggle the “INT/EXT” switch from “INT” to “EXT” on the “X-ray Source
Control”.
Parameter
Display/Control
Al source
Mg source
Parameter Adjust
“INT/EXT”
toggle switch
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Sample Positioning
1. Turn on the CRT.
2. Turn on the FOSTEC（lamp）. Adjust the brightness.
3. Using the knobs on the sample stage, position the desired analysis area in the
center of the field of view.
4. Adjust the stage so that analysis area is in focus.
5. With the desired analysis area in focus and located at the center of the field of
view.
6. Turn off the FOSTEC.
switch
Adjust dial
Zoom
Monitor CCD camera
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Z Alignment 1
1. Click the “Set up X-ray” from the “Hardware Control” on the pull-down menu
of the PC-ACCESS software.
2. Select the X-ray source .
1. Mg standard Anode 2 Current Mg Standard
2. Al standard Anode 1 Current Al Standard
3. Al monochro 2 mm or 7 mm Current 2 mm or 7 mm
3. Click the “EXIT” tab.
Monochromated Al 200W 2mm type source
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Z Alignment 2
1. Select the “Set up align” function from the “Aquire Set up” pull-down menu.
2. Set C1(1s electron of carbon) or O1 (that of oxygen) the “Element Name” and
25 for the Range(eV).
3. Click the “Refresh Aquire” tab.
4. The X-ray will turn on and the C1s peak will be displayed on the CRT. (If the
peak does not display, turn on the neutralizer.)
5. Calibrate the Z position using Z axis knob. (maximum count)
6. After doing the Z alignment, click the “Abort Acq.” tab and then “exit” tab.
Z alignment
Using C1s peak
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Preparation for the Measurement
1. Click the “Dir” function from the “Sample Setup” pull-down menu.
2. Select your data folder and click the “exit” tab.
3. Click on “Sample Setup” function on the “Sample Setup” pull-down menu.
4. Input the filename to the “Sample file prefix” and input any measurement
number in the “Start file number”.
5. If you want to write any comments, click the “Edit Comment” tab
6. Write the comments in the “comment” and click the “exit” to exit the “Edit
Comment” menu.
7. Click the “exit” tab to exit the “Sample Setup” menu.
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Measurement （Survey scan） 1. Select the “Setup Survey” from the “Aquire Setup” pull-down menu.
2. Enter the measurement conditions, lower energy (“lower limit”), energy range
(“Range”), and data collection time (“Acquisition time”).
3. Select the “SURV”（Survey mode）.
4. Select the X-ray source for example, monochromated Al and Mg standard.
5. Click the “Acquire” tab to start the measurement.
For example,
Monochromated Al X-ray
0 – 1200eV 10 min
Lower limit : 0 eV, Range: 1200 eV
Acquisition time: 10 min
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Measurement（Multiplex）1. Region Prameter.
1. Select the “Setup Multi” function from the “Aquire Setup” pull-down menu.
2. Enter the element name, you would like to analyze. (element symbol and
number, for example, carbon 1s electron is C1)
3. Now set the lower limit, range, resolution (HRES or UTIL) and sweeps.
4. Click the “Next Menu” tab.
For example
Measurement of the C1s, Cl2p,
Zn2p3, O1s peaks.
HRES: High resolution mode
UTIL : Utility mode
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Measurement（Multiplex）2.
1. Enter the desired data collection time in the “Acquition time (min)”.
2. Select the X-ray source.
3. Click on the “Acquire” tab to start the measurement.
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measurement（Profile）1 Diff. Pump
1. Turn on the differential vacuum pump. Press the “Diff Pump Ion Gun” switch
on the ”Auto Valve Control” console. V4 valve will open.
2. Check if “Beam Voltage” is off and emission is zero on the “Ion Gun Control”
panel.
V4 Diff Pump
Ion Gun switch
Beam voltage
switch
Emission Ion Gun Control panel
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Measurement（Profile）2 Set up Ion Gun 1. Turn on the “Ion Gun Control” panel.
2. Adjust the Emission for the desired emission current, typically 25 mA.
3. Toggle the “METER” switch from “Emission” to the “Pressure”.
4. Open the Ar gas valve (Open valve).
5. Adjust the regulator on the leak valve for the desired gas pressure, typically
15-20 mPa.
6. Turn on the ”Thermo Valve Control” console. And then toggle the switch from
“Limit” to “Set Point”.
7. Check to see if the gas pressure about 10 mPa.
Open Valve Leak Valve
“Thermo Valve Control” console
Limit/Set Point
toggle switch
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measurement（Profile）3 Region Parameter.
1. Adjust the raster beam size in millimeters in the x and y axis on the “Ion Gun
Control”. Switch to the “INT” on the “raster drive” and “Remote” on the
Beam voltage.
2. Select the “Setup Profile” function from the “Acquire setup” pull-down menu.
3. Enter the element name, energy range (lower value and measurement energy
range), and cumulative numbers (sweeps).
4. Click the “Profile Params” tab.
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Measurement（Profile） 4. Profile Prameter.
1. Enter the total sputtering time（min).
2. Enter the Sputter Interval (min).
3. Select the “X-ray ON during sputter” as “No” and “X-ray retracted during
sputter” as No.
4. Select the “Sputter type” as Alternating.
5. Select the X-ray source.
6. Enter the “Delay after sputter (sec)”.
7. Click “Acquire” tab to start the measurement.
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Measurement （Profile）5 Ion Gun Shutdown
1. Toggle back the “meter” position to the “emission” position on the “Ion Gun
Control” panel.
2. Emission turn to zero.
3. Turn off the “Raster Drive” and “High Voltage” switches.
4. Close the leak valve completely and then slightly reopen this leak valve.
5. Wait about 5min to cool the thermo valve.
6. Close the leak valve completely and turn off the “Thermo Valve Control”
console.
7. Press the “Pump Intro” switch on the “Auto Valve Control” console. (V4: close,
V2 Open)
Leak valve Pump Intro
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X-ray Shutdown Procedure 1
1. Check to see if the X-ray off. (High Voltage lamp is off)
2. Toggle to the “INT” mode.
“INT/EXT”
toggle switch High Voltage lamp
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X-ray Shutdown Procedure 2
1. X-ray source voltage turn to zero using the “High Voltage Control” knob on
the “X-ray supply” (X-ray power supply) panel.
2. Push the “High Voltage” switch to the OFF/Reset on the “X-ray Supply”.
3. Turn off the “X-ray supply” power switch.
4. Wait the 10 – 30 min to cool the X-ray source.
5. Turn off the “X-ray Source Control” panel (X-ray controller).
6. When you use Neutralizer, turn off the neutralizer by selecting the “Neutral.
ON/OFF” from the “Acquire Setup” pull-down menu.
High Voltage
“X-ray Supply” panel
High Voltage
Control knob
“X-ray Supply” “X-ray Source Control”
Power Switch
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Removing the Sample 1
1. Check to see if the “HI VAC” lamp is “ON”.
2. Set the exchange position using the Knobs on the sample stage. (X, Y, Z)
3. Push the “Intro Sample” switch on the “Auto Valve Control” console. The V1
valve will open.
4. Slide the Introduction rod assembly into its fully extended position.
5. Move down the sample stage. See if the sample holder is seated onto the Intro
arm.
6. Move the Z axis down to it’s lowest position.
7. Slide back the Introduction rod assembly to its fully extracted position. The V1
valve will automatically close.
slide
Intro arm
Sample stage
Sample holder
HI VAC
INTRO
SAMPLE
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Extract the sample 2
1. Open the N2 gas valve.
2. Press the “Backfill Intro” switch on the “Auto Valve Control” console.
3. Open the Intro cap and remove the sample holder from the Intro arm.
4. Close the N2 gas valve.
5. Replace the Intro cap.
6. Press the “Pump Intro” switch on the “Auto Valve Control” console to purge
the “Intro chamber”.
N2 gas
Valve 1
Valve 2
“Auto Valve Control” console
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Daily Shutdown
1. Powering down the PC-ACCESS. Select the “Exit Program” from the “System
Control” pull-down menu.
2. Click on the “Yes” tab.
3. Press the “Card Lack Power” switch.
4. Shutdown the PC.
5. Turn off the “ISA BusBridge” and the “Picoammeter”.
