2024/7/26 update

X-ray Photoelectron
Spectroscope (XPS)
Basic manual
Acquisition section
Laboratory of XPS analysis

Contact K. Suzuki Ext. 6882
S. Yoshida Ext. 6882
1

Caution
Please keep the following rules.
• Take off your shoes, change into slippers. No food or drink. Clean up
the garbage.
• Contact with the staff immediately when you encounter machine
trouble. Emergency contacts are mentioned beside the entrance.
• Don’t use the machines roughly.
• Don’t take out equipments of this laboratory.
• Keep valuables yourself. Lock a door of this laboratory when you
leave here.
• Return to original setting after using if you change parameters ofsoftware and hardware.
• Don’t connect your USB memory to XPS-PC. Use the USB of thislaboratory. And take out the data through the PCs for analysis.
• Don’t touch with your hand anything which enter XPS chamber.
Clean the equipment if you make it dirty.
• Be careful when moving the stage. Do not neglect the visual check.
• Reserve XPS before using by yourself. And use the machine on time.
If you want to change your reservation, please cancel by the day
before. Cancellation on the day is invalid.
• It is the responsibility of your laboratory if equipment fails due tooperation not described in this manual. Students must let yoursupervisor know.
• If you use first time, contact the facility staff before using and takethe training.
• Don’t enter fragile sample, too big sample, gas exhaust sample to the
XPS chamber without permission. Please contact the staff in advance
if you are worried.
• When using the transfer vessel, be sure to contact the facility staff.

2

Before using
Write your name and start timein the “logbook” and write finish
time and parameters after using.
Check the analytical chamber
vacuum before use and write thevalue. Use as scheduled. Change ofreservation on the day is invalid.
Ar⁺ etching
gun chamber

AnalysischamberCheck the Ar⁺ etching gunchamber vacuum and theanalysis chamber vacuum.
Normally,✓ Ar⁺ etching gun ~10−4 𝑃𝑎✓ Analysis chamber ~10−7 𝑃𝑎

If the degree of vacuum issignificantly deteriorated, inform
facility staff.
Ion gun unit

Press the “Channel / float voltage”
button on the ion gun unit to lightit up and confirm that the display
number is "7“.
The current and voltage conditions of theion gun are input to each channel, and theion gun is set by selecting the channel
number. Channel "7" is a setting that does
not use etching gun.
3

Sample preparation
Normal holder(spare)Normal holder

Holder forcharged sample
Cover of Holder
for charged
sampleLarge holder

Fastener

Holder base

Remove the bottom plateof the holder when thesample is thick.

Set your sample on the sample holder.
Holders are stored in the vacuum
desiccator. Use normal holder for normal
sample.
Use the large holder for large samples (less than
100mmφ). Please contact staff for samples thatare worried about setting, such as samples thateasily emit gas, are too thick or fragile.

a sample is fixed to the holder using theFastener or carbon tape. Make sure thesample is completely fixed.
• About powder samples
Use carbon tape or attach (press) to ametal thin film (Al, In, Si, etc.). Blow using
blower at least 30 times to completely
remove unbonded powder. Vibrate theholder to shake off powder. If even small
amount of powder scatter in the chamber,the device will break down. If it causes a
breakdown, we will charge a repair fee.
Do not put pelletized powder if it iscracked or chipped when setting.

Make sure to clamp both sides of a sample. Set a sample
does not move even if the holder is upside down. Pay
attention to the positional relation between the X-ray
source and fastener & sample.

4Sample preparation (Appendix)
・Holder for charged samples
By applying a bias voltage to a sample,
the charge reduction using theneutralizing electron gun is made more
effective.
Applying + 100V to the bottom of a sample andapplying a potential difference to the cover of the
GND allows the neutralizing electrons to beefficiently applied to a sample surface. And it has
the effect of suppressing surface potential deviation
due to etching when Ar+ ion etching.

Mount the sample as shown in thephoto, cover and fix. The sample
thickness is limited to 1.3mm. Set thecover so that do not tough the copper
plate of the holder. Make sure a sample
surface is below the cover. Confirm that
there is no conduction between theholder cover and terminal.
・About contamination
To prevent surface contamination in the air, samples prepared by the dry process should be
wrapped in aluminum foil or stored in a vacuum device immediately after preparation. Samples
prepared by the wet process are washed with pure water after washing with acetone. Immediately
blow with air duster and wrap in aluminum foil.

・About reference peaks
It is convenient to prepare reference peaks in a sample to correct the charge shift of a sample.
Samples containing carbon may be more necessary because they may not be available for reference
because C1s peak of the contamination and the carbon peak from a sample overlap. For example, Au
thin film or mesh is placed together for measurement, or a sample is coated with Au and measured
together, or in the case of a powder, other powder whose chemical state is known is mixed and5measured together It is better to do.

Set into the sample exchange chamber
Don’t touch2

1
Sample exchange chamber

VENT

Check
no gaps

Set the holder into the sample exchangechamber and vacuum evacuate. Unlock
the chamber and press “VENT” button to
return the chamber to atmosphericpressure. Put the holder horizontally on
the rail in the chamber, and close it tothe back.
Turn(any direction) the magnet ring on
the sample replacement rod to change
from "OPEN" to "CLOSE“. Turn the ring toraise the hook under the rail. Look into
the bottom and check that the hook is in
the hole on the back of the holder.
Check that the ring is retracted to therear. Close the door, lock it and press the“VENT” button again to evacuate.
If this setting fails, the holder cannot be introduced
into the analysis chamber. Check it is set properly.

Back of holder

Magnet ring & Sample
replacement rod

Vacuum gauge of sample
preparation chamber

Checkwith eyes

Wait more

Evacuation of thesample takes about 30
minutes for metal plates
and about 2 hours for
powder samples using
carbon tape. Startup XPS
device while waiting.
6

Startup equipment
Turn on the chiller first. Next, press “SPEC”
button and “X-R” button to light up.
The chiller power supply is always first. Pressing X-R button
activate another chiller(you will hear motor sound). If thechiller is not running, press X-R again.

Chiller
SPEC

Turn on the stage lamp, the camera power,
the camera monitor, XPS-PC, and PC
monitors. After starting the PC, click"SPECSURF Acquisition" on the desktop tolaunch the XPS software.

X-R
Camera monitor
Stage lamp

Camera power

CCD stage camera
Don’t touch

Select “XPS” from theAcquire menu to open
XPS acquisition window(if not, PC reboot)For analysis
7

Startup equipment

This is Al-Kα X-ray

For monochrome

First, select the type of X-ray
source from the following list.
・Mg-Kα X-ray
・Al-Kα X-ray
・Monochrome X-ray (Al)Turn on the “Al/Mg” button for
Mg, and turn it off for Al. For
monochrome X-ray, select Al andpress the “MONO/STD” button toturn it on.

After selecting the X-ray source,
turn on the power of FILAMENT, andturn the ADJ knob slowly to increase
the current to 3.5 A. Wait for 5
minutes after increasing.

Analyzer power

Switch the display to “X-RAY
POWER” and turn on the X-RAY
power(Rightmost button). Increase
the voltage knob by 1 kV every 3
minutes to 10 kV. After another 3
minutes, increase the current knob
by 5 mA to 10 mA. For
monochrome X-rays, increase theseby one every 3 minutes to 12kV and
25mA.
Turn on analyzer power.
8

Startup equipment
Select the Source tab from XPS
Acquisition in SPEC SURF, enter thetype of X-ray source and voltage andcurrent values, and click “On” in
Status.

When the Status display changes
to “Update”, press the“AUTO/MANU” button on the X-R
POWER unit to switch to “AUTO”.

CLOSE

screw

OPEN

Measure size

left

right

3.0mmφ36

36

1.0mmφ24

120.7mmφ12

100.2mmφ1280.03mmφ4

1

The measurement area can be set
by using the two apertures shownin the left picture. Loosen thelocking screw and turn theaperture in the CLOSE direction to
decrease the number, or in the
OPEN direction to increase it tomatch the number in the table on
the left. Be careful not to turn it
too far. 36 is 0 after one turn in
the OPEN direction.
For depth profile, please set 1
mmφ or 0.7 mmφ.
9

Transfer into analysis chamber
Move the stage to the sample
exchange position. Press “P/M”
button on the stage controller toswitch the display to MEMORY, thenuse “UP” and “DOWN” buttons to
select the memory No. SE. Press“MOVE” button to move the stage tothe displayed position. Basically, thestage will not move because it isalready, but be sure to check it.

Stage controller

Sufficientvacuum2
1
3

The stage will fit in thegroove on the back of theholder.

After the sample preparation chamber issufficiently evacuated, press the “V1”button. Move the magnet ring to the rightto transfer the holder to the analysis
chamber. Send it while checking theanalysis chamber from the viewing port.
When you put it to the end, turn the ring
to change it to “OPEN” and return the ringto the left end. Press “V1” button again. If
you notice anything unusual, please callfacility staff.

Move it to a position
where it cannot move.

Turn the magnetic
ring and pull it out.

10Transfer into analysis chamber

Stage lever

After the V1 valve is closed, check thevacuum level in the analysis chamber. If
the vacuum is worse than 5.0 × 10−6 Pa, return the holder to the sample
preparation chamber immediately,
continue vacuuming for a while, andthen retransfer the holder. Wait untilthe vacuum decreases 10.0× 10−7Pa or
lower.
Operate the stage lever to move theholder. The center of measurement is
the cross on the camera monitor. When
there are several samples, use theposition memory function. Switch to
MEMORY mode with “P/M” button,
select the No. to be memorized with
“UP” and “DOWN” buttons, and press
the “ENT” button to memorize thecurrent position.
Zoom upDon’t touch camera
body

When aligning themeasurement position, be
sure to align the Z-axis aswell. Zoom the camera tofind the Z value that thecamera will focus on.
11

Setting of monochrome X-ray(Appendix)
Increase the monochrome X-ray output
to 12 kV and 25 mA in advance. Contact
the staff when using the unit for the firsttime.
switcherlocking
screw

X-Ray Source
Position Scale
Be careful not toaccidentally touchother parts

Ratemeter cannot be selecteduntil XPS acquisition is closed.

Loosen the lock screw on the left
picture switcher in the center of themain unit and change it to monochrome.
Change the position of the X-ray sourcefrom 45 mm to 40 mm by turning theknob shown in the left photo at theback of the device.
After transfer the holder, move it to theanalysis position, change stage tilt to 10°. Select “Acquire”→”Ratemeter” inthe software, enter the main peak valueof the element to be measured inCentre in the Ratemeter window, andclick “Start”. Find the value on the stage
Z axis where the peak intensity ishighest, register that position in stage
controller. Change the Ratemeter values
for “Pass, Dwell, Refresh time”. so thatyou can easily see the increase or
decrease in peak intensity with Z
movement. If high intensity is notpossible, there is a way to tilt up to 20°. Please refer to “Angle Resolved”
to remove the tilt limitation. Contact
12
staff when using.

Setting of Ar⁺ etching gun(Appendix)
Set up the Ar⁺ gun when you want to remove contamination from thesample surface or measure the depth profile. Contact the staff when
you use it for the first time.
Use a measurement size of 1 mmφ or 0.7 mmφ. Ar⁺ etching may
affect the chemical state and composition of the sample surface. The
etching area is 3 x 3 mm centered on the camera display position.

Vacuum gauge of Ar⁺ gun

After transfer the holder, wait until thevacuum in the analysis chamber is less than
10.0× 10−7 Pa.
Turn the valve
at the backAr gas valve
This is too much gas.
Tighten the valve!

Auto valve controller

Press ”AVC” button on thevacuum gauge of Ar⁺ gun. Turnthe Ar gas valve on the left
picture slowly counterclockwise
to adjust the vacuum to
10.0×10-2Pa. The valve always
has a marker at 6 o‘clock
direction. About one turn will
adjust the vacuum to 10.0×102Pa. Watch the vacuum gauge
and turn it carefully. Too much
Ar gas will damage theequipment. Wait 10 minutes
after equilibrium is reached.

Turn the lever of the auto valve controller
to ON. the Ar gas valve will start to tighten
and the vacuum of the Ar⁺ gun will drop
temporarily.
13

Setting of Ar⁺ etching gun(Appendix)
Press the Channel button on the Ion
Gun unit and turn the X knob to selectthe etching condition. The conditions
are as shown in the table below.
Etching rate is measured on SiO₂.

2024/7/26update

channel

Ch1

Ch2

Ch3

Ch4

Ch5

Beam energy(eV)

3000

2000

1000

500

3000

Emis current(mA)

19.6

19

20

20

19.6

Gas Pressure(x10⁻²Pa)

9.7

9.7

9.7

9.7

9.7

Etching rate(nm/min)

5.5

3.6

1.4

0.3

5.3

6.0

4.0

1.5

0.3

5.5

previous rate Etching rate(nm/min)

Select “Depth Profile” in Experiment tab,select Profiling tab, enter channel number
to be used in Preset, enter Gas Pressure
value in above table to Gas Pressure, andclick Set.
If you want to do Depth profile, go to"Depth profile" page.
9.0

Etching can be started by pressing“Irradiation ON/OFF” button in Ion
Gun unit, and the elapsed time ofetching will be shown on the display
by turning on “Timer Display” (thetime will be reset by pressing “Timer
Reset”).
14

Setting of charge neutralizer(Appendix)

Glass sample

Neutralizer unused

charge neutralizer unit

Neutralizer used

In the case of non-conductive
samples, non-uniform charging
may occur on the sample surface.
The non-uniform charging affects
the energy value and the half
width. The use of charge
neutralizer can alleviate thecharging phenomenon by
supplying electrons to the sample
surface.
・How to use charge neutralizer
1. Power on charge neutralizer
unit
2. Press “SEL” button tochange the ADJUST item to“FIL”. and turn the ADJ knob
to increase the current
value slowly to 6.0A.
3. Select Ratemeter fromAcquire in the softwaremenu. If XPS Acquisition is
open, close it first.

15

Setting of charge neutralizer(Appendix)
4. Enter the photoelectron peak
position of the sample in “Centre”,
and change “Pass, Dwell, andRefresh time” to appropriate
values to make it easier to see thepeak shape. Click “Start” andcheck Intensity value.
5. Turn on “Acc.V” on the unit,change the ADJUST item to Acc.V
using the “SEL” button, and turn
the ADJ knob to change thevoltage value while searching forthe voltage value that has thehighest peak count and the proper
peak position.
6. Once the voltage value isdetermined, close the Ratemeterand measure wide and narrowscan. The appropriate voltage
value is different for each sample.

DC power supply device

When using the holder for charged samples
Before setting up the neutralizer, turn on thedevice as shown in the left figure and apply
voltage to the holder.
1. POWER On, and OUTPUT On.
2. Turn the current knob to apply asmall amount of current.
3. Turn the VOLTAGE knob to set to100.0V.
16

Setting of transfer vessel(Appendix)

Holder for transfer vessel
Do not touch the left part fromhere with your bare hands!

Transfer vessel

Opening/closingknob

Fix the holder in this orientation.

Always contact facility staff whenusing a transfer vessel. Do all work
carefully.
Do not give any shock to thetransfer vessel. Make sure that
there is no dust on the O-ring. Be
careful when transferring the holder.
After fixing the sample to theholder in the glove box, mount theholder in the transfer vessel. Pay
attention to the direction of theholder when mounting it (see thefigure on the left). Turn the
opening/closing knob to tighten it
firmly.
Remove the lock of the sample
preparation chamber door andremove the blank flange from thedoor after VENT.

Blank flange
Do not touch the inner partwith your bare hands!

17Setting of transfer vessel(Appendix)

Fixing ring

When evacuate, push thevessel body in a little by hand.

Align the pins to attach the transfer
vessel to the door and turn the fixing ring
to fix it to the door. Lock the door andpress the VENT button to evacuate.
When the vacuum in the sample
preparation chamber exceeds
0.5×10⁻³Pa, carefully turn the
opening/closing knob to open the vessel
little by little. Opening the vessel too large
will cause the pump to malfunction.
Check the vacuum level and open thevessel carefully.

Open the vessel slightly.

Stop opening. Wait until
the L lamp lights up.

Once the vacuum in the vessel is drawn, fully
open the opening/closing knobs. Operate themagnetic ring to receive the holder and close
the vessel. When the vacuum in the sample
preparation chamber is drawn, open V1 andtransfer the holder into the analysis chamber.
Close V1 valve.

18

Wide scan
There are a total of six different
measurement methods. It is
recommended to start with a wide scan
for all measurements.
Select “Wide scan” in Experiment.
Select “None” for Movement to measure at
the current stage position or select“Memory” to use the memory position of
the stage controller.
Select the measurement size in Lens Mode.
Input the first number (First) and the last
number (Last) of the memory number forcontinuous measurement in the Stage tab(when Memory is selected). Set eachcondition of Wide scan in Regions tab.
Mainly check the Start(eV) value and thenumber of scans. If you want to see peakson the high energy side, increase the startvalue, and if you want to see small peaks,
increase the number of scans.
Click “Start” to start measurement
and click “Check” to display theestimated measurement time.
19Markers
Use markers to identify the peaks thatappear in the wide scan spectrum. Click
Markers icon on the left.

The position of the marker is based on
the standard, so it may be different
from peak position of the actual sample.

A line will appear on the spectrum. Whenyou put the line to the peak position, a list ofelements will be displayed in “Suggested
Peaks”. Select an element from the list andclick “Add” to stamp the element name on thegraph. And you can select from “Element” item.
Some elements also have a Chemical Shift listthat can be stamped as well. Clicking OK at theend will leave the stamp.

You can see the spectrum of the standard
sample in the XPS handbook, so please refer
to it.
Handbookicon

In addition to the photoelectron peak, various satellite
peaks appear in the spectrum. In particular, the K-α₃,₄satellites appear at 10 eV lower energy than thephotoelectron peak. And when using Mg-Kα, Satellite
peaks called "ghost peaks” derived from O-Kα(730eV
higher), Al-Kα(230eV lower), Cu-Kα(320eV higher) appear.
When using Al-Kα, same satellites appear.(960eV higher(OKα), 230eV higher(Mg-Kα), 560eV higher(Cu-Kα))20

Narrow scan
It has a high energy resolution and mainly
acquires the spectrum of the main peak ofeach element. Select Narrow scan inExperiment. For Movement and Lens Mode,
refer to "Wide scan".
Set the memory number in the Stagetab (when using Memory position, see"Wide scan"). If the measurement
contents are different for each sample,
you can set the group. Enter a groupname in “Groups”, click “Add”, enter the
memory number in First and Last, andselect a name from “Group”.

Select region

Select “Group” in the “Regions”
tab (when using the Groupfunction), select the element to bemeasured from “Element”. Openthe measured wide scan spectrum
and click the "Select region" icon
to display Start (green) and Finish(red) lines on the spectrum. Adjust
the line position according to thepeak to change the measurement
range. Set the number of scans toabout 10~100. More scans willtake more time, but will reduce
the noise.
21Narrow scan

If you click “Pause” in “Acquisition
Status”, the measurement will beinterrupted after one scan, and only the
number of scans can be changed. Afterchanging, click “Continue” to restart themeasurement. Pressing “Stop” will end
the measurement after one scan cycle,“Abort” is force termination.
・About the spectrum window

Scale icons

When the mouse cursor is placed on the spectrum,
the energy position and intensity are displayed in thelower right of the spectrum window. In the upper left
corner, there are icons to adjust the display scale. The
spectrum obtained by continuous measurement isstored in one window. You can change the display ofeach sample, each region, and each level from themenu at the top right of the spectrum window.
Save, Open, etc. of data are also done in eachwindow. In the spectrum window, sample numbers
are assigned from 0. Don't make a mistake with thesample number.
22

Depth Profile
By repeating the Ar⁺ etching andmeasurement alternately, thedepth profile can be obtained.
Contact the staff when you use it
for the first time.
Select “Depth Profile” inExperiment and adjust Ar gas
pressure of the etching gun (see“Setting of Ar⁺ Etching gun").
Select “Full” in Acquisition Mode.
If you select “Separate” or “Simultaneous”, you can
set the energy positions of Peak and Background andacquire only their differential intensities. Since nospectrum is acquired, the measurement can be
performed at high speed. (See "Image & Linescan")In the upper image, the etching time isset to 0 seconds before the firstmeasurement (in the unit of level), each
15 seconds before the second to fourth
measurements, and each 60 seconds
before the fifth to tenth measurements.
The total etching time is 405 seconds.

Set the etching time in “Profiling”
tab.
“Regions” settings are the same as"Narrow scan".
Etching changes the state of thesurface potential and chemical
state, and the peak position may
move significantly, so you shouldmeasure a little wider.
Atomic mixing, selective
sputtering, etc. may need to betaken into account in the analysis.
23

Angle Resolved

Magnetic lensMagnetic lens stage

Locking screw

By measuring the spectrum while thestage is gradually tilted toward theanalyzer axis, the depth profile of thesample can be obtained nondestructively.
Contact the staff when you use it for the
first time.
The stage can be tilted up to 80° toobtain a depth profile from 6 nm to 1 nm.
A high tilt angle extends the area of thesurface to be measured in the Y-axis
direction, increasing the amount of signal.
It can be applied to the analysis of minuteamounts of components.
The stage will be moved a lot, so pleasebe very careful. After analysis, be sure to
restore the settings of both hardware andsoftware. After measurement, be sure todelete the positions registered in thememory function.

・Setup of the XPS main unit

SwitchMicrometer of themagnetic lens stage

Transfer the holder to the analysis
chamber. Be sure to fix the sample firmly
as it will be tilted. Loosen the locking
screw and turn the micrometer of themagnetic lens stage to lower it from
Z=17.95 to Z=8.5. Make sure the switch at
the bottom is pressed (you should hear asmall click. Be careful not to lower it too
far or it will break). Tighten the loosenedlocking screw again.
24Angle Resolved
・Setup in Spec Surf software
Go to "View" -> "Configuration" to launch"System Configuration", and select "High
Angle" for "Sample Holder". the tilt limit will be
released, allowing you to move the stage from 30° to 80°. After that, please operate thestage with great care. If you only want to dowide and narrow scan at high angle, you cancontinue as usual.
Configuration

Select "Angle Resolved" in theExperiment tab, and set the tilt angle ofthe stage in the Profiling tab. In the left
picture, XPS acquires spectra at each level
while tilting from 0° to 80° in 5° steps.
If you want to tilt the stage more than 10°, be sure to move the position of the
X-ray source back by 5 mm (see "Settingof monochrome X-ray").For the rest of thesettings, refer to "Wide Scan" and"Narrow Scan".

← If the holder is tilted in theminus direction, there is a riskof it hitting the X-ray source.
Basically, it is prohibited.
Please consult with staff.
25

Total Reflection

2000

1500

1000

500

0
540

536

532
O 1s BE (eV)

528

524

check the tendency of thesignal-to-noise ratio.

Total Reflection uses monochrome X-rays, andby adjusting the position of the stage so that
total reflection of X-rays occurs, it is possible toobtain spectra that are about two-thirds
shallower than the normal measurement depth,
and with a better signal-to-noise ratio due to theno penetration of X-rays. It is mainly used toevaluate contamination on the surface of asample. Only samples with smooth surfaces(such as Si wafers) can be measured. Contact thestaff when you use it for the first time.

・Measurement Method

1. Place the sample in the holder so thatthe sample surface is parallel to thestage, and transfer the holder.
O1s
2. Set up the monochrome X-ray andadjust the Z position while checking thephotoelectron spectrum of the sample
with Ratemeter (see " Setting of
monochrome X-ray ").
3. Select "Total Reflection" in "Experiment",
tilt 0.2° from -10° to -5°, andC1sacquire the spectrum, and check thetendency of the signal-to-noise ratio.
Si2p(see " Setting of Total Reflection")
4. Check the spectrum with Ratemeter by
1° from -4° to -1°, and fine adjust Z
600
400
200
0
Wide BE (eV)again to get the intensity.
5. After the Z adjustment, measure at theNormal wide scan Total Reflection scanangle with the best S/N ratio. Basically, You can see that the intensity of the1°.
contamination C1s peak is about twiceas large as in the normal measurement.

26

Image & Linescan

Bk2

Bk1

Peak
Separete

Simultaneous

Acquire the intensity at each energy
position with 9 detectors, and subtract
the background intensity from the peakintensity to draw the mapping.

Image can obtain elemental mapping
images up to 5.0 x 1.8 cm in size. If
chemical shifts are available, it ispossible to map the distribution ofoxides and metals, for example. Contact
the staff when you use it for the firsttime.
First, obtain a Narrow scan of theelement you want to measure. Select"Image" in "Experiment", and select"Separate (PB separate method, easy to
set up)" or "Simultaneous (PB
simultaneous method, fastmeasurement)" in "Acquisition Mode".
・Separate
Set the values of Peak, Bk1, and Bk2
based on the spectrum of Narrow scanacquired in the Regions tab. Only theintensity at that energy positions are
acquired.
・Simultaneous
Click the Channels column and selectwhether the intensity to be acquired byeach channel (detector) should be
Background or Peak. Change the Passvalue appropriately so that the highenergy side Background, Peak, and low
energy side Background of the element
to be measured.
27

Image & Linescan
No.1

Mapping area
No.2

Register the upper-left stage position tomemory No.1 and the lower-right stage
position to memory No.2 of the sample
area for which you want to acquire theimage using the stage controller.
In the Image tab, click "Read" toread the memory positions." In
Scan, select either Size or Step andset the resolution of the image. For"Mode", select "Image".

←Mapping image obtained by "Image". red:Siand blue:Au. The image of each element in the
mapping result can layered in different colors.

Select "Linescan"for "Mode" toperform line profile
from memory No.1
to No.2 position.
Si peak(SiO₂)
Si(SiO2)

Si(Si)

Si peak(Si)←Linescan results by
Simultaneous method. This is a
Si wafer etched with Ar⁺ in
the center.
28

Saving data
All measured spectrum data areautomatically saved with the name ofthe date, measurement method, and
X-ray source in “Auto Storage” folder.
Select the Auto Storage folder from
"File" -> "Open", select the data, thedetails of the data will be displayed at
the bottom of the save window.
To save the spectrum in a different
format, select "File" -> "Save as" andchoose the file type.In addition to
SpecSurf data, text format and VAMAS
format can be output.
You can output the spectrum as animage in report format by clicking"File" -> "Report". You can also paste
the spectrum as an image by clicking“copy“ on the spectrum window.
If you want to keep the data on thisXPS-PC, please save them in a folder“data”. Please keep a folder for eachlaboratory.
Basically, please bring back themeasurement data by yourself. We
cannot guarantee the preservation of
the data.

Report image
Save in eachlab folder
Open, Save &Copy icon

29

End procedure
If you have any of the following uses, please perform the following
end procedure before the normal end procedure.

・ Using the holder for charged samples
Return the voltage and current values of DC power supply device to 0.
OUTPUT OFF.
POWER OFF.

・ Charge neutralizer
Return the voltage and current values to 0.
Acc.V OFF.
Unit Power OFF.

・Using Ar⁺ etching gun
Auto Valve Controller OFF.
Close the Ar gas valve clockwise to about 9 o'clock (1/4 turn).
Wait for 3 minutes.
Close the Ar gas valve clockwise to about 6 o'clock (3/4 turn).
AVC of Ar⁺ etching gun chamber vacuum gauge OFF.

・When Angle Resolved measurement carried out
Move the stage to the sample exchange position.
Return the X-ray source position to 45mm(if it has been changed).
Return the Z-axis of the magnetic lens to Z=17.95 and retighten the locking screw.
Reset the holder setting in “Configuration” to “Standard”.
Delete all position registered in the stage memory.

・ Using monochrome X-rays
Move the stage to the sample exchange position.
Return the X-ray source position to 45mm.
Return the switcher device to “Baking” and tighten the locking screw.
After 15 minutes have passed since you performed the “X-ray shut down"
procedure on the next page, press the "MONO/STD" button to return to "STD".
If the stage tilted above -10 °, perform the procedure described in “When Angle
Resolved Measurement carried out”.

・When using the transfer vessel
return the holder to the sample preparation chamber, re-seal the holder in thetransfer vessel.
Unlock the door and VENT. After VENT, remove the transfer vessel and reattach
the blank flange to the door.
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Lock the door and draw a vacuum in the sample preparation chamber.

End procedure
This is a common procedure for all measurements. Please be sure tofollow the procedure.

・X-Ray shutdownPress “Auto/Manu” button to change to “Manual”.
Reset X-Ray current to 5 mA and voltage to 3 kV.
Turn off X-Ray power.
Change the display to show “FILAMENT POWER”.
Turn the ADJ knob of FILAMENT to set the current back to 0.
Turn off FILAMENT power.
Click “Off” in the Source tab of XPS acquisition in Spec Surf.

・ Take out the holder
Press the P/M button on the stage controller to change to MEMORY mode.
Press UP and DOWN buttons to display No.SE.
Press the MOVE button to move to the sample exchange position.
Press the V1 button to open the V1 valve.
Turn the magnetic ring to the “OPEN” position and push it forward.
Turn the magnetic ring to the “CLOSE” position.
Pull the black ring out to the end and return the holder to the sample exchangechamber. Press the V1 button again to close the V1 valve.
Open the lock of the sample exchange chamber.
Press the VENT button to return the sample exchange chamber to atmosphericpressure. Turn the magnetic ring to “OPEN” and take out the holder.
Lock the sample exchange chamber and press the VENT button to draw vacuum.

・Finish XPS equipment & other tasks
Remove the sample from the holder, clean the holder, and place it in the vacuum
desiccator to draw vacuum. Clean up the workbench.
Turn off analyzer power HT.
Turn off the camera, camera monitor and stage lamp.
Transfer measurement data to PC for analysis using the USB memory of this Lab.
Shut down Spec Surf, PC and turn off display.
After 15 minutes from X-ray shutdown (when using monochrome X-ray, switch
MONO/STD to STD), turn off the X-R and SPEC buttons.
Turn off the power of the chiller.
Enter the vacuum level of the analysis chamber and the end time in the logbook.
When using the laboratory at night, turn off the lights and lock the door.
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