2020/3/4 Update

Energy Dispersive X-ray
Spectrometer(EDS)
Basic Manual
Laboratory of XPS analysis

Contact M. Sakairi Ext. 7111
K. Suzuki Ext. 6882
1

Caution
Please keep the following rules.
• Take off your shoes, and change into slippers.
• No food or drink. Clean up the garbage.
• Contact with staff immediately when you encounter apparatus
trouble.
• Don’t use the apparatus roughly.
• Don’t take out tools of this laboratory.
• Keep valuables yourself. Lock a door of this laboratory when youleave here.
• Keep the limit of the stage transfer. The stage will hit the detector
if you move the stage beyond the limit.
• Return to original setting after using if you change parameters ofsoftware and hardware.
• Don’t connect your USB memory to SEM PC. Use the USB of thislaboratory, and take out the data via the PC for analysis.
• Don’t touch with your hand anything which put in SEM chamber.
Clean the tools if you make it dirty.
• Reserve the apparatus yourself before using, and use theapparatus on time. Changes to reservations must be made theday before. Change of reservation on the day is invalid.
• Respond the all troubles by your laboratory if you use at night,
early morning, holiday. Students must let your supervisor know.
Emergency contacts are mentioned beside the entrance.
• If the first time using, make contact with the staff before using
and reserve the training.
• Don’t put fragile sample, too big sample, gas exhaust sample into2
the SEM chamber without permission.

Before analysis
Check the scanning electron microscope (SEM)
Basic Manual for the usage of SEM.
Power on the EDS 10 minutes before
starting the EDS analysis software.

EDS power

After 10 minutes, start EDS software“Analysis Station”.
Create a new project folder oropen your existing project folder.
EDS data is saved as project folder unit.
SEM images taken into EDS and analytical
spectrum data linked to SEM images are
saved in the project folder. You can create
a new project for each sample, or you cantreat some sample groups with one
project. Always save the project after
measurement. It is better not to change
the contents of the project folder.

EDS software “Analysis Station” hasbeen installed in PCs for analysis. Youcan open the project and edit the data.
PCs for EDS analysis

3Import analysis area
SSM couting
rate monitor

Import the area for EDS analysis into the“Analysis Station”.
Check the “SSM couting rate monitor” thatappeared at the same time as the software
startup. Adjust the accelerating voltage andspot size of electron beam so that the value ofcps (the amount of X-rays) is increased to therequired value.
In general, about 5000 cps for spectrum analysis and about
20000 cps for mapping. Acceleration voltage 20 kV and SS 65 isbetter for analysis. When the main composition is light elements,
the acceleration voltage is better to be 10-15kV. If the value ofcps is low, signal-noise ratio will be poor. In that case, it can besolved to some extent by increasing the measurement time.

↑Reduce until
light blue

Image

After adjusting the focus and contrast, click
the “Image” icon to import the SEM image.

SEM image taken intoAnalysis station•The value of acceleration voltage
The magnitude of the acceleration voltage necessary for
excitation is decided by each characteristic X-ray of eachelement. Please note that EDS analysis can not be done
unless excited! Regarding the acceleration voltage required
for excitation, check the periodic table poster behind theSEM apparatus. Usually, it is better to set the acceleration
voltage to about 2-3 times the energy of the characteristic
X-ray to be measured. Also, the strength of the acceleration
voltage effects for the area, equivalent to the characteristic
X-ray generation area, that the electron beam diffuse in thespecimen. That is equivalent to the characteristic X-raygeneration area. Even if you carry out point analysis,
actually you measure X-rays from the point deeply andextensively (about 1 µm). For details, refer to the poster’s
Castaing formula.

4

Spectral analysis(Collection/Qualitative)
Collection

Analyze the EDS spectrum the whole of
the SEM image with “Collection” icon.
EDS spectrum

End with “Stop”
Qualitative

Periodic table
Green peaks
are main peaks

After acquiring the spectrum,identify the peak automatically with
“Qualitative” icon in the spectrum
window menu. You can check andchange the qualitative elementswith “Periodic table” icon.
Label

Qualitative elements
are indicated in pink
"Label" icon in the periodic table allows you to selectthe characteristic X-ray labeling of the selected
element. All types of characteristic X-rays are notlabeled and please change as needed. Especially small
peaks are not labeled, so if there are unknown small
peaks, you should check here.

Labeling edit menu

5Spectral analysis(Identification/Quantification)
Spectrum scale icons

You can change the scale with the icons
in the lower left of the spectrum window.

For small peaks that can not be identified
by automatic qualitative, it is necessary to
do by yourself.
Identification

QuantitativeRegisterOK

Click on the position an unknown
peak in eds spectrum. Click on“Identification” icon, acharacteristic X-ray suggestion isdisplayed for that peak. Selectingand registering the element, it isadded to the result ofidentification.

Click the "Quantitative" icon,
you can see the results of therelative quantitative values of
the qualitative elements. Click“OK” after confirming. You click“Yes” when close the spectrum
window, the quantitative
results will be registered in thespectrum data.
6Spectral analysis(Saving/Condition)
Click “ファイル(F)”→”エクスポート(E)” in the menu in the spectrum
window. spectrum graph data canbe output by selecting the file type
Setting “csv”.
The spectrum data is linked to thecaptured SEM image and placed in
the list below when the image wasselected. Quantitative results are
You can choose mass% or atm%
also listed. The display format canbe changed from the “Setting”
Periodic tablebutton on the list.
If you select multiple spectra datafrom the list and select “Analysis”
from the top menu, you canAnalysis
Start
quantify multiple spectra at once.
Select multiple spectra data from
Auto/manual
the list and click “Compare” in theright-click menu to display
multiple spectra side by side

Comparedisplay of multiple spectra7Spectral analysis(Saving/Condition)
CheckExport

Case of pointanalysis
Case of map

Click the “Check" icon in thespectrum window menu to display areport window for SEM images,spectrum image, and quantitative
results. Click "Export" in thewindow and selecting Word orPowerPoint, the report will beoutput. Multiple reports can beoutput at once by using “Compare”of previous page.
In the case of mapping, click “分析(N)” → “スペクトル表示(D)” from the mapping window
menu to open the spectrum window. After
performing quantification, click “Check” todisplay the mapping image, spectrum image,quantification result report.

Conditions

Collection

Continuous
analysis

Pixel size
scan times

Mapping
Expected time

In “Conditions” window, you can change theintegration time of spectrum measurement. It isbetter to set a long time when the X-ray
intensity is low.
S / N ratio is improved by the route times theintegration time. The S / N ratio is doubled at 4times the integration time. However, no matter
how the S / N ratio improves, the detection limitof the peak is about 0.1atm%.
In “Conditions” window, you can change
integration time of continuous analysis, pixel sizeand scan times for elemental mapping,
execution interval of probe tracking, etc. Ifchanged, please return to the original
8parameters at the end.

Continuous analysis
Continuous

You can carry out the point analysis, area analysis,
and line analysis from “Continuous” icon.
You can not select it unless you close the spectrum window. Andimport SEM image first.

Tools
Number ofline analysis
Quantification
Auto/manual

Probe tracking
Expected time
Start

Select the analysis method from the“Tools” and set the analysis position in
the imported image.
When the measurement time becomes
longer or the magnification of the image
is high, it is possible to prevent thesample deviation by “Probe tracking”.
“Probe tracking” correct the original analysis
position by beam shift when there is a position shiftcompared to the original captured image. Before
using, be sure to reset beam shift before capturing
images.
When you check the Quantitation, Quantitation will
be carried out automatically.

Click “Start” to take measurements inorder.

Copy

In line analysis, the horizontal
axis of the profile can be drawn
as distance. Results can besuperimposed on SEM images.
Click “Copy" to copy the line
profile graph data.
9Elemental mapping
Click the "Map" icon to draw the intensity distributionof each element in the capture SEM image area.
Click the “Condition” icon and set the number of mapping scantimes and resolution in advance.

Map

Mapping images

When start mapping, theelements that have beenregistered in the periodic table
are mapped. If you want to add
a mapping element, register it in
the periodic table (make it pink)
and click the "Playback" icon

Playback
Periodic table
Eagle eye spectrum(spectrum with smaller count)

Two spectrum windows appear at the sametime as the mapping. One is the spectrum of
the entire SEM image (same as “Collection").
The another is called "Eagle Eye Spectrum",which is a spectrum that shows thesuperimposition of spectra for each pixel of theimage. In the Eagle Eye spectrum, peaks can befound even for element that exist only in a smallarea. Can be used to find trace element.
Elements that exist
only in part of theanalysis area may
not show peaks inthe spectrum of theentire SEM image.

Spectrum of entire SEM image

10Elemental mapping(extract/line display)
Tools
Extract

In mapping window, you canpartially extract data andgenerate line profile frommapping measurement data.
• Extract
Selecting a tool and specifying
its position on the SEM ormapping image, create aspectrum in that area.
• Line display
Click the “Line display” icon todisplay the line profile of eachelement. The position and widthof the line can be adjusted freely.

Line display

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Elemental mapping(overlap/quantitative map)
• Overlap
The mapping images of eachelement can be overlapped in
RGB color.

Overlap

The image can be saved by right-click
copy or by “ファイル(F)” → “エクスポート(E)" from the mapping window menu.

• Quantitative map
Convert intensity mapping data
to quantitative maps. Click “分析(N)” → “定量マップ作成(Q)"from the mapping window menu.
Select the map size and unit in
the generate conditions window,and click ”Generate” to display
the quantitative map.

Map size

Generate
Mass%
atm%

Intensity map Au Al Ti

Since the intensity map is an intensity
distribution image of the main peak ofeach element, the distribution of eachelement can be understood, but theamount cannot be compared between
each element. Quantitative map represent
quantitative values of each element incolor. Intensity map has the influence ofshielding of characteristic X-rays (signalattenuation) due to irregularities on thesample surface. Quantitative map has
little influence, even if there is somesignal attenuation, because the map iscalculated quantitative values anddescribe the distribution.

Quantitative map Au Al Ti

12Other functions
When identifying a small peak, you can check thespectral fitting coefficient by using "VID" in the spectrum
window menu. The correctness of the identified element
can be evaluated by fitting calculation.
Fitting coefficient

Register

Fitting coefficient decreased

Considering an unknown peakas Fe and registering theelement, the value of the fitting
coefficient decreased.
→ Right qualitative.

Small peaks that could not be
determined by automatic qualification

Residue display

Identify as Fe

In addition, the residual between
the spectrum calculated from thequalitative composition and themeasured spectrum can bedisplayed. The residue display
makes it easier to find peaks thathave not been qualified.

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Residue display

Other functions
If the peaks overlap, quantification may not work. You can doquantitative calculation or regenerate new intensity map by changing toother X-ray that no overlapping peaks in the "Periodic Table".

W and Zrpeaks overlap

Select the type of Xray and re-register
the element

If change the X-ray type,
you may see a difference
in distribution

Fe-Kα map
30 µm

Fe K

Mass%Fe-Lα map
30 µm

PHA

Changed to W-LαFix

If the mass% of acertain element in thesample is known, themass% can be fixed inthe "Periodic Table".

Fe L

When the X-ray cps is small in the mapping,
you can increase the cps and measure bychanging “PHA” from T3 to T1 in the“Conditions” window. However, use it forelemental analysis after Na because the energy
resolution is reduced. Please be sure to return
initial condition after use.
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EDS analysis end procedure
Conditions• Please return each parameter toinitial state by "Conditions" icon.
• Save project folder.
• Close “Analysis station”.
• EDS power Off.

Don’t forget！
Initial stateSaveprojectfolder• Please refer to "SEM Basic
Manual" for how to end SEM.

Appendix
This table is an example of peaks overlapping. If thiscombination exists, use VID to check the peaks well.

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