2020/3/2 Update

Scanning Electron Microscope(SEM)
Basic Manual
Laboratory of XPS analysis

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

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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 machine
trouble.
• Don’t use the machines roughly.
• Don’t take out equipments 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 through the PC for analysis.
• Don’t touch with your hand anything which enter SEM chamber.
Clean the equipment if you make it dirty.
• Reserve SEM before using yourself, and use the machine on time.
Change the reservation beforehand if you can‘t finish on time.
• 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 you use first time, make contact with the staff before using andreserve the training.
• Don’t enter fragile sample, too big sample, gas exhaust sample to
the SEM chamber without permission.
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Before using
Write your name and start time on thelog book, and write finish time andparameters after using. Use as scheduled.
Change of reservation on the day is invalid.

The device PC shuts down every time.
Press the power button on the device PCand displays. Launch the SEM software by
double-clicking the SEM icon on theWindows desktop. When using EDS, turnon EDS power at least 10 minutes before
Launching EDS software

SEM log bookSEM icon
SEM-PC

Please manage your data by yourself. We
do not guarantee your data stored in SEM
PC or analysis PCs. To retrieve the data,
use the USB for data copy, copy it to PCs
for EDS analysis, and save it on your own
data media. It is forbidden to plug yourown USB into SEM PC.

EDS power
USB memoryfor data copy

“Analysis Station” which is EDS software
has been installed in PC for analysis.
Please feel free to use PC for analysis.

PCs for EDS analysis(EDS software installed )3Sample preparation
Set sample on the stage

SEM holder （Large / Small）

SEM holder and stages are in
SEM box. Carbon tapes and carbon
pastes are prepared.
Don’t touch with bare handanything which is put into SEM
chamber.

Stages

SEM holder
Large (32mmΦ×10mmh)
Small (10mmΦ×10mmh)
Stages4 kind of stage are prepared.
Set the stage to the SEM holder byhexagon head bolts.

ExampleSame height as holder✓ Don‘t put the large samples on thestage beyond the height of holder.
✓ Set the sample at same height of
SEM holder.
✓ Set the sample strongly to prevent
moving the sample in SEM chamber.
✓ Don’t insert samples which makeSEM chamber dirty.
✓ Enter the sample in SEM chamber
after blowing

Please ask the staff if you havesome questions.
Bonding agents4

Enter sample in SEM chamber #1
Open to air pressure
Click a “VENT” on SEM software,and then click a “OK”.
＊The Black display section noticechamber conditions.
Z axis is shownright scaleConfirm the stage position
before open the chamber door.
Notice the angleof tilt especially✓✓✓

Z axis：more than 25 mm
X・Y axis：around 20 mm
Rotation・Tilt：0°

The following are prohibited✓ Z axis：less than 10 mm✓ Tilt： more than 20°or -5°(When WD=10mm)
After confirming , Lay yourhands on knobs, and then openthe door5

Enter sample in SEM chamber #2
Set a holder on a stage in SEM chamber

Back side of holder

Projection

Stage in SEMchamber
Set the holder
to this line

Slide the holder to the projection on thestage from left side, and the projection
insert to chase on back side of holder.
Confirm the holder don’t hit any detector,
and then close the door.
Click a “EVAC” on the SEM software, andthen click “OK”. Evacuation start.
Hold the door by your hands after click “OK” forseveral seconds.

Electro beamemitting port

EDS
intake port

Detector of
secondaryelectron

Detector of backscattered electron

Confirm large
distance
Closechamber6

Observation #1
You can observe sample, after
changed the condition of thechamber to “Ready”.
Click a “HT” on SEM software, andthen SEM image will appear.

Set conditions of electron gun
Acceleration voltage：0.5kV - 30.0kV
Spot size (SS)：0 - 99
General conditions
SEM: Acceleration voltage 10 kV, SS40
EDS: Acceleration voltage 20 kV, SS65

Acceleration
voltage

Spot size

The effect of conditions of the electron gun
Low

Acceleration voltage

High

Spot size

Large

High

Resolution

Low

Irradiation current

smallLow

ResolutionClear

Surface structure

Unclear

Low

Charging up

HighHigh

Charging upLow

Small

Damage

Large

Large

DamageSmallBadHigh

Small

Backscattered electron image

GoodLarge

Large

Image noisesmall7

Observation #2
Stigma X/Y：
Modification ofastigmatism

ACB：Automaticadjustment ofcontrast & brightness

Move the stage (X/Y axis) to target
position at low magnification.
In the case of no image on SEM software,
put the ”ACB’ or click a “scan 2”.

Save a image

Set the working distance (WD) at 10mm, and then adjust Z axis to match
the WD.

Change Fine/Coarse

SEM observation : WD = 10 nm and more
EDS analysis : WD = 10 nm

Magnification

WorkingDistance

Focus

Contrast /Brightness

Projected distance

Recommended use of scan mode
Scan 1： Set stigma X/YScan 2： Search target position
Scan 3： Adjust brightness
Scan 4： Take a picture

If you set large WD, the focus easily be adjusted
even rough samples. However, the resolution will
decrease.

The image will be focused at
Z axis = 10 mm if the height ofsample and the holder are the same.
In the case of the sample project
over the holder, the image will befocused at
Z = 10 mm ＋ “Projected distance”

Adjust the focus by focus knob at
suitable scan mode, and observe theimages.
If WD deviate from 10 mm after adjusted focus,
adjustment of Z axis is not collect.
Adjust the Z axis at WD 10 mm again.

8Alignment
In the case of observation at high magnification,
you should adjust stigma X/Y and objective aperture.

Low astigmatism
Large astigmatism

・ Adjustment of stigma is need >x5000
observation.
・ Adjustment of objective aperture isneed >x10000 observation
・ Adjust objective aperture after change
the electron beam conditions.
・ Adjust alignment at scan 1 and at morethan twice magnification taking picture.

How to adjust the stigma X/Y
If stigma is out of alignment, the defocused image
have anisotropy (Large astigmatism).
Adjust the stigma X/Y knob so that the defocused
image is blurred a circle.
Click a “Wobbler”, and then the image will be defocused periodically,and you can easily adjust the stigma.

How to adjust the objective aperture X/YWobbler

Click the “Wobbler”, and then confirm whether
observing position shift or not.
If the position shifted, you need toadjust the objective aperture X/Y toprevent the moving.
After adjust the aperture, adjust thefocus and the stigma again.

Objective aperture X/Y9Save images
Freeze scan

Save a image after adjustment ofcontrast and brightness.
Adjust contrast and brightness yourself not only ACB.

Capture image

Text paste

SEM data
display

Scan/AutosaveCancel

Save image

Setting tab

To save image, click a “acquisition”
or put a “Photo”, and then you canget the image.
Check ☑ ”text paste” in the case ofput the information under the image.
If you want to change the content of theinformation added to a photo, select "SEM
data display" in the "Settings" tab under
the software and change conditions.
If there is a charging phenomenon, theimage will be less distorted if you take apicture with scan 2 or scan 3. To shoot with
Scan 2 or Scan 3, select the scan mode andclick “Freeze”

If contamination exist on the sample, thebeam irradiation area will change to dark like aleft image.To prevent the changing image, keep
the sample clean.
To use following methods, the affect ofcontamination will decrease.
• Decrease the electron beam power.
• To adjust the focus and stigma at different
place from the target position for savingimage.
You can change the scan speed with "Scan /Auto Save" in the "Settings" tab under thesoftware. Adjust the settings if there is acharging phenomenon, if you want to take a
lot of photos quickly, if add signals and10
increase the resolution, etc.

Observation of backscattered electron image (BEI)COMPOTOPOCOMPO+TOPO

Changesignal
2 screen modeThis SEM can observe composition
image (COMPO), topographic image(TOPO), and stereoscopic image(COMPO+TOPO) by backscatteredelectron detector besides secondary
electron image (SEI).
To observe BEI, change the signal
and then select suitable mode, andchange to high acceleration voltage
and large current.
•COMPO image：Heavycomposition particles
at deep-depth can beobserved.

TOPO image：Contrastof the right grain andthe left hole isreversed.

SEI⇒TOPO

Contrast of SEI image is refｌected that
information of sample shape.
SEI image is strongly affected bysurface electrification of sample.
The information is gotten from lessthan several nm depth.
•SEI⇒COMPO

Secondary electron image (SEI)

Backscattered electron image (BEI)

Contrast of COMPO image of BEI isreflected that surface composition ofspecimen. A heavy composition isbright and a light composition is dark.
Contrast of TOPO image of BEI isreflected that surface topographicalinformation. Shadow appears likethere is a light source on the right sideof the screen.
The information is gotten from lessthan several μm depth. Also contrast
based on the crystal orientation
appears.
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Other functions of SEM
To click a “Measurement”, you canmeasure the length of target .

Measurement

It is possible to save images on right
4 windows temporarily.

Diameter of objective aperture can bechanged. Small number of the knob means
small diameter of objective aperture, andyou can get small spot size.
Turn a knob after pulled out

If you change the diameter, please turn knob backNo. 2 position after using.

Icons
••
••

Blank
Don’ｔ irradiate electron beam to samples.
STIG reset
Initialize stigma X/Y
LENS reset
Degauss hysteresis of objective lens. Please click before using.
SHIFT reset
Initialize of observing position.

12Low vacuum modeThis SEM can observe and analyze samples
in low vacuum conditions (30 Pa - 270 Pa)
Biological sample, water including sample,
and sample has no electrical conductivity
can be observed without pretreatment.
Please ask the staff if you use low vacuum mode!

A petal of dandelion
Lowvacuummode

Highvacuummode

It is possible to observe only
backscatterd electron images (BEI)in low vacuum condition.

Select to “Low vacuum mode” before thesample into vacuum chamber, and then click the“VENT”. Enter the sample in the chamber and click
the “EVAC”.

VacuumdegreeStartDon’t use “High vacuum mode” when observing
the sample need low vacuum condition! SEM will
be broken by emitｔed gases!
“Vacuum degree” of the chamber can be
adjusted from 30 Pa to 270 Pa. Select the vacuum
degree, and then click ”Start”.
Please wait several minutes after the click.
You can observe SEM after turned on “Ready”.

After finish SEM use, change ”High vacuummode” and click a “EVAC”.
13How to end SEM observation
In the case of using EDS
Save the project folder, and close “Analysis Station”.
Turn off the power of EDS.
power of EDS•

Return the changed parameters.
（Acceleration voltage 10 kV, SS 40, WD 10 mm,
Objective aperture No.2)

Maintenance

Load current•••

SEM software shutdown••
Only exchange sample
・Turn off “HT”
・Return the stage position.
✓ Z axis：more than 25mm
✓ X/Y axis：around 20 mm✓ Rotation / Tilt：0°
・Click the “VENT” to returnthe chamber to air pressure.
・Open the door, and take out
sample holder from the stage
in the chamber.
・ Close the door, andexchange the sample
・ New sample set on thestage. Close the door, andclick the “EVAC”

••
•
•

•

Select "Maintenance" on the lower tab ofthe software and check the load current
valueTurn off “HT”.
Return the stage position.
✓ Z axis：more than 25 mm✓ X/Y axis：around 20 mm✓ Rotation / Tilt：0°
Click the “VENT” to return the chamber to
air pressure.
Open the door, and take out sample holder
from the stage in the chamber.
Close the door, and click the “EVAC” toevacuate the chamber. (If you used low
vacuum mode, return to high pressuremode and click the “EVAC”.)
Reject the sample from SEM holder, andclean the holder, and then the holder into
SEM box.
Data collection(do not use your USB)
After the vacuum state of the chamberchanges to “Ready”, SEM software
shutdown. And PC shutdown. Displays
power off.
Write on the SEM log book.
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