SEM Protocol - Whiting School of Engineering

JSM-6700F Quick Guide
SEM Quick Start Guide
The following instructions are provided as a Quick Start Guide for powering up, running
measurements, and shutting down the Field Emission Scanning Electron Microscope (SEM)
system.
Warning: Scanning Electron Microscopes produce potentially hazardous
ionizing radiation. Only users who have completed the Radiation Safety
section of the DMSE Safety Training, and who have received training by
qualified department staff or faculty are permitted to use this equipment.
Contact the DMSE for training information.
Notice: Italicized words indicate external buttons that can be found in
Figure 1.1 and Figure 2.4. Bolded words indicate computer icons that are
located in Figure 2.3 and Figure 3.1
Table of Contents
SEM Quick Start Guide
Preparing the Sample .....................................................................................................................2
Mounting & Loading............................................................................................................................. 2
Preparing the Machine ...................................................................................................................3
Liquid Nitrogen Setup........................................................................................................................... 3
System Settings .................................................................................................................................... 4
Finding Your Location ........................................................................................................................... 4
Performing Alignments ..................................................................................................................5
Using the Adjustment Knobs ................................................................................................................ 5
Getting Results ..............................................................................................................................5
Taking & Saving Photos ........................................................................................................................ 6
Finishing Up ...................................................................................................................................6
Resetting the SEM ................................................................................................................................ 6
Common Problems ........................................................................................................................6
Preparing the Sample
Mounting & Loading
Notice: Your sample must be electrically conductive in order for the
machine to be properly viewed. Use the SEM Sputter Coater to coat the
surface of any non-conducting sample with Platinum or Carbon.
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Notice: This guide assumes a basic knowledge of mounting. In case:
Use a three side wrap of carbon tape to cover the top, side, and bottom of the sample.
Match the height of the sample to that of the rails on the sample tray.
Wear gloves to prevent the transfer of oil and water into the system.
Figure 1.1: The SEM chamber
controls and stage position
1) Sign into the logbook.
2) Mount your sample.
3) Make sure the VENT light is on and open up the
Figure 1.2: Common terms for
the SEM exterior
chamber with the chamber clip.
4) Place the holder into the chamber.
a. The holder should be orientated to the arrows on the bottom of the holder.
5) Take a picture of your sample to see how the sample will appear on the monitor.
6) Lock the chamber with the chamber clip and press the EVAC button for 2 seconds.
7) Wait until the EVAC light is solid and turn on the left side Robinson Chamber View.
a. The camera can be shown on the monitor by selecting the VLC app.
8) Using the exchange rod and the camera, push the sample all the way into the SEM holder.
a. The handle should be flush and click when on the surface.
9) Put the handle back and press the VENT button for 2 seconds.
10) Turn off the camera and switch back to the SEM app.
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Preparing the Machine
Liquid Nitrogen Setup
Notice: Liquid Nitrogen is an extremely cold substance at -196 °C. Handling
without proper precautions can lead to cold burns, dismemberment, or
asphyxiation. Always remember to use PPE and ensure that air flow is
present when transferring Liquid Nitrogen into the SEM.
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Put on a face shield, insulated gloves, and apron.
Dispense enough N2 to fill the dewar about half-way.
Locate the compartment for filling LN2 on the SEM.
Pour LN2 into the SEM until it overflows.
When finished, take off all PPE.
Figure 2.1: The proper PPE
required to dispense LN2
Dispensing enough N2:
If the top of the compartment
has some frozen condensation
on the outside, fill the SEM
once. If not, fill twice.
Figure 2.2: The compartment
for filling LN2 in the SEM
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Figure 2.3: The location of commonly used icons
System Settings
Click on PVG (Penning Valve Gauge) on the monitor and wait until it reaches ~ 10-4 Pa.
Click on the HT button on the monitor when it turns blue.
Click on the Instrument Control icon on the control bar.
Use the general values below for standard operation:
Accelerating Voltage: 10kV
OL Aperture: 4
Focus: 8mm
Probe Current: 10 μA
Scan Rotation: 0
DFC: 15
Emission: 10 μA
SEI Detector: On
Mode: 2
5) Set your detector:
a. For a WD/Focus of 8mm, use the LEI detector. Else, use the SEI detector.
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Finding Your Location
Figure 2.4: The control panel for the SEM. A green light means that the function is engaged.
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1) Click on Low Mag mode on the control panel to enter
low magnification.
2) Make sure to zoom out (CCW) to the minimum
magnification using the Zoom knob.
3) Press RDC IMG on the control panel.
4) Adjust the Focus knob until the picture is crispest.
5) Use the joystick or the right mouse button to move the
screen with the joystick.
6) Use the picture from earlier to move to the location
that is to be analyzed.
7) Place the object of interest in the middle of the screen.
8) Click on Low Mag mode to exit low magnification.
Figure 2.5: The joystick for
the SEM.
Performing Alignments
Using the Adjustment Knobs
1) Make sure to zoom out to the minimum magnification using the
Zoom knob.
2) Adjust the Focus knob until the picture is crispest.
3) Zoom to 3000X using the Zoom knob (CW).
4) Adjust the Focus & the X and Y Stigmation knob until the picture is
crispest.
5) Press Align on the control panel.
6) Adjust the Gun Alignment:
a. First, increase the Probe Current to ~ 13. Rotate the X or
Y knob clockwise until the picture turns black. Note the
number and rotate counterclockwise while noting that
number. Rotate the knob to the average of the numbers.
Repeat with the other directional knob.
7) Press Wobble and adjust the OL Aperture:
a. The image will either be moving in the X, Y or X+Y axis.
If the image is moving primarily in the X axis, adjust the X
knob. Repeat with the other knob if necessary until the
image is stabilized.
8) Zoom to the magnification desired.
Anytime you adjust an alignment or zoom, adjust:
• X, Y Stigmation
• Focus
Note: The alignments need to only be done once.
Figure 3.1: The
alignment menu.
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Getting Results
Taking & Saving Photos
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Press the ACB button.
Rotate the Contrast knob CCW until the image goes off screen.
Rotate the Brightness knob CCW until the screen is black.
Rotate the Brightness knob CW until the first shade of gray appears.
Adjust the Contrast knob until the image shows a balance of white and black.
When you have focused on the area you want to capture and made it crispest, press the
Photo button.
7) Click on Save & Export to save your images into a folder.
8) Press the lighted FREEZE button to unfreeze the screen.
Finishing Up
Resetting the SEM
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Turn off beam by clicking the HT button.
Press the Exchange button in the Exchange icon.
Turn on the camera and VLC app on the monitor.
Press on the EVAC button for 2 seconds. Wait until it stops blinking.
Pull the sample out by pushing the sample exchange rod all the way in and pulling it out.
Press on the VENT button for 2 seconds. Wait until it stops blinking.
Unlock the chamber and take out the samples.
Lock the chamber.
Turn off the camera.
Common Problems
Notice: For any problems not covered under this section, contact Bryan
Crawford at (865) 257-3564 or [email protected].
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The beam is on and the picture is too bright.
o First, ensure that the camera is turned off. Check that the Probe Current is around
10 μA. Redo the adjustments for brightness and contrast.
The machine beeps when I try to move the sample.
o Be sure to check that the EXCHANGE light is lit. If the EXCHANGE light is not
lit, slowly rotate Working Distance Knob to ~ 80 mm until it is.
No image displays when HT is turned on.
o Check that the FREEZE button is not lit. If it is, press the FREEZE button.
The image is blurry.
o Redo all stigmations, alignments, and image correction methods.
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