osiris tem cheat sheet

OSIRIS TEM CHEAT SHEET
V.5
FIRST
Check that the high voltage is on: From the “go away” tab, look at the “High Tension” menu. The HIGH
TENSION button should be yellow, and the OPERATE button should be yellow.
If the voltage is not on, check the vacuum level and then turn it on. It will take just a few minutes for the
voltage to go up to 200 kV.
SECOND
Check the liquid nitrogen level from the SETUP tab. If you are going to use the xray detector, then you
will need liquid nitrogen. Otherwise, you do not. If you put nitrogen in the dewar, please fill it all the
way up.
LOADING
Line up the pin (the one near the end of
the rod) with the line labeled “close”, or
even a bit further counter-clockwise, at
~3:30
Insert the rod until it stops, turning it a
bit CLOCKWISE as you go. Do not turn it
the other way; that would be bad.
THE BLUE LINE ON THE ROD SHOULD
BE AT THE END OF THE HOLE!
Now you can let go. The rod might turn
slightly counter-clockwise, so remain
calm.
Inserting the rod will start the pump.
IF you are using the double-tilt holder,
then plug in the cable, placing the wire
up and over the holder.
Go over to the computer console and look at the message box.
Press the
button to clear away any previous messages. Ignore messages about the liquid
nitrogen level. Instead, check the liquid nitrogen level from the Vacuum Status box.
The message box should then ask you to choose a specimen holder. You are probably using the singletilt holder, so choose that one, then click on
IF you are using the double-tilt holder then click on
again to confirm that you have plugged in
the cable:
If you see the message “pumping sequence aborted” you can ignore it and click
message appears if you insert the rod slowly enough to double-hit the sensor
the pump.
again. That
that starts
Wait for the light (next to the sample rod) to go out. You will hear a click when the vacuum system
switches over to the turbo pump. Soon after, the light will go out. You can think of the light as meaning
“not ready”.
Seriously, do not rotate the rod until the light goes out. You could dump the vacuum, which would ruin
your day. It is NOT interlocked, so watch out!
Turn the holder counter-clock-wise and let it slip in the rest of the way.
DO NOT PUSH THE ROD. You should be holding
it back a little while the vacuum pulls it in. If you
think you should push then you are
doing it wrong. GET HELP!
Wiggle the rod a little to make sure it is seated
well, then tap on the end twice.
TURNING ON THE BEAM
Workset  Setup  Vacuum  Col. Valves
Click to open the valves.
On any button a yellow background means “this is the current
state”. So the button shown here on the right tells you that
the column valves are currently closed.
Load standard TEM conditions with
Workset  Setup  FEG Registers  TEM200Kv
then click on “Set”.
Do NOT click on “update”, “delete”, or “add”.
If you get an error message saying you can’t do this without
being in the “operate” mode, then this means the high voltage
is off (which happens whenever the pressure goes too high).
In that case, ask for help to get the high voltage back on.
Pull out the objective and “selected area” apertures, if either
of them are currently inserted. You might need these
apertures later, but for now, pull them out with
Workset  Tune  Apertures  Objective
Press the “Eucentric Focus”
button on the right knob panel.
Find your sample! Lower the magnification to M-2300 (or lower, although the LM range can be
annoying.) If the image is black, try using the joystick to move away from copper grid lines.
Set eucentric height:
Workset  Search  Stage Flapout
Set a wobble amplitude of 5° then click on “wobbler”.
Use the Z axis buttons on the right panel to minimize the
image shift. For most samples this will be at a Z value
between -40 and -80 um. Note that the contrast also
decreases when you reach the eucentric height.
BEAM ALIGNMENTS
Look at some features on your sample, and increase the magnification into the SA range.
Set the focus for MINIMUM contrast.
Lower knob = sensitivity
Upper knob = focus
Check condenser centering:
Use Intensity knob (counter-clockwise) to condense the beam to its minimum size.
Use the trackball to center the spot on the circular target.
Expand the beam with the intensity knob (clockwise) out to the larger circle.
If the beam does meet the circle evenly, you should adjust the C2 aperture position
Adjust the C2 condenser position by using
Workset  Tune  Apertures
and then click on
Condenser 2 Adjust
The multifunction knobs will now control the condenser aperture. Move the aperture so that
the expanded beam lines up with the outer circle. Then condense the beam to minimum, and
iterate if necessary.
Check condenser stigmation
Look for a circular spot at the intensity crossover (use the Intensity knob).
If the crossover is elliptical or weirdly shaped instead of round, then we need to adjust
the condenser stigmation.
Ask for help if the condenser needs adjustment.
Always leave the Intensity knob set so that the beam spreads when the knob is turned
clockwise.
Focus and Objective Stigmation
The screen is down, right? If not, use R1 to lower the screen.
Set the magnification into the “SA” range, about 39kx.
Set focus
for minimum contrast.
Use the Intensity knob to condense the beam, and use the trackball to center it.
Spread the beam by turning the Intensity knob clockwise.
Find some amorphous material to view.
Raise the screen with R1
Turn on the camera with
Workset  Camera  CCD/TV  Search
(This should insert the camera automatically, so you
do not need to click on “insert”.)
Click on Live FFT
Go a bit out of focus, to see rings in the FFT.
Condense the beam a bit (counter-clockwise) if the
rings are unclear.
Press the Stigmator
button on the left panel,
or find it on the Tune tab. The multifunction knobs
now control the objective stigmation.
Look at the FFT. The best focus is when all the rings spread out and disappear. But we need a
few rings to check stigmation.
The multifunction knobs are controlling objective stigmation, right? Use those knobs to make
the FFT rings more circular. Adjust the focus closer to ideal (no rings) and adjust the stigmation
again. Iterate until you are happy. Or, less sad.
When you are done with stigmation, it’s smart to click on None so you will not accidentally
change the stigmators by turning the multifunction knobs.
Take some pictures already!
Find an interesting region, with the screen down (that is, using the flucam)
Lift the screen with
R1
Workset  Camera  CCD/TV  Acquire
Look at the integration time for image acquisition. If the image is not drifting, then use 1
second. If the image is drifting slightly, use 0.25 seconds.
If the image is drifting rapidly, try tapping on the sample rod again. Or, you might just have to
wait 20 minutes or so for the sample to reach equilibrium.
Save the image on the support PC (“TecnaiD601PC”) in your own directory.
Move your image files to the YINQE server (there is a shortcut on the PC desktop) or use a web
browser to dump them into your Yale Box account.
The support PC is NOT backed up. Files on the support PC will be deleted randomly, without
notice.
STEM OPERATION FOR XRAY MAPPING
If you are looking at a crystal, use TEM mode first to set the alpha and beta tilt.
In TEM mode, position the sample over an open region. Later we will need to view an amorphous
region, such as carbon film or glue. Set the magnification somewhere in the M or SA range, so that
you’ll see an edge of the sample when you switch to STEM mode.
Load standard STEM conditions with
Workset  Setup  FEG Registers  EDSSTEM200Kv
and click on “Set”.
In the STEM Detector box, make sure the HAADF camera length is
set to 220 mm.
Do you need to do any alignments? Probably not!
But let’s just do a quick check:
Press the “eucentric focus” button on the right panel.
Lower the magnification. Your sample will be out of focus.
Focus with the Z buttons. This will be a “coarse” focus. Fine focusing can be done with the
“focus” knob.
Zoom in on your sample and look for astigmatism just as you would on a SEM. Pressing the
“stigmator” button will attach the multifunction knobs to the condenser stigmation control.
XRAY SPECTROSCOPY
You don’t need to use STEM mode to get an x-ray spectrum! If you do not care about resolution, then
simply condense the beam on a region of interest and grab a quick and dirty spectrum.
Turn on the x-ray detector with
Workset  STEM  Super X EDX
Pulse processor  On
 Acquire
The spectrum should appear in the TIA window, on the right. After a few seconds you can click on
Acquire again to stop. Did you see that count rate? Pretty amazing.
IF you are starting from STEM mode, then acquire a STEM image and freeze it.
Move the reference point
to a place of interest on the image
Super X EDX  Acquire
Now the spectrum should appear on the TIA window.
To identify the elements, choose “EDX Quant” on the left side of the TIA window
and then click on “Peak ID”.
XRAY MAPPING
First get STEM mode running, so you can use the x-ray detector while scanning the beam. If you need a
high count-rate, then choose the FEG Register “EDSSTEM200Kv” instead of the high-resolution register
“STEM200Kv”.
Refer to the section “STEM Operation” above for aligning the column.
You probably do not have to…
Turn on the x-ray detector with
Workset  STEM  Super X EDX
Pulse processor  On
Esprit is probably running already – look on the task bar. If not…
Fire up Esprit from the lower-left icon tray
Click on Login. The user name and password are both “edx”.
Click on Hypermap
New
Image stabilization!
Acquire
Acquire again to stop
Click on the little bed
icon that is supposed to
look like a periodic
table.
Choose two or three elements to display in the xray map
Click on Acquire
Of course there are all sorts of parameters you can set. Feel free to poke around Esprit.
Esprit has a very strange menu structure. Many important functions, such as “save” can be found by
clicking on
Once you have an xray map, you can have Esprit display an average spectrum of selected regions. Use
the eye dropper (lower right) to select a region and then click on the “Spectrum” tab to see the
averaged spectrum. Who would have guessed to use the eye dropper!
Use the “Auto” button next to the periodic table to identify elements in the spectrum.
Be sure to save
The composite image
The individual images
The complete database
WHEN YOU ARE DONE
0. Delete all images in TIA, using window  close all
1. If you are in STEM mode, go back to TEM mode using the FEG Register box.
2. Remove the objective and SA apertures, if necessary
3. Lower the screen with R1
4. Close the column valves with
Workset  Setup  Vacuum 
Col. Valves Closed
5. Reset the stage with
Workset  Search  Stage
Reset Holder
This is very important, to avoid
breaking the rod as your remove it.
6. Remove the sample rod (see below)
7. Remove your sample
8. Leave the rod in the plasma cleaner, pumping.
9. Log out of Badger (unless you want to spend lots of money)
REMOVING SAMPLE ROD
1. RESET THE STAGE
Workset  Search Stage  Flapout  Reset Holder
2. Pull the rod straight out until it stops, about 3 inches.
You’ll see the blue line on the rod.
Turn the rod clockwise until it stops – GENTLY
3. Very gently pull the holder out a little way more,
until it pops loose from vacuum.
5. Pull the rod out the rest of the way. Try to avoid hitting
anything on the way out.
Leave the rod pumping in the plasma cleaner.
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