Professional Documents
Culture Documents
SOP - SEM - Nova 230
SOP - SEM - Nova 230
SOP - SEM - Nova 230
1|Pag e
System Overview:
The Nova 230 NanoSEM Scanning Electron Microscope (SEM) produces enlarged images of a variety of
samples, achieving magnifications of over 500 000x providing ultra-high resolution imaging in a digital
format. This important and widely used analytical tool provides exceptional depth of field, minimal
sample preparation, and the combination with X-ray microanalysis (EDS) and Raman spectroscopy. The
Nova 230 NanoSEM has 2 operating vacuum modes to deal with different types of sample. High Vacuum
(HiVac) is the conventional operating mode associated with all scanning electron microscopes. The other
application mode is Low Vacuum (LoVac). In this mode the column is under high vacuum, and the
sample chamber is at a high pressure ranging from 0.075 to 1,5 Torr (10 to 200 Pa). This mode can use
water vapor from a built-in water reservoir, or auxiliary gas which is supplied by the user, and connected
to a gas inlet provided for this purpose. Using the Low Vacuum mode observation of outgassing or highly
charging materials can be made without the need to metal coat the sample, which would be necessary
for conventional High Vacuum mode. See Appendix 1 for an explanation of how the Nova NanoSEM
works.
2|Pag e
Important Hardware Components
Sample
Chamber
Manual User
Interface (UI)
Column
Pole Piece
Inside Sample
Chamber Backscattered Detector
BSED or GAD
ETD Detector
3|Pag e
Software Description with Important User Interface (UI) Elements
xT microscope Server starts and stops the basic microscope functions and makes it possible to open and
close the xT microscope Control UI (User Interface) application which in turn controls system functions
including detection and analysis, scanning, image gathering, manipulation and output, magnification and
vacuum, etc.
xT microscope server application should overlay Titlebar (1) of the xT microscope Control UI (as shown)
Vacuum Module
Column Module
4|Pag e
SEM Operation Protocol
1. Before starting your session, make sure microscope PC and
support PC are turned on (microscope PC controls SEM while
support PC is where you allowed to save your images and from
where you retrieve them after you finished your session using
the USB key). PLUGGING YOUR USB KEY INTO THE
MICROSCOPE PC IS STRICTLY FORBIDDEN!
2. Make sure that the SEM is in operational condition. The
assumption is that the xT microscope Control UI window is fully
maximized on the monitor. At the bottom right corner of the
xT microscope Control UI, the chamber and column should be
green and the small panel above the HV button is green.
3. Make a record in the Main Logbook, including your name, account information and start time. If
you are the first person using the SEM for the day, record vacuum gage and emission current
readings in Vacuum System Logbook. Keep in mind it is safe to use the SEM when both controls
are green color, however, you should report when the vacuum reading of the first gauge is
higher than 3·10-7Pa, second 4·10-5 Pa, the third and fours are not critical, and finally emission
current shouldn’t change faster than 4 μA per day.
4. Make sure the color of the high voltage (HV) button in the Column module is not yellow, which
indicates high voltage is turned OFF. If HV button is yellow (voltage is turned on), CLICK it to
switch HV off. When clicked, the HV button color will become colorless and the HV will be off.
OFF: ON:
5. Before the vent/pump the chamber make sure that the EDS
detector is withdrawn. Refer to the Apendix 8.
6. To vent the chamber. In the Vacuum module, CLICK the VENT
button.
Click YES when the confirmation dialogue window pops up.
7. Venting will take about 1 to 2 minutes. Once finished, the
sample chamber can be opened. There is no indication on
when it is ok to open the door just give it ampel time. If you
need to apply too much force to open the chamber door give
it more time for venting.
8. Remove all stored user positions by selecting Navigation Page and clicking
CLEAR in the Stage Module on the Map Tab (circled in red). Make sure the
lower right quadrant, which shows the infrared image of the chamber is live
(unpaused). If paused (denoted by the green pause icon in the upper right
corner of the infrared image window), click the window so that it has a blue
5|Pag e
border). Press the pause button in the Toolbar to unpause:
11. Use metal tool 9, Appendix 5 (“elephant”) to measure the height of your
sample. Place the elephant on the flat horizontal area of the stage near
to the stage adapter. Make sure that the elephant is leveled horizontally.
Your sample highest point should not exceed the height of the elephant
tip, as shown by the red arrow. If sample is too high, follow the
prosedure described in the Appendix 2.
12. When the pin stub with your sample is in the holder correctly, tighten set screw in stage adapter
head with 1.5 mm hex wrench (tool 10, Appendix 5) (finger tight, do not over tighten!) that
always resides near the sample chamber. To see the image of your sample on the computer
screen in proper orientation remember that the SEM door is parallel to the “Y” axis of the
computer screen.
13. Your defolt detector is ETD (secondury electrons detector in HiVac mode). It is always in place.
All other detectors should be installed prior to operation and removed after the session is over.
Install appropriate detector LVD, BSED or GAD (with gloves!). If using variable pressure, use LVD
or GAD detector, which is identified by a very prominent conical Pressure Limiting Aperture
(circled in red). Install the detector by gently positioning detector at the bottom of the column
(Pole Piece) rotating it
such that the final
position of the
detector is as shown
by the green arrow.
(For more details see
6|Pag e
the Appendix 3)
14. Close the chamber door slowly. Do not slam door! Monitor lower
right quadrant on the screen that shows the live infrared image of
the chamber (make sure there is no green pause button in the
image window). Make sure that as the door is closed, no part of the
sample, sample holder, or stage is above the yellow 5mm marker on
the live infrared image. At all times, you must keep your working
distance greater than 5 mm.
16. Once door is fully closed, click the Pump button in the Vacuum module. The pressure of the
chamber can be monitored in the Status module.
17. Select the appropriate accelerating voltage in the Column
module. For Spot size, choose 3 or 4. For organic samples,
choose 1-10kV. For metal samples 10-20kV.
For low vacuum, scan rate should be ~3µs. In high vacuum, scan rate is much less at ~0.1µs.
19. Select lowest magnification (~32X) by rotating
counter-clockwise the magnification knob on
the manual UI on the desk.
20. Click Detector in the Menu Bar and select the appropriate detector. The checkmark
should be next to LVD for low vacuum and ETD for high vacuum.
21. Make sure in the Status module that the chamber icon is green, which means the
7|Pag e
system is ready to have the high voltage (HV) turned ON.
8|Pag e
34. Vent the chamber (click Vent in the Vacuum module).
35. Check live infrared image window to make sure cable for detector hasn’t wound around sample.
If it has, move stage so that it is freed. Lower stage, if needed.
36. Slowly open chamber door while monitoring the live infrared image. Remove sample with the
hex wrench from stub holder.
37. Insert another sample if needed. Otherwise, close the chamber door.
38. In Vacuum module, select High Vacuum. Make sure the EDS detector is completely withdrawn.
(Refer to the Apendix 8). Then click Pump to start pumping system. NEVER KEEP THE SEM DOOR
OPEN LONGER THAN IT IS NESSASRLY TO REPACE THE SAMPLE. Wait until the vacuum system
achieve its target pressure. Do not leave SEM room without pumping system to High Vacuum.
When the SEM is not in use it should be always pumped to the HiVac.
39. Use SwitchBox to switch over to Support PC and copy files onto your USB drive. After images
have successfully been copied, eject USB drive.
40. Once session is completed, finish filling out logbook and calculate SEM session time. Leave SEM
room as clean as it was before your session started!
9|Pag e
Appendix 1: How Nova NanoSEM Works
•Aperture: The strip is made from a Mo coated Si. It has several small exchangeable holes (30, 30, 40, 50
100µm). It enables to choose the aperture most applicable to your imaging needs. Its function is to limit
the angular width of the electron beam in order to reduce lens aberration effect (through control of the
aperture angle) and to improve depth-of-field in the image.
•Sample Chamber This is large evacuated space below the objective lens contains the sample stage
with all its motions, the electron signal detector, the x-ray detector, and a pumping line. •Detection unit
Electrons striking the sample react with its surface producing three basic types of signal: backscatter
electrons, secondary electrons and X-rays. The detection system picks up these signals, converts it into
an amplified electrical signal which is sent to the control PC and displayed on the monitor.
10 | P a g e
Appendix 2: Adjustment of the height on the stage adapter This operation can be performed whith the
gloves on only!
1. Using 1.5mm allen wrench (tool 10, see appendix 5) loose (just a half turn is fine, you don’t need to
remove it!) the set screw (1) on the stage adapter head (2) and remove the sample (pin stub) from
the stage adapter (2). If there is no sample/stub in the stage adapter proceed to the Step 2.
2. Loose the cone (3) by turning it in anti clockwise direction. Never attempt to adjust position of the
stage adapter without performing this step! It can creat a seriouse damage of the stage adapter
and the stage platform.
3. Hold the cone (3) with one hand and rotate the stage adapter head (2) clockwise to lower the stage
adapter; or counter clockwise to raise it.
4. After the height is fixed properly make sure you position the stage adapter head (2) so that the set
screw (1) is facing you. It will make your easy access of the set screw to be fixed with the 1.5mm
allen wrench (tool 10, Appendix 5) after you put the pin stub in place on the top hole (4) of the stage
adapter head. Do not overtight the set screw (1)! Be aware that the set screw has teflon tip, so it
really makes “soft”
5. Now you can fix the cone (3) on the stage platform (5). Do not over tight it; just tight enough not to
feel the stage adapter is loose on the stage platform! Be aware, if you need to use exessive force it
means you doing something wrong! It is pretty much true at each step.
6. Don’t forget to check the sample height using the “elephant” (Step 10 Full Operation Protocol).
7. Here are few tips you can follow up to make it last longer than it was last time You don't need to
completely unscrew the set screw and let it go from the head of the stage adapter. If you do it you
the set screw can fall down and you can lose it. Try to keep it always in. At the same time it
4
2 1
3
5
11 | P a g e
shouldn't be all the way inside of the stage adapter head. It should leave enough space for the pin of
the stub to be inserted. Don't enforce the pin stub into the head of the stage adapter. If you need to
enforce it, it means that the set screw is advanced too much and it doesn't let the pine of the stub to
be inserted inside of the head of the stage adapter. If you feel that the pin doesn't go easily inside
of the stage adapter head unscrew the set screw a little bit more to open the pass for the pin. Also
keep in mind that the tip of the set screw is made of Teflon and it can be broken by the pin of the
stub if the set screw is advanced too far into the head of the stage adapter. The "golden rule" is
keeping the set screw steaking out of the head of the stage adapter at about 1.5-2mm before you
place the stub pin into the stage adapter. After all you don't need to overtight the set crew when
you secure the stub pin inside of the stage adapter head.
12 | P a g e
Appendix 3: Backscattered Detectors Storage Fixture
There are two backscattered detectors on Nova 230 SEM which can be used in different
operating modes: BSED detector for the high vacuum mode operation and Gaseous Analytical
Detector (GAD) for the high pressure (low vacuum) mode. Both detectors operate on exactly the
same principles, but they are slightly different by their design. GAD detector has copper
collimator placed on the opening of the detector. Such collimator reduces the “skirt effect” of
electron beam, when SEM operates in low vacuum.
Both detectors are attached to the storage fixture exactly the same way they get attached to the
pole piece when you use the detectors. To remove the detector from the fixture you need to
turn it about 20 deg clockwise and pull it forward. To return it back you do the opposite
procedure. Always return detectors to the fixture after you finish your operation. Never
disconnect the detectors from the outlet.
Pole-piece
ETD
BSED GAD
outlet
collimator
13 | P a g e
There are two different orientations the backscattered detector can be installed on the pole
piece. Keep in mind that both work fine for the imaging purpose. However, if you need to
perform the EDS, incorrect orientation of backscattered detector can block the X-Ray signal from
reachin the EDS detector. For that reason make sure that the bulk copper part (arrowed) of
detector’s body is installed at about 7-8 o’clock (when your watch is below and facing the pole
piece).
14 | P a g e
Appendix 4: Fast Track SOP
2) Verify that the electron beam is off. High Voltage (HV) control is not yellow color.
3) If you are first person for the day using the SEM (if you are not the first, still checkit) make the day
record of the vacuum system satutus and the beam currrent in the “Vacuum System Log book”.
4) Before venting/pumping the SEM chamber make sure the EDS detector is fully withdrawn. Refer to
the Apendix 8.
5) Vent the SEM chamber; You have to do it after you have your sample placed on the SEM stub.
6) Blow away the dust and fine debries from the surface of your sample before placing it in the SEM
chamber! Loose samples (particles) are not allowed in the SEM chamber! Blowing the dust and debries
from your sample is very critical for cleaved semiconductors since their cleavage can leave sharp debries
on the wafer which can seriosly damage the EDS detector during the SEM chamber pumping!
7) Check the hight of the sample before closing the chamber door!
8) After reassuring that the EDS detector is completely withdrawn (A.8) you can strat pumping the
chamber.
9) When the chamber icon turned green on the UI, HV control become available.
18) Before you turn the SEM off you have to return all advanced setting to their initial condition.
21) Take your sample out. Close the door of the chamber and pump the system to high vacuum.
15 | P a g e
Appendix 5: Tools and their regular location.
While using the SEM it is important to keep all the tools and consumables in place. Please refer to the
images in this appendix to identify the tools and their regular location in the lab. It is a curtesy to place
the tools on their place after you finish your job. All tools which are not shown on those images should
be stored in the blue tool box on the sample preparation desk.
1 – carbon tape;
2 – sample preparation
block;
3 – sissors;
4 – allen wrench to be used
8 with the tool 2 (not on the
SEM!);
5 – twizzors for handling
small SEM stubs (can be
also on the SEM desk);
7 6 – screw driver;
1 2 7 – container for the used
3 4 stubs;
5 6 8 – tools box;
9
10
16 | P a g e
Appendix 6: Saving your images.
1. After you take the image you get computer window with the prompt to save the image. If you just
click OK the image will be saved in the previouse user’s folder. For that not to happened go one level up.
Most likely you’ll get to the existed month (current) folder. Creat your own folder putting your name
and correct job number. Also when you save your image make sure that the window boxes for the Data
Bar and Embeded Graphics of your image are checked. Otherwise they will not be saved with your
image. Usually those two boxes on the Save window are always checked unless someone uncheck them
by mistake.
2. If you accidentally lost the established pass to save your image in correct place (it will be saved on the
support computer) use the following pass in the Save window:
My Network/ Shared Data on 192.168.0.2/current year/current month
There is a Shared Data folder on the C drive of the support computer where your results got saved. In
addition there is a shortcut folder to the current month on the Desktop of support computer where your
data can be found.
3. C drive of the support computer has ability to store the results from the main computer. However its
capasity is limited and usually we don’t have possibility to store there results from more than two
month of operation (it depends on the numbed of the images created). When the C drive gets
completely full you don’t have possibility to take/save your images. To fix this situation you can go to
the C drive and move previouse month results folder to the D drive. On the D drive you can see the
current year folder. That is the place where you can transfer the data from the previouse month
operation.
17 | P a g e
Appendix 7: EDS spectrometer SOP
Please refer to the A.8 to set up the operating position for the EDS detector. Make sure that the
detector is completely withdrawn when you need to pump/vent the SEM chamber
1. Obtain the desired image in the upper left quadrant window. Ensure that this image is unpaused.
2. Make sure that the live-camera of the chamber (lower right quadrant) is now paused because the IR
radiation is in conflict with EDS detector giving overwhelmingly strong zero-peak.
3. The EDS software is run on its own computer located on the floor and labeled EDS computer. Turn
this computer on and log in as User (password: user). After you finish your job, turn off this
computer, don’t keep it on when not in use.
4. After logging in, open the NSS software.
5. If you are a new user, go to the project explorer. In the “Users” subfolder, create a new project
folder and rename it with your name. (Note: The new project folders are green, not yellow). All your
saved data will be stored in the computer’s “C: drive” -> “Users” -> [Your folder].
6. To collect the spectra for your sample, click the “Spectrum” button on the left-sided toolbar
(Microanalysis Panel). Then hit the black play button to collect spectra from the sample. Notice the
two parameters on the bottom right taskbar: DT (Dead Time) and SR (counts rate). Optimal
conditions are when DT is under 30% and SR greater than 1000. Both could be adjusted by changing
the Spot Size on the SEM computer.
7. After you are satisfied with the result, click the black stop button. Then hit the “quantify spectra”
button. To save your report, click the “Export to Word” button in the toolbar. This will open a word
document and automatically export your data and spectra.
8. The next operations below “Spectrum” on the Microanalysis Panel will allow you to collect point,
line, or rectangular spectrum on specific locations on your sample. First, click the “acquire image”
button on the toolbar. Then click the point directly on the image where you would like to collect the
spectrum. Keep in mind that the spatial resolution of collected signal is roughly 1µm3 no matter
how small is the point you choose on the image. When satisfied with the results, click the “stop”
button and “quantify results” button. You can collect multiple spectra on your sample, just
remember to hit the “play, stop, and quantify results” buttons between each spectra.
9. The next operation will allow you to obtain an elemental mapping of where each identified element
is located on your image. Similarly, click the “acquire image” button. Then hit play. Elements on the
periodic table can be adjusted so that you show/hide the specific elements in which you are
interested.
10. Quantify results and export to Word when you are finished. Save your work and close the NSS
software.
11. Copy your data with a USB from the C: Drive under “Users” and search for your folder.
12. Turn off the computer when you are finished using EDS.
18 | P a g e
Appendix 8. EDS detector inserting/withdrawal
Be aware that the SOP has been modified due to a new operation protocol active regardless the EDS
detector use. Make sure that the EDS detector is fully withdrawn during the pumping/venting
procedure on the SEM. That should be done to prevent the possible damage of the EDS detector
window. The window is made of thin polymer (formvar) and it can be easily damaged by the sharp micro
size debris that flies inside the chamber during the pumping/venting chamber procedure. Every time
you vent or pump the chamber make sure that EDS detector is fully withdrawn. To find out correct
position of the detector please refer to the following guidance supplied with the images.
A. The EDS detector position identification. It can be recognized using the infrared (IR) camera image
(SEM chamber inner view) on the main computer: User Interface (UI), quad 4 (refer to the main SOP
text). Figure 8.1 A, B. The second more accurate way to identify the correct operating position of the
EDS detector involves the use of the EDS detector translation mechanism scale (ruler). To proceed with
this way please identify the location of the EDS detector chamber, which is located behind the SEM
chamber and can be recognized by the red label Thermo Figure 8.1 E. The EDS position scale can be seen
right below the vacuum bellows. In the operating position the EDS chamber edge should be at 5.0
(Figure 8.1 C) and when the detector is completely withdrawn it should be at 7.2, Figure 8.1 D.
B. The EDS detector withdrawal from the operating position. Please identify a chrome knob about 1
inch in diameter on the back side of the EDS detector chamber (Figure 8.1 F). Rotate this knob in the
clockwise direction. Please proceed until it stops. The translation mechanism ruler should show about
7.2. You can also see the probe of the EDS detector is practically not shown in the IR camera image
(Figure 8.1 A) Now it is safe to vent or pump the SEM chamber.
C. Placing the EDS detector to the operating position. Such position is shown in Figure 8.1 B. You need
to do so only if you consider to perform the EDS chemical analysis of you sample. Otherwise it is
absolutely safe to operate the SEM with the EDS detector completely withdrawn like it is shown in
Figure 8.1 A. To place the detector into operating position, rotate the chrome knob of the EDS detector
translation mechanism in the counterclockwise direction until it stops. The translation mechanism ruler
should show about 5.0 (Figure 8.1 C).
19 | P a g e
20 | P a g e