Standard Operating Procedure: SEM

Contents

Hardware Description and Principle of Operation ....................................................................................... 1

Procedure...................................................................................................................................................... 1
Emergency Stop ............................................................................................................................................ 5
Allowed Activities.......................................................................................................................................... 6
Disallowed Activities ..................................................................................................................................... 6
What to watch out for during operation ...................................................................................................... 6
Common Troubleshooting Tips ..................................................................................................................... 6
When to call staff? ........................................................................................................................................ 6
Badger Criteria .............................................................................................................................................. 7
 Standard Operating Procedure: SEM
Hardware Description and Principle of Operation
Nova NanoSEM 450

The Nova Scanning Electron Microscope (SEM) is a high resolution scanning electron microscope
intended for sample characterization. In addition to the powerful combination of advanced optics
(including a two-mode final lens), SE/BSE (Secondary Electrons/Backscattered Electrons) in-lens
detection and beam deceleration, the Nova NanoSEM 450 series introduces a new suite of latest
generation, high sensitivity, retractable SE/BSE and STEM detectors, as well as versatile SE/BSE
filtering capabilities, to best optimize the information of interest. Intelligent scanning modes are
available to minimize imaging artifacts.

Material Requirements
Equipment: substrate, sample holder, clips or carbon tape and tweezers

Personal Protective Equipment: nitrile gloves and face mask

Procedure
Estimated Time: ~25 min to prep/load/unload + imaging time

Sample Preparation

1. If the sample is nonconductive (plastic, fiber, polymer or other substance with an electrical
resistance greater than 1010 ohms) the specimen can be coated with a thin layer (~10-15
nm) of gold using the Cressington sputter coater. This conductive layer will help to reduce
sample charging and improve image quality. If no coating is desired as it might alter the
specimen, “Low Vacuum” mode can be used to stabilize the specimen for observation.
2. Mount the sample on a sample holder using carbon tape, or if the holder has clips, tighten
the clip with a screwdriver to secure the sample. Be sure the clip holds the sample securely
and that the clip is not obscuring any area that you intend to image. The specimen must
be electrically grounded to the sample holder to minimize specimen charging.
3. Insert the stub of the sample holder into the specimen holder and secure the stub with a
hex-wrench.

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 Standard Operating Procedure: SEM
4. Check whether the sample will fit through the load lock door using the
load lock door emulator. If the sample is small enough to fit through
the load lock door, then you can use the load lock procedure to
load the sample. If the sample is too big, then you will have to
vent the main chamber door.

Load Sample – Load Lock

1. Vent the load lock by pressing the button labeled V (vent) and then lift and swing
open the load lock lid.
2. Place the sample on the carrier in the load lock and then insert the rod into the
sample carrier compressing the spring on the rod. While holding it in place, turn
the manipulator to lock the carrier in place and then place the rod into the
parking position to prevent the rod from slowly creeping forwards.
3. Close the load lock lid and press the button labeled P (pump), which will pump
the load lock and move the stage into the loading position. Once the load lock
is pumped and the stage is in place, the OK button will light up and the gate
valve interlock will release allowing the door to the main chamber to be
opened.
4. Turn the gate valve knob from LOCK to UNLOCK and then carefully pull the
knob bar fully out from the first mark to the second mark. Turn the gate valve
knob from UNLOCK to LOCK.
5. Move the loading rod from the parking position and into the chamber until the sample
carrier engages with stage at the end of travel. Turn the rod counterclockwise to the base
of the slot, pull the rod to the back of the slot, turn it clockwise out of the slot and then
withdraw it back to the parking slot.
6. Close the gate valve by turning the knob bar to the UNLOCK position, pressing the knob
in to engage the valve over the opening and then turn the knob to the LOCK position to
secure it. Leave the load lock under vacuum.

Load Sample – Main Chamber Door

1. Click the Vent button and then click Yes when the confirmation box appears. This will
begin venting the chamber and move the stage into position. Venting will take around 5
minutes to complete. There is no pressure gauge that will read when the chamber is at
atmosphere so you will simply have to wait and then try opening it.

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 Standard Operating Procedure: SEM
2. Once the chamber has finished venting, open the specimen chamber and insert the
specimen holder with sample into the slot on the stage.
3. Close the specimen chamber. Check to see that the proper vacuum mode is selected and
click the Pump button.

Stage Movement – Nav-Cam Photo

1. Select the Stage menu, select Take Nav-Cam Photo. If the function does not work, try
clicking on the Nav-Cam quad (Quad 3) and then try again. Or instead of selecting Take
Nav-Cam Photo, select Move Stage to Nav-Cam and once the stage has moved into
position select Take Nav-Cam Photo.
2. Once the Nav-Cam photo is acquired, it can be used for navigating in the x- and y-plane.
Either drag the cross over a desired feature in the image of the sample, or double click on
a feature and the stage will move to center that position under the detector.

Stage Movement – Navigation

1. Before you do any navigation, select the Stage menu and check that Touch Alarm
Enabled and External Current Measurement are both checked. These need to be active
in case you drive the sample into the detector. With these enabled the stage will stop as
soon as it touches the detector preventing significant damage. Nonetheless, be careful
not to crash your sample into the detector.
2. Open the Navigation page and select the Coordinates tab. In this tab, you control the x,
y, z, tilt, and rotation of the sample stage.
3. There are three modes for changing the position: actual, target, and relative.
a. Actual mode displays the actual position coordinates in the edit box.
b. Target mode activates when clicking a stored position or when editing a coordinate
value.
c. Relative mode is used to move a stage by a given value and to repeat it several
times if needed.

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 Standard Operating Procedure: SEM
4. In order to move a stage, select the mode you wish to use and enter a value into the edit
box and click the Go To button. If you wish to stop the stage while it is in motion, click the
Stop button (the Go To button becomes the Stop button when the stage is in motion) or
press the Esc key.
5. There are simpler options for moving in the x, y and z coordinates using live images and
the scroll wheel on the mouse. When the beam is on and there is a live image in Quad 1
or Quad 2, hold down the scroll wheel and drag the mouse in the direction you would like
to move. You can also double click on a feature to center it within the quad.
6. The safest way to move the z-stage in order to avoid crashing into the detector is in the
live camera quad (Quad 4), hold down the scroll wheel and drag the mouse up or down to
move the stage in that direction.

Imaging

1. Turn on the beam by clicking the Beam On button.

2. Set the voltage (High Voltage) and current (Spot) to
your preferred settings.
3. Select Quad 1, which should be set to the Everhart Thornley Detector (ETD), and click the
pause icon to begin imaging.
4. Adjust the contrast and brightness using the control knobs behind the keyboard or by
selecting Auto Contrast Brightness (tool bar icon or press F9).
5. Set the dwell time and resolution for imaging by making adjustments in the tool bar or by
selecting one of the presets.
6. Find a feature that you can use for focusing and then use the control knobs behind the
keyboard to adjust the magnification, focus and stigmator to optimize your image.
7. If you want to use the Through Lens Detector (TLD), select Quad 2, which should be set
to the TLD, and click the pause icon to begin imaging (doing so will automatically pause
Quad 1 as the SEM switches the detector. When using the TLD you have the option of
changing the lens mode between Field-Free (the default mode for ETD) or Immersion
(used for ultra-high resolution imaging).
8. To capture an image, click on the Photo button or press F2.
9. When prompted to save your image, save to your folder in the User SEM Images folder
on the Litho-PC. When you are finished imaging switch to the Raith computer and copy
your files from User SEM Images to your folder in the NanoFab01 shared drive. DO NOT
use a flash drive on either computer and DO NOT try to access the internet. You can
retrieve your files from the NanoFab01 folder on any of the computers in the wipe down
room.

Unload Sample – Load Lock

1. Turn off the beam by clicking the Beam On button.

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2. Check that the load lock is properly closed and the press the P button, which will pump
the load lock if it is not already at vacuum and move the stage into the loading position.
Once the load lock is pumped and the stage is in place, the OK button will light up and the
gate valve interlock will release allowing the door to the main chamber to be opened.
3. Turn the gate valve knob from LOCK to UNLOCK and then carefully pull the knob bar fully
out from the first mark to the second mark. Turn the gate valve knob from UNLOCK to
LOCK.
4. Move the unloading rod from the parking position and into the chamber until it meets
resistance at the start of the slot. Turn the rod counterclockwise to the base of the slot
and push the rod forward to the front of the slot inserting it into the sample carrier. Turn
the rod clockwise to lock the sample carrier onto the rod and then withdraw it back to the
parking slot bringing the sample out of the main chamber. Warning: be sure to put the rod
into the parking position at the end; turning it the other way disengages it from the rod and
the spring will fling the sample carrier into the gate valve.
5. Close the gate valve by turning the knob bar to the UNLOCK position, pressing the knob
in to engage the valve over the opening and then turn the knob to the LOCK position to
secure it.
6. Press the V button to vent the load lock. Once vented the lid can be opened and the
sample carrier can be released by turning the rod bar to the far left.
7. Remove your sample from the load lock.
8. Close the load lock lid and press the P button to evacuate the loader chamber.

Cleanup and Waste Disposal

1. Tidy up area.
2. Throw away used tape into the trashcan.

Emergency Stop
- The only thing users should ever turn off is the beam.

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Allowed Activities
- Users may open the chamber and insert the low vacuum detector, but only if they have
been trained on how to do so.
- Users may open the chamber and change the sample holder setup on the stage, but only
if they have been trained on how to do so.

Disallowed Activities
- Users should never disable the touch alarm or the external current measurement.

What to watch out for during operation

- Users should be sure that the chamber pressure is less than 4.0E-5 range before turning
on the beam.
- Users should not adjust the setting for the source tilt and alignment.

Common Troubleshooting Tips

- If the image shifts whenever the focus is adjusted, try adjusting the lens alignment, though
only if you’ve been shown how to do so.
- If a user is seeing a lot of charging, they could try switching to another detector, or change
the detector setting to backscatter electrons or custom mode.
- If a user is seeing a significant amount of image drift, they should try pausing everything
and waiting about 10 minutes before trying to image again.
- If controls are not working properly, try closing and then restarting the software. Login to
the software as “user” with password “Hilda001”.

When to call staff?

- If the cooling water is not flowing.
- If your sample gets stuck in the load lock door.
- If the stage position for loading from the load lock is not correct.
- If none of the common troubleshooting tips are able to fix a problem.

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 Standard Operating Procedure: SEM

Badger Criteria
Report Problem:

1. If none of the common troubleshooting tips are able to fix a problem.

Shutdown:

1. If the cooling water is not flowing.

2. If your sample gets stuck in the load lock door.

Revision History:

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