10. Vent the transfer lid airlock for 3 s, then close the venting line.
11. Open the sliding valve on the transfer lid to allow access to the
shuttle.
12. While observing the shuttle, insert the transfer arm and close
the grabber to hold the shuttle. Verify the hold by pulling the
shuttle back slightly by a few millimeters. The next two steps
should be done quickly in succession to minimize
contamination.
13. Quickly and smoothly withdraw the shuttle completely to the
back position, lock the transfer arm, and close the sliding valve
on the transfer lid.
14. Pump the transfer lid airlock for 35–40 s to evacuate both the
transfer lid airlock and the transfer arm, then close the transfer
arm valve. Check that the transfer arm is in the “locked”
position.
15. Vent the transfer lid airlock, then release and lift the transfer
arm from the transfer lid.
16. Attach the transfer arm to the microscope airlock and pump the
airlock by pressing the “P” button. This will pump the airlock
and move the stage to the loading position.
17. Wait for the airlock vacuum to reach an acceptable level–the
“OK” button will turn on and the quickloader valve will unlock
(see Note 6). Listen for a click.
18. Open the microscope airlock gate valve, then open the transfer
arm valve.
19. Unlock the transfer arm and insert it all the way to dock the
shuttle into the stage. Release the shuttle grabber and retract
the arm. Check that the shuttle is no longer attached to the
arm. Lock the transfer arm.
20. Close the microscope gate valve to isolate the microscope
chamber. Leave the transfer arm attached to the quickloader.
The transfer arm valve may be left open.
21. Verify that the stage temperature is around À180
C and that
the chamber pressure is similar to the value before the transfer
(within 2–3 Â 10
À7 mbar).
Sample Inspection
and Milling Preparation
While milling, the user should periodically check the stage temperature and chamber pressure for appropriate values. If there is any
large deviation, the user may need to respond rapidly to salvage the
sample. The heat exchanger dewar will last about 8 h after initial
cooldown, depending on gas flow rate. If the instrument needs to
be operated for longer, the dewar can be refilled by slightly propping the heat exchanger aside and using a funnel to pour liquid
nitrogen into the tank.
Practical Approaches for Cryo-FIB Milling
65
11. Open the sliding valve on the transfer lid to allow access to the
shuttle.
12. While observing the shuttle, insert the transfer arm and close
the grabber to hold the shuttle. Verify the hold by pulling the
shuttle back slightly by a few millimeters. The next two steps
should be done quickly in succession to minimize
contamination.
13. Quickly and smoothly withdraw the shuttle completely to the
back position, lock the transfer arm, and close the sliding valve
on the transfer lid.
14. Pump the transfer lid airlock for 35–40 s to evacuate both the
transfer lid airlock and the transfer arm, then close the transfer
arm valve. Check that the transfer arm is in the “locked”
position.
15. Vent the transfer lid airlock, then release and lift the transfer
arm from the transfer lid.
16. Attach the transfer arm to the microscope airlock and pump the
airlock by pressing the “P” button. This will pump the airlock
and move the stage to the loading position.
17. Wait for the airlock vacuum to reach an acceptable level–the
“OK” button will turn on and the quickloader valve will unlock
(see Note 6). Listen for a click.
18. Open the microscope airlock gate valve, then open the transfer
arm valve.
19. Unlock the transfer arm and insert it all the way to dock the
shuttle into the stage. Release the shuttle grabber and retract
the arm. Check that the shuttle is no longer attached to the
arm. Lock the transfer arm.
20. Close the microscope gate valve to isolate the microscope
chamber. Leave the transfer arm attached to the quickloader.
The transfer arm valve may be left open.
21. Verify that the stage temperature is around À180
C and that
the chamber pressure is similar to the value before the transfer
(within 2–3 Â 10
À7 mbar).
Sample Inspection
and Milling Preparation
While milling, the user should periodically check the stage temperature and chamber pressure for appropriate values. If there is any
large deviation, the user may need to respond rapidly to salvage the
sample. The heat exchanger dewar will last about 8 h after initial
cooldown, depending on gas flow rate. If the instrument needs to
be operated for longer, the dewar can be refilled by slightly propping the heat exchanger aside and using a funnel to pour liquid
nitrogen into the tank.
Practical Approaches for Cryo-FIB Milling
65