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Sample manipulation

Sample manipulators


manipulator 4-axes, z 300 mm 5-axes, z 500 mm
usually mounted in analysis chamber preparation chamber - top
(reaching also preparation chamber - bottom)
x, y 0-50 mm
manual by micrometers with digital reading
centre = 25 mm
 
0-50 mm
manual by micrometers
center = 25 mm
x = 42 mm in order to pass through the valve!
z (height) 0-300 mm
motorized with end-switches
useful range 80-250 mm
reading on motor controller or vertical ruler
0-500 mm
motorized with end-switches
useful range 40-480 mm
reading on motor controller or vertical ruler
Θ (polar) 0-360°
motorized without end-switches
useful range 30-270°
reading on motor controller or index above the motor
0-360°
manual by handle
useful range 90-300°
reading on rotatable flange scale
Φ (azimuth) fixed ±100°
motorized with end-switches
useful range ±90°
reading on motor controller
annealing up to 1300 K up to 1300 K
cooling 100 K in 20 minutes not available (when in preparation chamber)
150 K in 1 hour (when in analysis chamber)
typical Θ 30°
60°
90°
150°
180°
185.3°
190°
195°
210°
220°
230°
270°
Ce evaporator
bottom exchangeable evaporator
Oxford evaporator, LEED
SR normal incidence
SR 30° incidence, 30° emission; top exchangeable evaporator
SR magic angle
XPS (20° emission)
ion sputtering (45° incidence)
SR normal emission
SR grazing incidence (20° off surface)
SR grazing incidence (10° off surface)
sample transfer
270°










 
sample transfer










 


Motor controllers



The controllers are connected using standard UTP cables serving for both power and data transfer between them and the computer. Each controller has 3 equal sockets. The most distant socket from the computer should be fitted by a terminator but usually it works also without it.

The display shows actual value of its own axis or rC.00_ for remote controlled axis which can be:
  • rC.002 for Φ (azimuth angle) in the analysis chamber (not connected if the manipulators are not swapped, see below);
  • rC.003 for zmain (height) in the analysis chamber;
  • rC.004 for Θ (polar angle) in the analysis chamber;
  • rC.005 for zprep (height) in the preparation chamber (not connected when not in use).
The LEDs on the left side of the display indicate the actual state (stopped, moving, end-switches...).

Remote control selects the other axis to be controlled (rc.00_ on the display) or its own axis (value on the display).

Speed button selects the speed between low (green LED) for fine slow setting and high (red LED) for coarse fast setting.

The arrows buttons increase or decrease the value.

Stop button stops and blocks all axes. Press it if any software, e.g. KolXPD, is moving the manipulator to a risky position.

Buttons Speed and Stop pressed together unblock the blocked axes.

Several seconds after the last movement the controller saves the actual position into its memory in order not to lose it in case of sudden power failure (indicated by "saved" on the display).


Swapping manipulators

For angle-resolved measurements (ARPES, XPD) the manipulator must be swapped in order to automatically rotate the sample in Θ and Φ directions during the data acquisition. At this point the 5-axes manipulator is moved into the analysis chamber while the 4-axes manipulator is stored in the preparation chamber - top (where it cannot be used due to insufficient z-range being only 300 mm).
  1. Vent the chambers.
  2. Remove the 4-axes manipulator (z 300 mm) from the analysis chamber using the Elettra crane and put it on a temporary support.
  3. Move the 5-axes manipulator (z 500 mm) from the preparation chamber - top into the analysis chamber using the Elettra crane.
  4. Move the 4-axes manipulator (z 300 mm) from the temporary support into the preparation chamber - top using the Elettra crane.
  5. Bake-out the analysis chamber.
  6. Swap the zmain and zprep motor controllers in order to have zmain on the analysis chamber again.
  7. Install and connect the Φ motor at the top of the manipulator.
  8. Connect the Φ endswitch cable.
  9. Connect the Φ motor controller into the zmain motor controller.
  10. Swap the Θ motor with the Θ handle in order to have the motor on the analysis chamber again.


Part of the manipulators inside the chambers (without and with sample holder inserted):



Sample insertion from air into the analysis chamber

  1. Mount the sample(s) on the chosen sample holder.
  2. Check that there is no sample holder inserted in the analysis chamber.
  3. Check that the gate valve (between load lock and preparation chamber - bottom) and the angle valve (between load lock and preparation chamber - top) are properly closed.
  4. Switch off the load lock turbopump and let it vent with nitrogen gas. During venting observe that the pressures in the preparation chamber and analysis chamber do not change.
  5. Open the load lock door, remove the previous sample holder (if any) from the transfer rod bayonet adapter and put there your sample holder (by inserting the sample holder part into the bayonet slit, pushing fully in, rotating the transfer rod by 90° and releasing). The sample holder should be sufficiently fixed in the bayonet.
  6. Rotate the sample facing upwards.
  7. Close the load lock door.
  8. Close the nitrogen gas inlet.
  9. Start the load lock turbopump.
  10. Wait at least 30 min. The pressure in the load lock should go below 10-6 mbar.
  11. Open the gate valve (between load lock and preparation chamber - bottom). The pressure in the preparation chamber - bottom should stay in low 10-7 mbar order.
  12. Transfer the sample into the preparation chamber - bottom.
  13. Check that LEED, electron analyzer, X-ray source, evaporators etc. are off and that the electropneumatic valve 10 towards the beamline is properly closed.
  14. Open the gate valve (between preparation chamber - bottom and analysis chamber). The pressure in the analysis chamber should stay in low 10-8 mbar order.
  15. Transfer the sample into the analysis chamber while observing the procedure through the CF160 viewport using a mirror or CF100 viewport and stop well before reaching the manipulator.
  16. Rotate the transfer rod by 90° in order to make the sample face the CF160 viewport.
  17. Carefully approach the manipulator with the sample holder and check the situation through the CF160, CF100 and CF63 viewports. The approximate position is x = 24, y = 25, z = 236Θ = 270°. Adjust x, z and transfer rod rotation in order to insert the sample without crashing, bending or forcing anything.
  18. When the sample holder is inserted in the manipulator push the transfer rod bayonet fully in and block it with a screw in this position.
  19. Rotate the transfer rod by 90°. You should not feel any force.
  20. Unblock the screw of the transfer rod translation and carefully release the bayonet from the sample holder. The holder should stay inserted in the manipulator. If the holder moves out by some milimeters push it carefully in by the transfer rod again.
  21. Check heating current and thermocouple electrical contacts (if installed on the sample holder).
  22. Retract the transfer rod completely into the load lock.
  23. Close both gate valves.

Sample removal from the analysis chamber into air

  1. Check that the manipulator is not cooled down by liquid nitrogen, that LEED, electron analyzer, X-ray source, evaporators etc. are off and that the electropneumatic valve 10 towards the beamline is properly closed.
  2. Set the manipulator to the approximate position for sample removal x = 24, y = 25, z = 236, Θ = 270°.
  3. Check that the pressure in the load lock is below 10-6 mbar.
  4. Open the gate valve (between load lock and preparation chamber - bottom). The pressure in the preparation chamber - bottom should stay in low 10-7 mbar order.
  5. Move the transfer rod into the preparation chamber - bottom.
  6. Open the gate valve (between preparation chamber - bottom and analysis chamber). The pressure in the analysis chamber should stay in low 10-8 mbar order.
  7. Carefully approach the transfer rod towards the sample holder inserted in the manipulator with the sample holder inserted in the manipulator. Check the situation through the CF160, CF100 and CF63 viewports. Adjust x, z and transfer rod rotation in order to freely insert the sample holder part into the bayonet without crashing, bending or forcing anything. In case of problems consult Troubleshooting - Transfer rod bayonet.
  8. When it freely enters push the transfer rod bayonet fully in and block it with a screw in this position.
  9. Rotate the transfer rod by 90°. You should not feel any force.
  10. Unblock the screw of the transfer rod translation and carefully remove the sample holder from the manipulator to a safe distance.
  11. Rotate the transfer rod by 90° in order to make the sample face upwards.
  12. Retract the transfer rod with the sample holder completely into the load lock.
  13. Close both gate valves.
  14. Check that the angle valve (between load lock and preparation chamber - top) is properly closed.
  15. Switch off the load lock turbopump and let it vent with nitrogen gas. During venting observe that the pressures in the preparation chamber and analysis chamber do not change.
  16. Open the load lock door, remove the sample holder from the transfer rod bayonet adapter (by pushing the sample holder fully in, rotating the transfer rod by 90° and releasing).
  17. If you do not plan to immediately insert any other sample holder close the load lock door.
  18. Close the nitrogen gas inlet.
  19. Start the load lock turbopump.

Sample transfer to preparation chamber - bottom and back

If the sample is not to be annealed in this chamber you can perform the desired experimental procedure (deposition, ion sputtering) while keeping the sample holder attached to the transfer rod, without using the manipulator installed in the preparation chamber - top.
  1. Follow steps 1-12 of Sample removal described above.
  2. Close the gate valve (between preparation chamber - bottom and analysis chamber).
  3. Perform the desired operation (deposition, ion sputtering).
  4. Wait until the pressure recovers at least in low 10-7 mbar order.
  5. Follow steps 13-23 of Sample insertion described above.

Sample transfer to preparation chamber - top and back

If this case the sample holder cannot stay on the transfer rod and it must be inserted into the manipulator.

Every time you need to pass the manipulator through the gate vale the x value must be 42, y = 25, Θ = 270°!
  1. Follow steps 1-12 of Sample removal described above.
  2. Close the gate valve (between preparation chamber - bottom and analysis chamber).
  3. Connect the zprep (height) motor controller to the zmain (height) one using a UTP cable.
  4. Set the position x = 42, y = 25, Θ = 270°.
  5. Open the gate valve between preparation chamber - bottom and preparation chamber - top (if not yet open).
  6. Carefully set zprep approximately to 45. During this procedure the manipulator must freely pass down through the gate valve.
  7. Set x approximately to 25.
  8. Transfer the sample into the preparation chamber - bottom while observing the procedure through the CF100, CF63 and CF38 viewports and stop well before reaching the manipulator.
  9. Rotate the transfer rod by 90° in order to make the sample face the CF100 viewport.
  10. Carefully approach the manipulator with the sample holder and check the situation through the CF100, CF63 and CF38 viewports. The approximate position is x = 25, y = 25, z = 45Θ = 270°. Adjust x, z and transfer rod rotation in order to insert the sample without crashing, bending or forcing anything.
  11. When the sample holder is inserted in the manipulator push the transfer rod bayonet fully in and block it with a screw in this position.
  12. Rotate the transfer rod by 90°. You should not feel any force.
  13. Unblock the screw of the transfer rod translation and carefully release the bayonet from the sample holder. The holder should stay inserted in the manipulator. If the holder moves out by some milimeters push it carefully in by the transfer rod again.
  14. Check heating current and thermocouple electrical contacts (if installed on the sample holder).
  15. Retract the transfer rod completely into the load lock.
  16. Close the gate valve between preparation chamber - bottom and load lock.
  17. Set x to 42.
  18. Carefully set zprep approximately to 450. During this procedure the manipulator must freely pass up through the gate valve.
  19. Set x to 25.
  20. If you need to perform sample exposure at high pressures reduce pumping of the preparation chamber - top by full/partial closing of the gate valve between preparation chamber - bottom and preparation chamber - top and/or of the angle valve between load lock and preparation chamber - top).
  21. Perform the desired operation (sample annealing, gas exposure...).
  22. After that fully open the gate valve between preparation chamber - bottom and preparation chamber - top (if closed in step 20). Wait until the pressure recovers at least in low 10-7 mbar order.
  23. Set the position x = 42, y = 25, Θ = 270°.
  24. Carefully set zprep approximately to 45. During this procedure the manipulator must freely pass down through the gate valve.
  25. Set x approximately to 25.
  26. Carefully approach the transfer rod towards the sample holder inserted in the manipulator with the sample holder inserted in the manipulator. Check the situation through the CF100, CF63 and CF38 viewports. Adjust x, z and transfer rod rotation in order to freely insert the sample holder part into the bayonet without crashing, bending or forcing anything. In case of problems consult Troubleshooting - Transfer rod bayonet.
  27. When it freely enters push the transfer rod bayonet fully in and block it with a screw in this position.
  28. Rotate the transfer rod by 90°. You should not feel any force.
  29. Unblock the screw of the transfer rod translation and carefully remove the sample holder from the manipulator to a safe distance.
  30. Rotate the transfer rod by 90° in order to make the sample face upwards.
  31. Retract the transfer rod with the sample holder completely into the load lock.
  32. Set x to 42.
  33. Carefully set zprep approximately to at least 120. During this procedure the manipulator must freely pass up through the gate valve.
  34. Insert the sample into the analysis chamber by following steps 13-23 of Sample insertion described above.


Last Updated on Thursday, 22 October 2020 17:32