Elettra-Sincrotrone Trieste S.C.p.A. website uses session cookies which are required for users to navigate appropriately and safely. Session cookies created by the Elettra-Sincrotrone Trieste S.C.p.A. website navigation do not affect users' privacy during their browsing experience on our website, as they do not entail processing their personal identification data. Session cookies are not permanently stored and indeed are cancelled when the connection to the Elettra-Sincrotrone Trieste S.C.p.A. website is terminated.
More info
OK

Sample manipulation


Sample insertion

  1. Mount the sample(s) on the chosen sample holder.
  2. Check that there is no sample holder inserted in the experimental 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 turbopumping stage and let it vent with nitrogen gas. During venting observe that the pressures in the preparation chamber and experimental 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 turbopumping stage.
  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 experimental chamber). The pressure in the experimental chamber should stay in low 10-8 mbar order.
  15. Transfer the sample into the experimental chamber while observing the procedure through the CF160 viewport using a mirror 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 and CF63 viewports. The approximate position is x = 19, y = 25, z = 256Θ = 268°. 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

  1. Check 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 = 19, y = 25, z = 256, Θ = 268°.
  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 experimental chamber). The pressure in the experimental 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 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 the 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 turbopumping stage and let it vent with nitrogen gas. During venting observe that the pressures in the preparation chamber and experimental 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 turbopumping stage.

Sample transfer to preparation chamber - bottom

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 experimental 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

If this case the sample holder cannot stay on the transfer rod and it must be insterted 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 experimental 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 ??. During this procedure the manipulator must freely pass down through the gate valve.
  7. Set x approximately to ??.
  8. Transfer the sample into the preparation chamber - bottom while observing the procedure through the CF100 of 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 and CF38 viewports. The approximate position is x = ??, y = 25, z = ???Θ = 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 ??. 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 or partial opening 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 ??. During this procedure the manipulator must freely pass down through the gate valve.
  25. Set x approximately to ??.
  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 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 the 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 ??. During this procedure the manipulator must freely pass up through the gate valve.
  34. Insert the sample into the experimental chamber by following steps
  35. Follow steps 13-23 of Sample insertion described above.


Last Updated on Thursday, 18 October 2018 09:54