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Hitachi S-5000 SEM Operation General Instructions

(March 2007)

1. Before starting the SEM

  • 1a. GET EML STAFF person to fill cold trap with liquid nitrogen.
  • 1b. Record IP1, IP2, IP3 pressures (Fig 1) into log book along with your name, date, and time. Ensure that IP-1 < 1.5E-7, IP2 < 2E-6, and IP3 < 7E-5 Pa.
  • 1c. Check the transfer position of the stage on the panel (Fig 2) near the monitors, and press the EX POSIT button to position the holder for sample transfer. The X, Y, and T of the stage goniometer should be 0, 0, 0.This must be done as damage to the specimen holder may result otherwise.
  • 1d. Confirm HV settings - Vacc, Vext and EMISSION, are all zeros (Fig 4). Press the HV OFF button if necessary.
  • 1e. Confirm SC Air Lock Valve switch (Fig 3) is in the CLOSE position.

 



2. Removing empty/sample wand from SEM

  • Step 1c, 1d and 1e must be done every time before removing or inserting any wand.
  • Pull out the holder knob straight out about 24 mm until it stops.
  • Turn the knob about 15 degrees clockwise until it stops.
  • Pull out the specimen holder straight out until it stops and turn it counterclockwise until it stops at the entrance.
  • Important: Set to AIR the EVAC/AIR switch on the specimen exchange chamber. After the EVAC lamp on the specimen chamber goes out, wait 10 more seconds.
  • After you hear a 'click', gently pull the holder straight out. Do not pull forcefully as it will cause air to rush into the chamber!
  • Place the empty wand into the plexiglass holder on the SEM console.

3. Loading specimen into sample wand

  • Insert wand into plexiglass preparation stage, making sure that the control knob is turned fully clockwise to lower the control shaft.
  • Use screwdrivers and tweezers for sample handling. Do not touch the wand or specimen holder beyond the O-ring with your fingers.
  • Loosen the right setscrew, and move the set piece to the right. Raise the control shaft until it reaches the upper groove of the sample holder.
  • Insert your specimen stub, move the set piece to hold the stub in the V-grooves, and lightly tighten the set screw.
  • Fully lower the control shaft and tighten the set screw.
  • Important: Verify that your sample is securely held by turning the holder upside down, gently testing stub motion with tweezers. If stub is not stable, it may fall into the SEM column.

4. Inserting sample wand into SEM

  • Insert the specimen wand into the specimen exchange chamber by matching the guide pin with the groove at the entrance and push it straight in until it stops.
  • After you hear a 'click', set to EVAC the EVAC/AIR switch on the specimen exchange chamber and wait until the EVAC lamp blinks.
  • When the EVAC lamp is blinking, FIRMLY grasp the holder, as it will be drawn into the column by the vacuum after this step. Turn the holder clockwise until it stops and while firmly grasping it, push it straigt in until it stops. Turn the holder counterclockwise, and push it straight in until it stops.
  • Note: If you wait too long after the blinking, you will not be able to insert the wand and you must set the switch to AIR, and then again to EVAC to repeat the above step.

5. SEM Operation

  • After the EVAC lamp on the specimen exchange chamber has stopped flashing, open the SC AIR LOCK valve switch (Fig 3).
  • Check that HV ready light is lit, and press the ON/ADJ button (Fig 4).
  • Press the 'stage' button above the mouseball twice, the STAGE light will be on.
  • Scan away using the focus, magnification, stage position mouseball, automatic contrast brightness (ACB) adjustment, manual contrast brightness adjustment and X/Y stigmation as necessary.

6. Collecting digital images

  • Turn on the DigiScan box above the SEM console.
  • Double click the 'Digital Micrograph' icon on computer desktop.
  • Change the SEM scanning speed from 'TV' to '3'.
  • Capture the image by pressing the 'turtle' button in the 'Digital Micrograph' software. The SEM image on the console will become blurry which is normal as the DigiScan is now controlling the microscope.
  • After collecting the image, save the image by clicking the menu 'Custom' -> 'Save'. Don't use the function in 'File' -> 'Save', otherwise the image file will not be opened correctly later.
  • Please save all the files in the 'emluser' folder on desktop. That folder is on our wilfred sever.


7. Shutdown

  • Remove the wand by following the "Removing empty/sample wand from SEM" in step 2.
  • Insert the large empty specimen holder back into the SEM.
  • Remove your specimen from the specimen wand by reversing the procedure for inserting it.
  • Remove the sample wand and store in wooden wand box.
  • Turn off DigiScan box, and turn off the computer monitor.
  • Be sure to clean up anything left behind. Fill out the log book and check out in our EML store.