eTraining Introduction

Specimen Preparation

Leica Ultracut UCT

Histology

JEOL JSM-6400 SEM

Hitachi S-4700 FE-SEM

Hitachi FB-2000A FIB

Microanalysis

Veeco Dim 3000 AFM

Fluorescence Microscopes

Support

Coating

Carbon Coating Procedure

Equipment is DV-502A, Denton Vacuum Inc. and Affinity.

WARNING

The arc produced by the evaporation process will damage unprotected eyes. Use the red welding goggles or otherwise shield your eyes from the bright source. See step 10 in Coat the Samples below.

Open the Bell Jar

1. Switch SYSTEM CONTROL to ON. VIEW
2. Switch MECH PUMP to ON. VIEW
3. Open the valve for the red nitrogen tank to the right hand side of the coater.
4. Turn upper left knob to AUTO VENT. VIEW
 4.1. Wait until it is done hissing.
 4.2. Tip the bell jar until it loosens, and then raise it. WARNING: The bell jar can be ruined if you drop it onto the base plate. Please be very careful—the bell jar is $800. VIEW
 4.3. At the top turn slightly to latch it. VIEW

To Close the Bell Jar Without Having Coated

NOTE: The instructions assume that the HI-VAC PUMP was never started.

1. Turn upper left knob to AUTO PUMP. VIEW
 1.1. Wait until the THERMOCOUPLE GAUGE reads less than 20. VIEW
 1.2. If it will not go down or it keeps moving back and forth over the 20 mark, then use the manual procedure:
  1.2.1. Turn upper left knob to MANUAL. VIEW
  1.2.2. In VALVES switch on ROUGH. VIEW
  1.2.3. Wait until the reading on the THERMOCOUPLE GAUGE is all the way down, then switch back on the AUTO PUMP.
2. Return the upper left knob to MANUAL. VIEW
3. Switch MECH PUMP to OFF. VIEW
4. Switch SYSTEM CONTROL to OFF. VIEW
5. Bleed the valve switch (located on the far right under the panel). VIEW
6. Close the valve switch after it is done venting (hissing). VIEW

Coat the Samples

1. Prepare the carbon rods.
 1.1. Pull back the spring. Rotate the carbon rods in opposite directions. VIEW
 1.2. Twist the holder to release the rods. VIEW
 1.3. Take the beveled rod and grind on the sandpaper to replace its surface. VIEW
 1.4. Throw out the sharpened rod. Take a new one and place it in the sharpening machine. Switch on the motor and slide the sharpener (flat side facing the carbon) along until you can see the edge line up on the far flat side. VIEW
 1.5. Slide the beveled rod back into the fixed holder until only about ¼ of it shows.
 1.6. Slide the sharpened rod back in the spring loaded holder. (Do not tighten into place just yet.)
 1.7. Rotate the rods (while holding the spring loaded one back) back into position.
 1.8. While holding the spring back, pull the sharpened rod out until it touches the beveled surface of the other rod (be careful, the sharpened rod is fragile!), then tighten it into place. VIEW
 1.9. Let go of the spring, making sure there is contact between the carbon rods and that the sharpened rod does not break.
2. Prepare the brass specimen. VIEW
 2.1. Polish the brass using the rag containing polishing compound until the brass appears shiny.
 2.2. Wipe the polish compound off using a paper towel.
 2.3. Place the brass on pennies to boost it to about the same height as the sample that is being coated. VIEW
3. Place samples on the plate, orienting them so that surface to be coated is under the touching carbon rods. VIEW
4. Lower the bell jar and give a push/twist to seat it into position. VIEW
5. Turn upper left knob to AUTO PUMP, pumping to 20 on the THERMOCOUPLE GAUGE. If it stops and keeps moving back and forth over the 20, then use the manual procedure. VIEW
6. Turn ON Affinity Cooler (located underneath the table next to the carbon coater). VIEW
7. Switch HI-VAC PUMP to ON. VIEW
8. Switch HIGH VACUUM GAUGE to ON. (Wait until it gets down to 10-5 range. This takes a while.) VIEW
9. Pour 2 funnels worth of liquid nitrogen into the funnel. See Properties of LN2 in General Lab Safety under Support. VIEW
10. Switch FIL/GLOW POWER to ON. WARNING: The arc produced by the evaporation process will damage unprotected eyes. Use the red welding goggles or otherwise shield your eyes from the bright source. VIEW
11. Turn the FIL ADJUST knob slowly, keeping an eye on the carbon rods until they start to heat up (i.e. turn red). VIEW
12. Adjust your view so that you cannot see the rods but can see the brass sample. Continue to turn the FIL ADJUST knob until sparks are observed. The carbon will turn in sequence Orange-Red-Purple-Blue.
13. When the brass turns blue (~20 nm thickness), turn the knob OFF.
14. Switch FIL/GLOW POWER to OFF.
15. Switch HIGH VACUUM GAUGE to OFF. VIEW
16. Turn upper left knob to AUTO VENT. VIEW
17. Take the specimens out.

To Close the Bell Jar After Coating

1. Turn upper left knob to AUTO PUMP until BACK and HI-VAC lights go on. VIEW
2. Switch HI-VAC PUMP to OFF. (Wait about 5 minutes to let it stop spinning.) VIEW
3. Turn upper left knob to MANUAL. VIEW
4. Switch MECH PUMP to OFF. VIEW
5. Switch SYSTEM CONTROL to OFF. VIEW
6. Bleed the valve switch (located on the far right under the panel). VIEW
7. Close the valve switch after it is done venting (hissing). VIEW
8. Wait about 10 minutes and shut OFF the Affinity Cooler. VIEW

Clean the Bell Jar

NOTE: The procedure should only be carried out by lab personnel.

  1. Cover the base plate apparatus with tin foil and then cover that with some towels to keep it from getting wet.

  2. Take a moist white towel and apply liquid hand soap to the interior of the bell jar to remove the carbon.

  3. Using another wet towel wipe up the excess soap. Then dry with a clean towel.

  4. Use the spray bottle on top of the towel dispenser over the sink that says "Bell Jar cleaner" and spray the inside of the bell jar. Make sure to coat the entire inside.

  5. Let it dry completely before returning it into position and closing bell jar or carbon coating samples using the above instructions.

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