manual model 180 xtem prep kit 2007

7/25/2019 Manual Model 180 XTEM Prep Kit 2007

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MODEL 180 Cross-Section TEM (XTEM) Prep Kit

INSTRUCTION MANUAL

E.A. Fischione Instruments, Inc.

9003 Corporate Circle

Export, PA 15632 USA

Phone (724)325-5444FAX (724)325-5443

www.fischione.comPN 010-0034 Revision 00
http://www.fischione.com/http://www.fischione.com/


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Basic Cross-Section TEM (X-TEM) step-by-step

1. Cleave or cut the specimen to a size that will fit on the aluminum specimen slide ofthe Model 170 Ultrasonic Disk Cutter. Cut the specimen so that the area of interest

falls near the center.

2. Set hot plate temperature to 150C. If specimen is patterned, mount the specimen

with Crystal Bond Type 509 to aluminum slide, device side up. If the specimen

does not have a pattern, the specimen can be mounted face down on the aluminumslide and step 3 can be skipped.

3. Cover specimen with glass cover slip using Crystal Bond.

4. Fit the 4 mm x 5 mm or 2 mm x 3 mm rectangular cutting tool onto the disk cutter.

5. Cut rectangular sections of area of interest from mounted wafer.

Use 600 or 1000 grit SiC powder for cutting. Cubic Boron Nitride can also beused, 45mm size in water base paste.

Figure 1. Cutting rectangular sections for XTEM specimen preparation.

6. If Crystal Bond was used, heat the specimen sections on hot plate to remove glass

cover slip, and use acetone to remove all traces of Crystal Bond. Rinse specimens

several times with acetone.

7. Decide how many sections to use in the built-up cross section.

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8. Mount these sections face side down on the Model 160 Grinder and back side thin.

a) Thin to ~200 m with 600 grit SiC paper.

b) Thin to final thickness in steps using diamond lapping films in order: 6 m, 3

m, 1 m. Remove at least 25 m per step.

c)

Final thickness depends upon number of sections to be used in the crosssection. The more specimens in the cross section, the thinner each section

needs to be.

9. Remove the sections from grinder and soak again in acetone in a clean glass vial to

remove any Crystal Bond. Rinse several times.

10. Pour off excess acetone and place glass vial containing the specimens on a hot plate

to evaporate remaining acetone.

11. Carefully dump dry specimen pieces onto lint free paper. Handle pieces as little as

possible to avoid breakage.

12. Mix M Bond 610 two part epoxy following the manufacturers directions.

13. Arrange pieces to prepare building XTEM stack, again handling as little as possible

to avoid breakage. Use two extra (dummy) pieces on each side of the specimenpieces. Use thicker specimen pieces as the innermost dummy pieces. A typical stack

is 4mm x 5mm x 5mm.

Dummy Pieces

Thinned Specimen Pieces

Dummy Pieces

Thicker Specimen Pieces

Figure 2. Specimen section layout to create the XTEM stack.

14.

Paint epoxy on inside of first dummy piece and place in Teflon stack vise. Repeatwith other dummy pieces and stack pieces until complete stack is built. Use enoughepoxy to completely cover the pieces. If screw type vise is used, create stack, wait 5

min, then place assembly into vise. Turn cap screw until finger tight or use an allen

wrench (7/64) until snug.

15. Place entire vise on hot plate and cure epoxy. Suggested time for curing is 40

minutes.



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Figure 3. Creating the XTEM stack.

16. Remove rectangular tool from Model 170 Ultrasonic Disk Cutter and replace with

2.3 mm coring tool.

17. Make partial cut with coring tool into a glass slide.

18. Move the alignment microscope into place, swinging the microscope in the same

direction as the cutting tool is swung over the plate to be cut.

19. Looking through the microscope, align the microscope to the partially cut circle

using the 4 round thumb screws at the base of the eyepiece so that the circle cut withthe coring tool in step 16 is in the center of the field of view. The microscope is now

aligned with the cutting tool.

20.

Remove stack from vise and place on edge in the aluminum stack mounting plate.Use Crystal Bond to secure stack in place.

21. Place stack mounting plate under the disk cutter and using the alignmentmicroscope, move the specimen until the center of the cross section is in the center

of the field of view. Do not cut too near the wedge shaped walls of the specimen

mounting plate as proximity of the cutting tool to these walls will activate theautomatic termination of cutting.



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22. Cut the 2.3 mm core from the stack using 600 or 1000 grit SiC or Cubic Boron

Nitride. If cutting slows while coring the specimen, add abrasive near the cuttingtool and push and pull lightly on the plunger of the cutting water assembly. This

will allow cutting to continue without moving the cutting tool and possibly moving

the cutting course. If the process of cutting slows, place additional abrasive near the

cut with a Q-tip. The cutting may need to be paused and the tool carefullywithdrawn to allow the abrasive to be pushed down into the cut.

Figure 4. Using the 2.3 mm cutting tool to core the XTEM stack.

23. Soak the 2.3 mm core in acetone and then epoxy the core into a 3 mm brass tube.

Place upright on hot plate in the Teflon tube holder and cure. The epoxy to be used isEpotek type 353ND and it can be mixed in the supplied Teflon dish. This is also a

two part epoxy. Follow the manufacturers directions for mixing. Completely fill the

tube with the epoxy. Cure for at least 40 minutes.

Figure 5. Inserting the XTEM core rod into the 3 mm brass tube.



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24. Using a low speed diamond wafering saw, cut the brass tube into 400-500m thickdisks. (A thinner section can be cut with a wire saw, if available.)

25.

Mount one thick disk to a platen and polish one side to 1 m diamond finish usingthe same steps outlined in step 8, parts a) through c). Total specimen thickness atthis point does not matter, but for safe removal of damage, final thickness after

polishing this one side should be approximately half of the starting thickness.

Note:

Polishing is best done with

diamond lapping films

placed over a glass toppedplaten on the rotating

grinder being used.

Figure 6. XTEM disk cut from 3mm brass tube.

26. Remove disk from specimen grinder. At this point the decision must be made for theprocess used to remove bulk material from the back side of the disk. To remove

with the Model 160 specimen grinder, proceed to step 27. To remove using the

Model 200 dimple grinder, proceed to step 28.

27. Turn over the disk and place on the Model 160 specimen grinder platen polished side

down:

a) Thin to ~200 m with 600 grit SiC paper.

b) Thin to final thickness in steps using diamond lapping films in order: 6 m, 3

m and 1 m. Remove 25 m of specimen thickness with each step.c) Aim for a final disk thickness of


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29. If you thinned with the Model 160 specimen grinder, remove the specimen platen

from the grinder and place on the dimple grinder. If you thinned with the dimplegrinder, leave the specimen platen in place if you plan on measuring specimen

thickness with the Model 200. An alternative is to remove the specimen, measure

thickness by micrometer and re-glue the specimen to its platen. Zero on top of the

specimen.

Note: Refer to Model 200 Dimple Grinder for choice of grinding wheels and parameters.

30. Select the dimpling wheel you wish to use and place on the grinding wheel spindle.

31. Dimple the specimen using 3 m diamond paste until the specimen is 30 m thick.Change counterweight from 50g to 40 or 30g.

32. Clean dimple wheel well and switch to 1 m diamond compound. Remove material

until the specimen is 20-25m thick. Check condition of specimen with microscope.

33.

Clean dimple wheel well and dimple the specimen until the first sign of transmittedlight shows through the specimen (~10 m) and is deep red or brown in color.Transmitted lights and colors will only be seen in specimens of silicon.

34. Clean dimple wheel well and add more 1 m diamond compound. Dimple the

specimen until dark orange in color (~7-8 m).

35. Continue dimpling carefully with 1 m diamond paste until the specimen is brightorange in color.

36. Remove specimen platen from dimpling wheel. Remove specimen from platen

carefully by either placing the specimen on the hot plate and removing the specimenwhen the Crystal Bond becomes molten or by soaking entire specimen platen inacetone until specimen falls off. The second option is the safest and requires

approximately 30 minutes.

37. Soak specimen in acetone to remove any remaining Crystal Bond and rinseseveral times.

38. Load specimen into ion mill holder.

39. Ion mill specimen at 3.5 kV, 5 mA and 10 degrees until perforation.


manual model 180 xtem prep kit 2007

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