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2. Contents

OVERVIEW

1. Ion milling

2. FIB

3. Tripod polishing

4. Electro-polishing

5. Ultra-microtomy

3. Overview

Sample preparation

Specimen requirements

4. ATEM : CTEM (BF) (DF) HRTEM : (SAED) Kikuchi : (EDS) (EELS) 5. TEM C2 lens: Brightness knob cond stigmator x/y knob focus button focus button obj stigm x/y knob Magnification button Gun tilt x/y knob Gun horizon x/y knob Specimen holder button 6. TEM-EDS JEM-2000FXII 7. Sample Preparation

Sample Preparation>> TEM Work

Metarials Matal Ceramics Semiconductor Powder Fiber Bio-material, . Purpose of Work TEM-microstructure,HREM SEM-Topography, Microstructure EPMA-Quantitative, Qualitative EELS, Preparation Methods Ion milling, Tripod polishing, FIB, Ultramicrotomy, SACT, 8. Specimen requirements

Thin : less than 1000

Shape : 3mm disk type

Representative of, and unchanged, from bulk

Flat, not rugged

Amount of transparent area

Stable in the electron beam

Very clean : free from extraneous particles or debris

( possibly from specimen preparation )

Conductive, non magnetic

TEM specimen must be . TEM specimen with varing thickness will affectx-ray quantitative analysis. 9.

1. Ion milling

2. FIB

3. Tripod polishing

4. Electro-polishing

5. Ultra-microtomy

10. ?? Chemicalpolishing Chemicaletching Cleavage FIB Ion Milling Tripodpolishing Ultra- microtomy Electro-polishing Replica 11. Ion Milling : , 12. Ion Milling

dimpling

Tool material / coating

Tool profile

Tool thickness/diameter

Pressure(force) of tool

Slurry composition and grit

Speed of rotation

Tool / sample contact area

13. Ion Milling

Ion milling

14. FIB(Focussed Ion Beam)

2. FIB Milling :2-4 :-0.2 :-100nm or less 1.Bar 1.Initial Cut 2.Fine Milling 3.Last Milling 3. Grid ( V-shaped Area ) 4. 50 2. 15. Tripod Polishing

diamond lapping film

polishing 100-500 , ion milling .

Advanced method * : Tripod Polishing + Sector Speed Control * - - - - ( ) * - Mechanical Polishing * Tripod Polisher - Designed to accurately prepare SEM and TEM samplesof pre-specified micron-sized regions - - ( , radiation damage, , , .) * - - wax pyrex - - Diamond abrasive film wet polishing ( : 60, 30, 15, 6, 3, 1 micron) - - -pyrex - wedge1micron - - - 2 x 1oval grid , 16. Electro-polishing

Electrolytic etching/polishing

Requirement :the specimen must be conductive

- this process works like a galvanic cell. The applied current forces the anode(sample) into solution to deposit onto the cathode

Initial condition of specimen surface influences polishing time

-better the surface at start the higher the current density, the shorter the polishing time

Window technique / Jet polishing

Basic 17. Electro-polishing

Jet polisher

Disc Punch

18. Fiber, Powder - Cross section kit fiber, powder 19. Ultramicrotomy

, , , ,

20. Ultramicrotomy

Self-supporting specimen: hard material-shape to a pencil stubsoft/small/delicate-embed in epoxy resin

Trim to a fine facet :trim the pencil point to a small flat with the microtome and assorted knives

Align knife to specimen : consider what type of information your section should provide

Section : for example, 1mm/sec cutting speed, 50nm thick, onto distilled water, proper setting

Collection sections onto TEM grid : fine-mesh or formbar coated, eliminate water

Basic 21. Ultramicrotomy

Ultramicrotome

Ultramicrotome Fine hair 22.

- CuNi, Au, CP(Cu/Pd)

Ultramicrotomy 23. Ultramicrotomy Knife

Diamond knife

35 : for reduced compression

45 : for general purpose

55 : for hard material

Glass knife

Ultramicrotomy 25.

Embedding

Ultramicrotomy

, , , LR

:6005 , 40-100nm

: LR , 901

Mould : ,

26. Ultramicrotomy

Trimming

trimming 27. Ultramicrotomy

Trimming

28. Ultramicrotomy Cutting Ultramicrotome (a)ultramicrotome(b)cutting 29. Ultramicrotomy

Cutting

30. Ultramicrotomy Cutting incorrect correct 31. Ultramicrotomy Cutting 32. Ultramicrotomy Cutting 33. Ultramicrotomy Cutting- Artifact : Thickness Variation 34. Ultramicrotomy - Artifact : Poor ribbon formation Cutting < edge of block face are not parallel to the knife edge> 35. Ultramicrotomy

Collection

Ultramicrotomy < The method for collecting sections from the trough > 37. Hard to clean,Soft materialLargetransparent area ( mm) Site-specific with great precision, , Tripod polishing crack 3 . , , , , fiber Ultra-microtomy Limited specimen area and tilt capability, artifactual waterfall surface effect, specimen material redeposition and Ga contamination , . Site-specific with great precision, mechanical/chemically unstable material FIBIon beam damage , . . , , Ion milling Si , , , , nm 38. System dependent 1 day Moderate Good None Can be severe Very good Moderate Often significant Easy with jigs day Large Good Very small Small Good Moderate planar Various methods 1-2 days Moderate Moderate Often significant Moderate Moderate Moderate Often significant Alignment of interface Total preparation time Transparent area Control of thickness Temperature rise Mechanical damage Compositional integrity Interface artifact Surface topography Ultramicrotomy Tripod polisher Ion beam thinning Characteristics 39.

http://www.ksem.com

PracticalMethods in ELECTRON MICROSCOPYV.13,Elsevier, 1991,

, , , 2000

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