2. Contents
3. Overview
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
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
TEM specimen must be . TEM specimen with varing thickness will affectx-ray quantitative analysis. 9.
10. ?? Chemicalpolishing Chemicaletching Cleavage FIB Ion Milling Tripodpolishing Ultra- microtomy Electro-polishing Replica 11. Ion Milling : , 12. Ion Milling
13. 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
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
Basic 17. Electro-polishing
18. Fiber, Powder - Cross section kit fiber, powder 19. Ultramicrotomy
20. Ultramicrotomy
Basic 21. Ultramicrotomy
Ultramicrotome Fine hair 22.
Ultramicrotomy 23. Ultramicrotomy Knife
24.
Ultramicrotomy 25.
Ultramicrotomy
26. Ultramicrotomy
trimming 27. Ultramicrotomy
28. Ultramicrotomy Cutting Ultramicrotome (a)ultramicrotome(b)cutting 29. Ultramicrotomy
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
36.
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.
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