MSE 510 – Microstructural Characterization

Techniques - Lecture 19
• Sample preparation for TEM

Apr. 2, 2020 1
Take good care of yourself – part 2

2
Take good care of yourself – part 2

https://youtu.be/6Mem4zvfizw https://youtu.be/sV0NVrJ0PjI
TEM Sample Preparation
• What types of materials are we analyzing?

• What are the specific details of the specimen we are interested in

analyzing? Are there specific areas of interest that we need to focus
on?

• What type of information are we interested in obtaining?

TEM Sample Preparation – Specimen
• Self-supporting disk

• Grid

Williams & Carter, 1996.

FIB Grid
TEM Self-Supporting Disk
• Preparation:
TEM Self-Supporting Disk: Initial thinning
• Method selected depends on material characteristics (brittle, ductile, soft,
single phase, composite, etc.) and what you are interested in studying.
 TEM Self-Supporting Disk:
Cut / Punch 3mm disk
Williams & Carter, 1996.
• If material is ductile and mechanical damage is not crucial (at least
around the edges), a mechanical punch can be used.

• If material is brittle there are 3 main methods of sample preparation:

TEM Self-Supporting Disk:
Pre-Thin Central Region of Disk
• Purpose:
• Any damage created during this stage must be removed
later.
• Commercial dimplers:

Specimen

Robins, Fishione, 2013.

TEM Self-Supporting Disk: Final Thinning
• Electropolishing
• Ion Milling
 TEM Self-Supporting Disk: Final Thinning
Electropolishing (Jet Polishing)
• Only be used for conductive specimens (metals, alloys)
• Produces foils with no mechanical damage
• Can change surface chemistry
• Dangerous chemicals
• How it works:

Williams & Carter, 1996.

Robins, Fishione, 2013.
TEM Self-Supporting Disk: Final Thinning
Ion Milling

Williams & Carter, 1996.

Comparison of Ion Milling Energies

From: D. Laub, 2014

Cross-sectional TEM Specimen

Williams & Carter, 1996.

Specimens on Grids / Washers
• Electropolishing – Window method for metals
and alloys
• Focused Ion Beam (FIB)
• Ultramicrotomy
• Grinding and crushing
• Replication and extraction
• Cleaving
• 90o Wedge, Lithography, Preferential chemical
etching (See Williams & Carter)
Electropolishing – Window method for metals
and alloys
 Conventionally prepared FIB TEM specimen
(cross section method) <100 nm

Focused Ion Beam

Giannuzzi and Stevie, Micron 30 (1999) 196-204.

FIB TEM specimen (lift out method)

FIB Grid

F. Bobard, M. Cantoni, CIME-EPFL!

TEM Samples preparation_D.Laub_2014
FIB and Nanomilling Comparison

Robins, Fischione, 2013.

Ultramicrotomy
TEM Samples preparation_D.Laub_2014
Grinding and Crushing
Replication and Extraction
Cleaving
Williams & Carter
Final thoughts on sample preparation
• Ultimately, there are many different types of sample preparation.
• Want to think about the information that we intend to obtain from
the specimen and the techniques that we are using.
• Want to consider any influence on the sample that the preparation
techniques may impose.