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Novel Method for Preparing Transmission Electron Microscopy Samples of Micrometer-Sized Powder Particles by Using Focused Ion Beam

Part of: Micrographia Collection

Published online by Cambridge University Press:  13 September 2017

Tae-Hoon Kim ,
Min-Chul Kang ,
Ga-Bin Jung ,
Dong Soo Kim  and
Cheol-Woong Yang
Tae-Hoon Kim
Affiliation:
School of Advanced Materials Science and Engineering, Sungkyunkwan University, Suwon 16419, Korea
Min-Chul Kang
Affiliation:
School of Advanced Materials Science and Engineering, Sungkyunkwan University, Suwon 16419, Korea
Ga-Bin Jung
Affiliation:
School of Advanced Materials Science and Engineering, Sungkyunkwan University, Suwon 16419, Korea
Dong Soo Kim
Affiliation:
Powder & Ceramics Division, Korea Institute of Materials Science, Changwon 51508, Korea Metals Technology Research Department, Convergence Research Center for Development of Mineral Resources, Korea Institute of Geoscience and Mineral Resources, Daejeon 34132, Korea
Cheol-Woong Yang*
Affiliation:
School of Advanced Materials Science and Engineering, Sungkyunkwan University, Suwon 16419, Korea
*
*Corresponding author. [email protected]
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Abstract

The preparation of transmission electron microscopy (TEM) samples from powders is quite difficult and challenging. For powders with particles in the 1–5 μm size range, it is especially difficult to select an adequate sample preparation technique. Epoxy is commonly used to bind powder, but drawbacks, such as differential milling originating from unequal milling rates between the epoxy and powder, remain. We propose a new, simple method for preparing TEM samples. This method is especially useful for powders with particles in the 1–5 μm size range that are vulnerable to oxidation. The method uses solder as an embedding agent together with focused ion beam (FIB) milling. The powder was embedded in low-temperature solder using a conventional hot-mounting instrument. Subsequently, FIB was used to fabricate thin TEM samples via the lift-out technique. The solder proved to be more effective than epoxy in producing thin TEM samples with large areas. The problem of differential milling was mitigated, and the solder binder was more stable than epoxy under an electron beam. This methodology can be applied for preparing TEM samples from various powders that are either vulnerable to oxidation or composed of high atomic number elements.

Keywords

TEM sample preparationsolderFIB millingpowderoxidation
Type
Micrographia
Information
Microscopy and Microanalysis , Volume 23 , Issue 5 , October 2017 , pp. 1055 - 1060
Copyright
© Microscopy Society of America 2017 

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