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An Efficient and Cost-Effective Method for Preparing Transmission Electron Microscopy Samples from Powders

Published online by Cambridge University Press:  09 September 2015

Haiming Wen ,
Yaojun Lin ,
David N. Seidman ,
Julie M. Schoenung ,
Isabella J. van Rooyen  and
Enrique J. Lavernia
Haiming Wen*
Affiliation:
Department of Chemical Engineering and Materials Science, University of California at Davis, Davis, CA 95616, USA Department of Materials Science and Engineering, Northwestern University, Evanston, IL 60208-3108, USA Idaho National Laboratory, Fuel Performance and Design Department, Idaho Falls, ID 83415-6188, USA
Yaojun Lin
Affiliation:
State Key Laboratory of Metastable Materials Science and Technology and College of Materials Science and Engineering, Yanshan University, Qinhuangdao, Hebei 066004, P.R. China
David N. Seidman
Affiliation:
Department of Materials Science and Engineering, Northwestern University, Evanston, IL 60208-3108, USA Northwestern University Center for Atom Probe Tomography (NUCAPT), Evanston, IL 60208-3108, USA
Julie M. Schoenung
Affiliation:
Department of Chemical Engineering and Materials Science, University of California at Davis, Davis, CA 95616, USA
Isabella J. van Rooyen
Affiliation:
Idaho National Laboratory, Fuel Performance and Design Department, Idaho Falls, ID 83415-6188, USA
Enrique J. Lavernia
Affiliation:
Department of Chemical Engineering and Materials Science, University of California at Davis, Davis, CA 95616, USA
*
*Corresponding authors. hmwen@ucdavis.edu; haiming.wen@inl.gov
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Abstract

The preparation of transmission electron microcopy (TEM) samples from powders with particle sizes larger than ~100 nm poses a challenge. The existing methods are complicated and expensive, or have a low probability of success. Herein, we report a modified methodology for preparation of TEM samples from powders, which is efficient, cost-effective, and easy to perform. This method involves mixing powders with an epoxy on a piece of weighing paper, curing the powder–epoxy mixture to form a bulk material, grinding the bulk to obtain a thin foil, punching TEM discs from the foil, dimpling the discs, and ion milling the dimpled discs to electron transparency. Compared with the well established and robust grinding–dimpling–ion-milling method for TEM sample preparation for bulk materials, our modified approach for preparing TEM samples from powders only requires two additional simple steps. In this article, step-by-step procedures for our methodology are described in detail, and important strategies to ensure success are elucidated. Our methodology has been applied successfully for preparing TEM samples with large thin areas and high quality for many different mechanically milled metallic powders.

Keywords

TEMsample preparationpowdersepoxyion milling
Type
Equipment and Software Development
Information
Microscopy and Microanalysis , Volume 21 , Issue 5 , October 2015 , pp. 1184 - 1194
Copyright
© Microscopy Society of America 2015 

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