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Title: An efficient and cost-effective method for preparing transmission electron microscopy samples from powders

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. Furthermore, our methodology has been applied successfully for preparing TEM samples with large thin areas and high quality for many different mechanically milled metallic powders.
 [1] ;  [2] ;  [3] ;  [4] ;  [5] ;  [4]
  1. Univ. of California, Davis, CA (United States); Northwestern Univ., Evanston, IL (United States); Idaho National Lab. (INL), Idaho Falls, ID (United States)
  2. Yanshan Univ., Hebei (People's Republic of China)
  3. Northwestern Univ., Evanston, IL (United States)
  4. Univ. of California, Davis, CA (United States)
  5. Idaho National Lab. (INL), Idaho Falls, ID (United States)
Publication Date:
Report Number(s):
Journal ID: ISSN 1431-9276; applab; PII: S1431927615014695
Grant/Contract Number:
Accepted Manuscript
Journal Name:
Microscopy and Microanalysis
Additional Journal Information:
Journal Volume: 21; Journal Issue: 05; Journal ID: ISSN 1431-9276
Microscopy Society of America (MSA)
Research Org:
Idaho National Lab. (INL), Idaho Falls, ID (United States)
Sponsoring Org:
Country of Publication:
United States
22 GENERAL STUDIES OF NUCLEAR REACTORS; TEM; sample preparation; powders; epoxy; dimpling; ion milling
OSTI Identifier: