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

Wen, Haiming; Lin, Yaojun; Seidman, David N.; Schoenung, Julie M.; van Rooyen, Isabella J.; Lavernia, Enrique J.

doi:10.1017/S1431927615014695

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

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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. 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.

Authors:

Wen, Haiming ^[1]; Lin, Yaojun ^[2]; Seidman, David N. ^[3]; Schoenung, Julie M. ^[4]; van Rooyen, Isabella J. ^[5]; Lavernia, Enrique J. ^[4]

Univ. of California, Davis, CA (United States); Northwestern Univ., Evanston, IL (United States); Idaho National Lab. (INL), Idaho Falls, ID (United States)
Yanshan Univ., Hebei (People's Republic of China)
Northwestern Univ., Evanston, IL (United States)
Univ. of California, Davis, CA (United States)
Idaho National Lab. (INL), Idaho Falls, ID (United States)

Publication Date:: Wed Sep 09 00:00:00 EDT 2015

Research Org.:: Idaho National Lab. (INL), Idaho Falls, ID (United States)

Sponsoring Org.:: USDOE

OSTI Identifier:: 1259463

Report Number(s):: INL/JOU-14-33403
Journal ID: ISSN 1431-9276; applab; PII: S1431927615014695

Grant/Contract Number:: AC07-05ID14517

Resource Type:: Accepted Manuscript

Journal Name:: Microscopy and Microanalysis

Additional Journal Information:: Journal Volume: 21; Journal Issue: 05; Journal ID: ISSN 1431-9276

Publisher:: Microscopy Society of America (MSA)

Country of Publication:: United States

Language:: English

Subject:: 22 GENERAL STUDIES OF NUCLEAR REACTORS; TEM; sample preparation; powders; epoxy; dimpling; ion milling

Citation Formats


                    Wen, Haiming, Lin, Yaojun, Seidman, David N., Schoenung, Julie M., van Rooyen, Isabella J., and Lavernia, Enrique J. An efficient and cost-effective method for preparing transmission electron microscopy samples from powders.  United States: N. p., 2015. 
Web.  doi:10.1017/S1431927615014695.

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                    Wen, Haiming, Lin, Yaojun, Seidman, David N., Schoenung, Julie M., van Rooyen, Isabella J., & Lavernia, Enrique J. An efficient and cost-effective method for preparing transmission electron microscopy samples from powders.  United States.  https://doi.org/10.1017/S1431927615014695

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                    Wen, Haiming, Lin, Yaojun, Seidman, David N., Schoenung, Julie M., van Rooyen, Isabella J., and Lavernia, Enrique J. Wed .  
"An efficient and cost-effective method for preparing transmission electron microscopy samples from powders".  United States.  https://doi.org/10.1017/S1431927615014695.  https://www.osti.gov/servlets/purl/1259463.

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@article{osti_1259463,

  title        = {An efficient and cost-effective method for preparing transmission electron microscopy samples from powders},

  author       = {Wen, Haiming and Lin, Yaojun and Seidman, David N. and Schoenung, Julie M. and van Rooyen, Isabella J. and Lavernia, Enrique J.},

  abstractNote = {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.},

  doi          = {10.1017/S1431927615014695},

  journal      = {Microscopy and Microanalysis},

  number       = 05,

  volume       = 21,

  place        = {United States},

  year         = {Wed Sep 09 00:00:00 EDT 2015},

  month        = {Wed Sep 09 00:00:00 EDT 2015}

}

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