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Transmission Electron Microscopy Specimen Preparation of Delicate Materials Using Tripod Polisher
Applied Microscopy 2016;46:110-5
Published online June 30, 2016
© 2016 Korean Society of Microscopy.

Hyun-Woo Cha, Min-Chul Kang, Keesam Shin1, and Cheol-Woong Yang*

School of Advanced Materials Science & Engineering, Sungkyunkwan University, Suwon 16419, Korea, 1School of Nano and Advanced Materials Engineering, Changwon National University, Changwon 51140, Korea
Correspondence to: Yang CW, Tel: +82-31-290-7362, Fax: +82-31-290-7371, E-mail: cwyang@skku.edu
Received May 30, 2016; Revised June 23, 2016; Accepted June 23, 2016.
This is an open-access article distributed under the terms of the Creative Commons Attribution Non-Commercial License (http://creativecommons.org/licenses/by-nc/4.0) which permits unrestricted noncommercial use, distribution, and reproduction in any medium, provided the original work is properly cited.
Abstract

Transmission electron microscopy (TEM) is a powerful tool for analyzing a broad range of materials and provides localized information about the microstructure. However, the analysis results are strongly influenced by the quality of the thin foil specimen. Sample preparation for TEM analysis requires considerable skill, especially when the area of interest is small or the material of interest is difficult to thin because of its high hardness and its mechanical instability when thinned. This article selectively reviews recent advances in TEM sample preparation techniques using a tripod polisher. In particular, it introduces two typical types (flat type and wedge type) of TEM sample preparation and the benefits and drawbacks of each method; finally, a method of making better samples for TEM analysis is suggested.

Keywords : Tripod polisher, Flat-type polishing, Wedge-type polishing, Hard materials, Sample preparation
Figures
Fig. 1. Schematic of tripod polisher and specimens for flat-type (A, B) and wedge-type (C, D) polishing. TEM, transmission electron microscopy.
Fig. 2. Tripod polishing procedure. Reference plane preparation for flat-and wedge-type polishing (A-C) and wedge-type polishing (D?F) method. (A) Mounting specimen on Pyrex glass, (B) fixing Pyrex glass on tripod, (C) polishing a reference plane, (D) remounting on edge-cut Pyrex glass, (E) fixing Pyrex glass on L-bracket, and (F) thinning the wedge specimen at a slight angle.
Fig. 3. Schematic of specimen mounting configurations for wedge-type polishing: (A) parallel, (B) oblique, and (C) perpendicular mounting.
Fig. 4. Schematic of specimen mounting for wedge-type polishing. A specimen, the reference plane of which has been polished, is mounted on the dummy transmission electron microscopy grid with an excess amount of thermal wax. The dummy grid and thermal wax protect the specimen from the risk of film delamination and cracking during polishing. Then the specimen is polished at a slight angle known as the wedge angle.
Fig. 5. Optical microscopy image of wedge-type polished Ni-SiC sample. Thickness fringes (red arrows) appear at the edge when the specimen becomes thin enough. The thin Ni layer is not visible because of the limited resolution of optical microscopy.
Fig. 6. Transmission electron microscopy (TEM) images of sample prepared by wedge-type polishing and low-energy ion milling. (A) Ni-SiC interface specimen. Inset is a high-resolution TEM image of Ni-SiC interface. (B) Si-selective epitaxial growth (SEG) pattern and high-resolution TEM image (inset).
References
  1. Ayache, J, Beaunier, L, Boumendil, J, Ehret, G, and Laub, D (2010). Sample Preparation Handbook for Transmission Electron Microscopy: Techniques. Berlin: Springer
  2. Barna, A, Radnoczi, G, and Pecz, B (1997). Sample preparation techniques for TEM Handbook for Microscopy Vol 3 Applications, Amelinckx, S, Dyck van, D, Landuyt van, J, and Tendeloo van, G, ed. Weinheim: Wiley-VCH Verlag GmbH, pp. 751-801
  3. Chen, J, and Ivey, DG (2002). Preparation of metallized GaN/sapphire cross sections for TEM analysis using wedge polishing. Micron. 33, 489-492.
    Pubmed CrossRef
  4. Goodhew, PJ (1985). Thin Foil Preparation for Transmission Electron Microscopy. Amsterdam: Elsevier
  5. Hirsch, PB, Nicholson, RB, Howie, A, Pashley, DW, and Whelan, MJ (1965). Electron Microscopy of Thin Crystals. London: Butterworths
  6. Kato, NI (2004). Reducing focused ion beam damage to transmission electron microscopy samples. J Electron Microsc. 53, 451-458.
    CrossRef
  7. Klepeis, SJ, Benedict, JP, and Anderson, RM (1987). Specimen Preparation for Transmission Electron Microscopy, Bravman, JC, Anderson, RM, and McDonald, ML, ed. Pittsburgh: Materials Research Society, pp. 179-184
  8. Srot, V, Gec, M, Aken van, PA, Jeon, JH, and ?eh, M (2014). Influence of TEM specimen preparation on chemical composition of Pb (Mg 1/3 Nb 2/3) O 3?PbTiO 3 single crystals. Micron. 62, 37-42.
    Pubmed CrossRef
  9. Voyles, P, Grazul, J, and Muller, D (2003). Imaging of individual atoms inside crystals with ADF-STEM. Ultramicroscopy. 96, 251-273.
    Pubmed CrossRef
  10. Williams, DB, and Carter, CB (2009). Transmission Electron Microscopy: A Text Book for Materials Science. New York: Springer
    CrossRef


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