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Preparation of Cross Sections of Diffi cult Materials for SEM Imaging


wire. Because the epoxy layer is very thin at the top and bottom of the wire, the wire may detach from the epoxy; if it does, recut in another area. Polish the cut end of the wire. Procedure for embedding larger irregular single


particles . Press down the Aclar  fi lm epoxy to the surface of the particle. When trimming, cut through the particle if possible to expose some of the interior for polishing. Aſt er trimming, the edge of the epoxy wafer can be shaved with a razor blade to expose more of the interior area of interest. Polish the exposed particle ( Figures 4 and 5 ).


Micrographs were taken using either a JEOL JSM-6490LV variable-pressure SEM or a JEOL JSM-7600F fi eld-emission SEM (JEOL USA, Peabody, Massachusetts).


Results


High-quality SEM images can be obtained from samples embedded in commercial epoxy and polished with an argon-beam cross-sectional polisher. Wire cross sections of copper alloys, like most metals, exhibit polycrystalline grain structure, and grain size is readily discernable after polishing ( Figure 3 ). Polishing a powder results in smooth cross sections of many powder particles (for example, diatomaceous earth, Figure 4 ). Epoxy embedding holds larger particles firmly for polishing. The iron-impregnated carbon particles illustrated in Figure 5 are extremely hard and difficult to hold. Other methods to view the interior structure had been unsuccessful.


Discussion


The transparent epoxy holds the sample material firmly, and accurate alignment is simplified so that the structures to be polished can be selected with precision. Pressing down the liquid epoxy makes the final preparation thin, eliminating the need for prolonged polishing to an excessive depth in order to reach the object(s). The pressing also concentrates as many powder grains as possible in the smallest possible amount of matrix. Argon-beam cross-section polishing does not introduce artifacts such as smearing or mechanical deformation [ 3 ].


Conclusion


Embedding in a thin layer of transparent consumer epoxy makes cross-sectional polishing using a broad argon beam simpler and more consistent, enabling good scanning electron microscopy of cross sections on a variety of diffi cult sample types.


Acknowledgments


This material is based on work supported by the National Science Foundation under Grants No. 0619098 and 0923354.


References [1] N Erdman et al ., Adv Mater Process 164 ( 6 ) ( 2006 ) 33 – 35 . [2] N Erdman et al ., Microscopy Today 14 ( 3 ) ( 2006 ) 22 – 25 . [3] N Erdman et al ., Adv Mater Process 168 ( 2 ) ( 2010 ) 14 – 15 .


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44 www.microscopy-today.com • 2018 May


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