4.5 Article

Using Xe Plasma FIB for High-Quality TEM Sample Preparation

Journal

MICROSCOPY AND MICROANALYSIS
Volume 28, Issue 3, Pages 646-658

Publisher

CAMBRIDGE UNIV PRESS
DOI: 10.1017/S1431927622000344

Keywords

EELS; FIB; gallium; PFIB; TEM sample preparation; xenon

Funding

  1. U.S. Department of Energy's National Nuclear Security Administration [DE-NA0003525]

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This study compared TEM samples prepared with gallium and xenon focused ion beams to determine if both ion species can produce equivalent quality samples. The results showed that despite the different preparation techniques, high-quality TEM samples can be obtained using xenon focused ion beam. The study also provided best practices for TEM sample preparation using xenon focused ion beam.
A direct comparison between electron transparent transmission electron microscope (TEM) samples prepared with gallium (Ga) and xenon (Xe) focused ion beams (FIBs) is performed to determine if equivalent quality samples can be prepared with both ion species. We prepared samples using Ga FIB and Xe plasma focused ion beam (PFIB) while altering a variety of different deposition and milling parameters. The samples' final thicknesses were evaluated using STEM-EELS t/lambda data. Using the Ga FIB sample as a standard, we compared the Xe PFIB samples to the standard and to each other. We show that although the Xe PFIB sample preparation technique is quite different from the Ga FIB technique, it is possible to produce high-quality, large area TEM samples with Xe PFIB. We also describe best practices for a Xe PFIB TEM sample preparation workflow to enable consistent success for any thoughtful FIB operator. For Xe PFIB, we show that a decision must be made between the ultimate sample thickness and the size of the electron transparent region.

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