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Sample Preparation Methodologies for In Situ Liquid and Gaseous Cell Analytical Transmission Electron Microscopy of Electropolished Specimens

Published online by Cambridge University Press:  07 November 2016

Xiang Li Zhong ,
Sibylle Schilling ,
Nestor J. Zaluzec  and
M. Grace Burke
Xiang Li Zhong
Affiliation:
School of Materials, Materials Performance Centre· and Electron Microscopy Centre, University of Manchester, Manchester M13 9PL, UK
Sibylle Schilling
Affiliation:
School of Materials, Materials Performance Centre· and Electron Microscopy Centre, University of Manchester, Manchester M13 9PL, UK
Nestor J. Zaluzec*
Affiliation:
School of Materials, Materials Performance Centre· and Electron Microscopy Centre, University of Manchester, Manchester M13 9PL, UK Argonne National Laboratory, Electron Microscopy Center, Center for Nanoscale Materials, Argonne, IL 60439, USA
M. Grace Burke
Affiliation:
School of Materials, Materials Performance Centre· and Electron Microscopy Centre, University of Manchester, Manchester M13 9PL, UK
*
*Corresponding author. [email protected]
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Abstract

In recent years, an increasing number of studies utilizing in situ liquid and/or gaseous cell scanning/transmission electron microscopy (S/TEM) have been reported. Because of the difficulty in the preparation of suitable specimens, these environmental S/TEM studies have been generally limited to studies of nanoscale structured materials such as nanoparticles, nanowires, or sputtered thin films. In this paper, we present two methodologies which have been developed to facilitate the preparation of electron-transparent samples from conventional bulk metals and alloys for in situ liquid/gaseous cell S/TEM experiments. These methods take advantage of combining sequential electrochemical jet polishing followed by focused ion beam extraction techniques to create large electron-transparent areas for site-specific observation. As an example, we illustrate the application of this methodology for the preparation of in situ specimens from a cold-rolled Type 304 austenitic stainless steel sample, which was subsequently examined in both 1 atm of air as well as fully immersed in a H2O environment in the S/TEM followed by hyperspectral imaging. These preparation techniques can be successfully applied as a general procedure for a wide range of metals and alloys, and are suitable for a variety of in situ analytical S/TEM studies in both aqueous and gaseous environments.

Keywords

liquidgasE-cellsample preparationS/TEMAEM
Type
Instrumentation and Software Techniques
Information
Microscopy and Microanalysis , Volume 22 , Issue 6 , December 2016 , pp. 1350 - 1359
Copyright
© Microscopy Society of America 2016 

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