Journal
MICROSCOPY AND MICROANALYSIS
Volume 22, Issue 6, Pages 1350-1359Publisher
CAMBRIDGE UNIV PRESS
DOI: 10.1017/S1431927616011855
Keywords
liquid; gas; E-cell; sample preparation; S/TEM; AEM
Categories
Funding
- Engineering and Physical Sciences Research Council UK PROMINENT program
- Defense Threat Reduction Agency [HDTRA1-12-1-0013]
- BP DRL Innovation Fund
- Electron Microscopy Center in the Center for Nanoscale Materials, a US Department of Energy Office of Science User Facility [DE-AC02-06CH11357]
- [EP/G035954/1]
- [EP/J021172/1]
- EPSRC [EP/J021229/1] Funding Source: UKRI
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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.
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