A versatile and reproducible cryo-sample preparation methodology for atom probe studies
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Published version
Author(s)
Type
Journal Article
Abstract
Repeatable and reliable site-specific preparation of specimens for atom probe tomography (APT) at cryogenic temperatures has proven challenging. A generalized workflow is required for cryogenic specimen preparation including lift-out via focused ion beam and in situ deposition of capping layers, to strengthen specimens that will be exposed to high electric field and stresses during field evaporation in APT and protect them from environment during transfer into the atom probe. Here, we build on existing protocols and showcase preparation and analysis of a variety of metals, oxides, and supported frozen liquids and battery materials. We demonstrate reliable in situ deposition of a metallic capping layer that significantly improves the atom probe data quality for challenging material systems, particularly battery cathode materials which are subjected to delithiation during the atom probe analysis itself. Our workflow design is versatile and transferable widely to other instruments.
Date Issued
2023-12-21
Date Acceptance
2023-10-01
Citation
Microscopy and Microanalysis, 2023, 29 (6), pp.1992-2003
ISSN
1083-0375
Publisher
Oxford University Press
Start Page
1992
End Page
2003
Journal / Book Title
Microscopy and Microanalysis
Volume
29
Issue
6
Copyright Statement
© The Author(s) 2023. Published by Oxford University Press on behalf of the Microscopy Society of America.
This is an Open Access article distributed under the terms of the Creative Commons Attribution License (https://creativecommons.org/licenses/by/4.0/), which
permits unrestricted reuse, distribution, and reproduction in any medium, provided the original work is properly cited.
This is an Open Access article distributed under the terms of the Creative Commons Attribution License (https://creativecommons.org/licenses/by/4.0/), which
permits unrestricted reuse, distribution, and reproduction in any medium, provided the original work is properly cited.
License URL
Identifier
https://www.ncbi.nlm.nih.gov/pubmed/37856778
PII: 7324651
Subjects
atom probe tomography
battery cathodes
cryo-focused ion beam
frozen liquids
Publication Status
Published
Coverage Spatial
England
Date Publish Online
2023-10-19
