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Detecting structural variances of Co₃O₄ catalysts by controlling beam-induced sample alterations in the vacuum of a transmission electron microscope

Kisielowski, C. and Frei, H. and Specht, P. and Sharp, I. D. and Haber, J. A. and Helveg, S. (2016) Detecting structural variances of Co₃O₄ catalysts by controlling beam-induced sample alterations in the vacuum of a transmission electron microscope. Advanced Structural and Chemical Imaging, 2 . Art. No. 13. ISSN 2198-0926. PMCID PMC5093192. doi:10.1186/s40679-016-0027-9.

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This article summarizes core aspects of beam-sample interactions in research that aims at exploiting the ability to detect single atoms at atomic resolution by mid-voltage transmission electron microscopy. Investigating the atomic structure of catalytic Co₃O₄ nanocrystals underscores how indispensable it is to rigorously control electron dose rates and total doses to understand native material properties on this scale. We apply in-line holography with variable dose rates to achieve this goal. Genuine object structures can be maintained if dose rates below ~100 e/Ų s are used and the contrast required for detection of single atoms is generated by capturing large image series. Threshold doses for the detection of single atoms are estimated. An increase of electron dose rates and total doses to common values for high resolution imaging of solids stimulates object excitations that restructure surfaces, interfaces, and defects and cause grain reorientation or growth. We observe a variety of previously unknown atom configurations in surface proximity of the Co₃O₄ spinel structure. These are hidden behind broadened diffraction patterns in reciprocal space but become visible in real space by solving the phase problem. An exposure of the Co₃O₄ spinel structure to water vapor or other gases induces drastic structure alterations that can be captured in this manner.

Item Type:Article
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URLURL TypeDescription CentralArticle
Kisielowski, C.0000-0001-6425-0779
Sharp, I. D.0000-0001-5238-7487
Haber, J. A.0000-0001-7847-5506
Additional Information:© 2016 The Author(s). This article is distributed under the terms of the Creative Commons Attribution 4.0 International License (, which permits unrestricted use, distribution, and reproduction in any medium, provided you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons license, and indicate if changes were made. Received: 25 June 2016. Accepted: 19 October 2016. Published: 2 November 2016. Authors’ contributions: CK recorded and reconstructed the images and drafted the manuscript. PS and SH contributed to the image interpretations. HF, JH and IS provided the differently grown Co_3O_4 material. All authors commented on the manuscript. All authors read and approved the final manuscript. Electron microscopy is supported by the Molecular Foundry, which is supported by the Office of Science, the Office of Basic Energy Sciences, the U.S. Department of Energy under Contract No. DE-AC02-05CH11231. The samples were provided by the Joint Center for Artificial Photosynthesis, a DOE Energy Innovation Hub, supported through the Office of Science of the U.S. Department of Energy under Award No. DE-SC000499. In situ annealing experiments were kindly supported by Haldor Topsoe A/S, Denmark. The authors acknowledge Dr. Jinhui Yang for performing plasma-enhanced ALD. The authors declare that they have no competing interests.
Funding AgencyGrant Number
Department of Energy (DOE)DE-AC02-05CH11231
Department of Energy (DOE)DE-SC000499
Haldor Topsoe A/S DenmarkUNSPECIFIED
PubMed Central ID:PMC5093192
Record Number:CaltechAUTHORS:20161109-115755580
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Official Citation:Detecting structural variances of Co3O4 catalysts by controlling beam-induced sample alterations in the vacuum of a transmission electron microscope C. Kisielowski, H. Frei, P. Specht, I. D. Sharp, J. A. Haber and S. Helveg Advanced Structural and Chemical Imaging20162:13 DOI: 10.1186/s40679-016-0027-9
Usage Policy:No commercial reproduction, distribution, display or performance rights in this work are provided.
ID Code:71886
Deposited By: Ruth Sustaita
Deposited On:09 Nov 2016 21:06
Last Modified:08 Apr 2022 18:26

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