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Structure Determination of Superatom Metallic Clusters Using Rapid Scanning Electron Diffraction

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Department of Physics and Astronomy, The University of Texas at San Antonio, One UTSA Circle, San Antonio, 78249, United States
School of Chemical Sciences, National University of Cordoba, Avenue Haya de la Torre Cordoba, Cordoba, 5000, Argentina
*(M.J.-Y.) E-mail: [email protected]
Cite this: J. Phys. Chem. C 2016, 120, 3, 1902–1908
Publication Date (Web):January 7, 2016
https://doi.org/10.1021/acs.jpcc.5b09524
Copyright © 2016 American Chemical Society

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    Abstract

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    Experimental analysis of electron diffraction patterns for ligand-stabilized gold clusters in transmission electron microscopy is a cumbersome procedure, due to electron beam–induced irradiation damage. We propose herein a method for instantaneous data collection using scanning nanobeam electron diffraction and the subsequent determination of the crystal metallic clusters. The procedure has been tested on a known structure, namely Au102(p-MBA)44 nanoclusters and has been compared with their structure theoretically determined by ones previously obtained from X-ray diffraction analysis. The method can be unambiguously applied for the case of any nanoscale system susceptible to electron beam damage and it is capable to register the rotation effect on the metallic clusters caused due to the electron beam interaction during the raster scanning on the sample.

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    The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.jpcc.5b09524.

    • ESI–MS experimental details, NBD patterns acquired with a typical CCD camera, details related to the image processing algorithm (PDF)

    • Video showing the whole area of the electron diffraction patterns (MPG)

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    Cited By

    This article is cited by 11 publications.

    1. Ryo Takahata, Seiji Yamazoe, Yosuke Maehara, Kenji Yamazaki, Shinjiro Takano, Wataru Kurashige, Yuichi Negishi, Kazutoshi Gohara, Tatsuya Tsukuda. Electron Microscopic Observation of an Icosahedral Au13 Core in Au25(SePh)18 and Reversible Isomerization between Icosahedral and Face-Centered Cubic Cores in Au144(SC2H4Ph)60. The Journal of Physical Chemistry C 2020, 124 (12) , 6907-6912. https://doi.org/10.1021/acs.jpcc.9b11412
    2. David M. Black, Marcos M. Alvarez, Fangzhi Yan, Wendell P. Griffith, Germán Plascencia-Villa, Stephan B. H. Bach, and Robert L. Whetten . Triethylamine Solution for the Intractability of Aqueous Gold–Thiolate Cluster Anions: How Ion Pairing Enhances ESI-MS and HPLC of aq-Aun(pMBA)p. The Journal of Physical Chemistry C 2017, 121 (20) , 10851-10857. https://doi.org/10.1021/acs.jpcc.6b12073
    3. Marcos M. Alvarez, Jenny Chen, Germán Plascencia-Villa, David M. Black, Wendell P. Griffith, Ignacio L. Garzón, Miguel José-Yacamán, Borries Demeler, and Robert L. Whetten . Hidden Components in Aqueous “Gold-144” Fractionated by PAGE: High-Resolution Orbitrap ESI-MS Identifies the Gold-102 and Higher All-Aromatic Au-pMBA Cluster Compounds. The Journal of Physical Chemistry B 2016, 120 (26) , 6430-6438. https://doi.org/10.1021/acs.jpcb.6b04525
    4. Liang Qiao, Nia Pollard, Ravithree D. Senanayake, Zhi Yang, Minjung Kim, Arzeena S. Ali, Minh Tam Hoang, Nan Yao, Yimo Han, Rigoberto Hernandez, Andre Z. Clayborne, Matthew R. Jones. Atomically precise nanoclusters predominantly seed gold nanoparticle syntheses. Nature Communications 2023, 14 (1) https://doi.org/10.1038/s41467-023-40016-3
    5. Alexandra Bruefach, Colin Ophus, Mary C Scott. Analysis of Interpretable Data Representations for 4D-STEM Using Unsupervised Learning. Microscopy and Microanalysis 2022, 28 (6) , 1998-2008. https://doi.org/10.1017/S1431927622012259
    6. Celina Sikorska, Nicola Gaston. Modified Lennard‐Jones potentials for nanoscale atoms. Journal of Computational Chemistry 2020, 41 (22) , 1985-2000. https://doi.org/10.1002/jcc.26368
    7. Colin Ophus. Four-Dimensional Scanning Transmission Electron Microscopy (4D-STEM): From Scanning Nanodiffraction to Ptychography and Beyond. Microscopy and Microanalysis 2019, 25 (3) , 563-582. https://doi.org/10.1017/S1431927619000497
    8. Yoshiki Niihori, Kana Yoshida, Sakiat Hossain, Wataru Kurashige, Yuichi Negishi. Deepening the Understanding of Thiolate-Protected Metal Clusters Using High-Performance Liquid Chromatography. Bulletin of the Chemical Society of Japan 2019, 92 (3) , 664-695. https://doi.org/10.1246/bcsj.20180357
    9. Alejandra Londoño-Calderon, Arturo Ponce, Ulises Santiago, Sergio Mejia, Miguel José-Yacamán. Controlling the Number of Atoms on Catalytic Metallic Clusters. 2017, 185-220. https://doi.org/10.1016/B978-0-12-805090-3.00006-1
    10. Eduardo Ortega, Arturo Ponce, Ulises Santiago, Diego Alducin, Alfredo Benitez-Lara, Germán Plascencia-Villa, Miguel José-Yacamán. Structural damage reduction in protected gold clusters by electron diffraction methods. Advanced Structural and Chemical Imaging 2016, 2 (1) https://doi.org/10.1186/s40679-016-0026-x
    11. C. Heath Turner, Yu Lei, Yuping Bao. Modeling the atomistic growth behavior of gold nanoparticles in solution. Nanoscale 2016, 8 (17) , 9354-9365. https://doi.org/10.1039/C6NR01881E

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