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Transformation of K2Sb8Q13 and KSb5Q8 Bulk Crystals to Sb2Q3 (Q = S, Se) Nanofibers by Acid–Base Solution Chemistry

  • Hyungseok Lee
    Hyungseok Lee
    School of Chemical and Biological Engineering, and Institute of Chemical Processes, Seoul National University, Seoul 08826, Republic of Korea
    Center for Correlated Electron Systems, Institute for Basic Science (IBS), Seoul 08826, Republic of Korea
  • Byeongjun Yoo
    Byeongjun Yoo
    School of Chemical and Biological Engineering, and Institute of Chemical Processes, Seoul National University, Seoul 08826, Republic of Korea
    Center for Nanoparticle Research, Institute for Basic Science (IBS), Seoul 08826, Republic of Korea
  • Dawoon Kim
    Dawoon Kim
    School of Chemical and Biological Engineering, and Institute of Chemical Processes, Seoul National University, Seoul 08826, Republic of Korea
    Center for Correlated Electron Systems, Institute for Basic Science (IBS), Seoul 08826, Republic of Korea
    More by Dawoon Kim
  • Joonil Cha
    Joonil Cha
    School of Chemical and Biological Engineering, and Institute of Chemical Processes, Seoul National University, Seoul 08826, Republic of Korea
    Center for Correlated Electron Systems, Institute for Basic Science (IBS), Seoul 08826, Republic of Korea
    More by Joonil Cha
  • Yeo Kyung Kang
    Yeo Kyung Kang
    School of Advanced Materials Science & Engineering, Sungkyunkwan University, Suwon 16419, Republic of Korea
  • Sung-Pyo Cho
    Sung-Pyo Cho
    National Center for Inter-University Research Facilities, Seoul National University, Seoul 08826, Republic of Korea
    More by Sung-Pyo Cho
  • Taeghwan Hyeon
    Taeghwan Hyeon
    School of Chemical and Biological Engineering, and Institute of Chemical Processes, Seoul National University, Seoul 08826, Republic of Korea
    Center for Nanoparticle Research, Institute for Basic Science (IBS), Seoul 08826, Republic of Korea
  • Myung-Gil Kim*
    Myung-Gil Kim
    School of Advanced Materials Science & Engineering, Sungkyunkwan University, Suwon 16419, Republic of Korea
    *Email: [email protected]
  • Mercouri G. Kanatzidis*
    Mercouri G. Kanatzidis
    Department of Chemistry, Northwestern University, Evanston, Illinois 60208, United States
    *Email: [email protected]
  • , and 
  • In Chung*
    In Chung
    School of Chemical and Biological Engineering, and Institute of Chemical Processes, Seoul National University, Seoul 08826, Republic of Korea
    Center for Correlated Electron Systems, Institute for Basic Science (IBS), Seoul 08826, Republic of Korea
    *Email: [email protected]
    More by In Chung
Cite this: J. Am. Chem. Soc. 2023, 145, 29, 15951–15962
Publication Date (Web):July 12, 2023
https://doi.org/10.1021/jacs.3c03925
Copyright © 2023 American Chemical Society

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    Abstract

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    The ability to manipulate crystal structures using kinetic control is of broad interest because it enables the design of materials with structures, compositions, and morphologies that may otherwise be unattainable. Herein, we report the low-temperature structural transformation of bulk inorganic crystals driven by hard–soft acid–base (HSAB) chemistry. We show that the three-dimensional framework K2Sb8Q13 and layered KSb5Q8 (Q = S, Se, and Se/S solid solutions) compounds transform to one-dimensional Sb2Q3 nano/microfibers in N2H4·H2O solution by releasing Q2– and K+ ions. At 100 °C and ambient pressure, a transformation process takes place that leads to significant structural changes in the materials, including the formation and breakage of covalent bonds between Sb and Q. Despite the insolubility of the starting crystals in N2H4·H2O under the given conditions, the mechanism of this transformation can be rationalized by applying the HSAB principle. By adjusting factors such as the reactants’ acid/base properties, temperature, and pressure, the process can be controlled, allowing for the achievement of a wide range of optical band gaps (ranging from 1.14 to 1.59 eV) while maintaining the solid solution nature of the anion sublattice in the Sb2Q3 nanofibers.

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    The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/jacs.3c03925.

    • Additional experimental details about analytical techniques, the optimized volumetric ratio of N2H4·H2O solution according to bulk crystals, cell parameters, analyzed compositions, structural motif and crystal structure, SEM-EDS images and corresponding spectra, powder XRD patterns, UV–vis absorption spectra, and TEM-EDS images (PDF)

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