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Topotactic Reduction-Induced Stabilization of β-La2Mo2O8.68 Phase: Structure, Static Oxygen Disorder, and Electrical Properties

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Download Hi-Res ImageDownload to MS-PowerPointCite This:Inorg. Chem. 2024, 63, 48, 22667-22676
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    Topotactic Reduction-Induced Stabilization of β-La2Mo2O8.68 Phase: Structure, Static Oxygen Disorder, and Electrical Properties
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    • Xueting Zhang
      Xueting Zhang
      MOE Key Laboratory of New Processing Technology for Nonferrous Metals and Materials, Guangxi Universities Key Laboratory of Non-ferrous Metal Oxide Electronic Functional Materials and Devices, College of Materials Science and Engineering, Guilin University of Technology, Guilin 541004, PR China
      More by Xueting Zhang
    • Cecile Genevois
      Cecile Genevois
      CNRS, CEMHTI, UPR 3079, Université Orléans, Orléans F-45071, France
      More by Cecile Genevois
    • Cheng Li
      Cheng Li
      Neutron Scattering Division, Oak Ridge National Laboratory, 1 Bethel Valley Rd, Oak Ridge, Tennessee 37830, United States
      More by Cheng Li
      Orcidhttps://orcid.org/0000-0002-6546-6413
    • Xiaoyan Yang
      Xiaoyan Yang
      MOE Key Laboratory of New Processing Technology for Nonferrous Metals and Materials, Guangxi Universities Key Laboratory of Non-ferrous Metal Oxide Electronic Functional Materials and Devices, College of Materials Science and Engineering, Guilin University of Technology, Guilin 541004, PR China
      Guangxi Key Laboratory of Electrochemical and Magnetochemical Functional Materials, College of Chemistry and Bioengineering, Guilin University of Technology, Guilin 541004, P. R. China
      More by Xiaoyan Yang
      Orcidhttps://orcid.org/0000-0003-2493-7079
    • Michael J. Pitcher
      Michael J. Pitcher
      CNRS, CEMHTI, UPR 3079, Université Orléans, Orléans F-45071, France
      More by Michael J. Pitcher
      Orcidhttps://orcid.org/0000-0003-2044-6774
    • Mathieu Allix
      Mathieu Allix
      CNRS, CEMHTI, UPR 3079, Université Orléans, Orléans F-45071, France
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      Orcidhttps://orcid.org/0000-0001-9317-1316
    • Xiaojun Kuang*
      Xiaojun Kuang
      MOE Key Laboratory of New Processing Technology for Nonferrous Metals and Materials, Guangxi Universities Key Laboratory of Non-ferrous Metal Oxide Electronic Functional Materials and Devices, College of Materials Science and Engineering, Guilin University of Technology, Guilin 541004, PR China
      Guangxi Key Laboratory of Electrochemical and Magnetochemical Functional Materials, College of Chemistry and Bioengineering, Guilin University of Technology, Guilin 541004, P. R. China
      *E-mail: [email protected]
      More by Xiaojun Kuang
      Orcidhttps://orcid.org/0000-0003-2975-9355
    • Alberto J. Fernández-Carrión*
      Alberto J. Fernández-Carrión
      MOE Key Laboratory of New Processing Technology for Nonferrous Metals and Materials, Guangxi Universities Key Laboratory of Non-ferrous Metal Oxide Electronic Functional Materials and Devices, College of Materials Science and Engineering, Guilin University of Technology, Guilin 541004, PR China
      Departamento de Química Inorgánica and Instituto de Ciencia de Materiales de Sevilla (ICMS), Centro Mixto CSIC-Universidad de Sevilla, Av. Américo Vespucio, 49, Sevilla 41092, Spain
      LE STUDIUM Loire Valley Institute for Advanced Studies, Centre-Val de Loire region, Orleans 45000, France
      *E-mail: [email protected]
      More by Alberto J. Fernández-Carrión
      Orcidhttps://orcid.org/0000-0001-8320-2828
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    Inorganic Chemistry

    Cite this: Inorg. Chem. 2024, 63, 48, 22667–22676
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    https://doi.org/10.1021/acs.inorgchem.4c02151
    Published November 19, 2024
    Copyright © 2024 American Chemical Society
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    Abstract

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    La2Mo2O9 is acknowledged as an exceptional oxide ion conductor. It undergoes a reversible phase transition around 580 °C from the nonconductive low-temperature monoclinic α-La2Mo2O9 phase to the highly conductive high-temperature cubic β-La2Mo2O9 phase. In addition, La2Mo2O9 demonstrates complex chemistry under reducing conditions. This study reports, for the first time, the stabilization at ambient temperature of a novel cubic phase through a topotactic reduction of α-La2Mo2O9 employing CaH2. This phase contains approximately ∼3 atom % oxygen vacancies relative to the nominal composition (La2Mo2O8.68(1)). The cubic symmetry is associated with a static distribution of these vacancies, in contrast to the dynamic distribution observed in the high-temperature cubic β-La2Mo2O9 phase reported previously. Additionally, the material exhibits mixed-ion-electronic conduction, which expands its potential use in applications requiring both ionic and electronic transport.

    Copyright © 2024 American Chemical Society

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    Supporting Information

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    The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acs.inorgchem.4c02151.

    • XRD patterns of La2Mo2O9−δ reduced at different temperatures and with different amounts of CaH2; representation of the cationic sublattices of α-La2Mo2O9 and β-La2Mo2O9; DSC-TG data of reduced La2Mo2O9. XPS spectra comparison of La2Mo2O9 and La2Mo2O9−δ; mass spectrometry of gas species during heating of La2Mo2O9−δ under flowing O2 gas; combined Rietveld refinement against time-of-flight neutron and X-ray synchrotron powder diffraction data collected on La2Mo2O9−δ from banks 1 to 4; comparison between the experimental PDFs of La2Mo2O9 before and after reduction; comparison between the calculated PDFs of La2Mo2O9 from the monoclinic and cubic models; Mo–O (a) and O–O (b) partial PDFs; Rw evolution of the PDF fittings as a function on the radial distances obtained for La2Mo2O9-reduced sample; equivalent circuit; binding energies and relative percentages for the different elements in La2Mo2O9 and La2Mo2O9−δ; weighted residual (Rw) of the PDF fittings; imaginary impedanceZ’’ and modulus M’’ as a function of frequency at 673 K for the La2Mo2O8.68(1) pellet; refined atomic parameters and main bond distances for β-La2Mo2O9 from room temperature neutron total scattering (PDF)

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    Inorganic Chemistry

    Cite this: Inorg. Chem. 2024, 63, 48, 22667–22676
    Click to copy citationCitation copied!
    https://doi.org/10.1021/acs.inorgchem.4c02151
    Published November 19, 2024
    Copyright © 2024 American Chemical Society
    Request reuse permissions

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