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Nanoscale Colocalization of Fluorogenic Probes Reveals the Role of Oxygen Vacancies in the Photocatalytic Activity of Tungsten Oxide Nanowires

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    Research Article

    Nanoscale Colocalization of Fluorogenic Probes Reveals the Role of Oxygen Vacancies in the Photocatalytic Activity of Tungsten Oxide Nanowires
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    • Meikun Shen
      Meikun Shen
      Department of Chemistry, Washington University, St. Louis, Missouri 63130, United States
      More by Meikun Shen
    • Tianben Ding
      Tianben Ding
      Department of Electrical and Systems Engineering, Washington University, St. Louis, Missouri 63130, United States
      More by Tianben Ding
      Orcidhttp://orcid.org/0000-0003-0710-2344
    • Steven T. Hartman
      Steven T. Hartman
      Institute of Materials Science & Engineering, Washington University, St. Louis, Missouri 63130, United States
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    • Fudong Wang
      Fudong Wang
      Department of Chemistry, Washington University, St. Louis, Missouri 63130, United States
      More by Fudong Wang
      Orcidhttp://orcid.org/0000-0003-2914-1360
    • Christina Krucylak
      Christina Krucylak
      Department of Chemistry, Washington University, St. Louis, Missouri 63130, United States
      More by Christina Krucylak
    • Zheyu Wang
      Zheyu Wang
      Institute of Materials Science & Engineering, Washington University, St. Louis, Missouri 63130, United States
      More by Zheyu Wang
    • Che Tan
      Che Tan
      Department of Energy, Environmental & Chemical Engineering, Washington University, St. Louis, Missouri 63130, United States
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    • Bo Yin
      Bo Yin
      Institute of Materials Science & Engineering, Washington University, St. Louis, Missouri 63130, United States
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    • Rohan Mishra
      Rohan Mishra
      Institute of Materials Science & Engineering, Washington University, St. Louis, Missouri 63130, United States
      Department of Mechanical Engineering and Materials Science, Washington University, St. Louis, Missouri 63130, United States
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      Orcidhttp://orcid.org/0000-0003-1261-0087
    • Matthew D. Lew*
      Matthew D. Lew
      Department of Electrical and Systems Engineering, Washington University, St. Louis, Missouri 63130, United States
      Institute of Materials Science & Engineering, Washington University, St. Louis, Missouri 63130, United States
      *E-mail: [email protected] (M.D.L.).
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      Orcidhttp://orcid.org/0000-0002-5614-3292
    • Bryce Sadtler*
      Bryce Sadtler
      Department of Chemistry, Washington University, St. Louis, Missouri 63130, United States
      Institute of Materials Science & Engineering, Washington University, St. Louis, Missouri 63130, United States
      *E-mail: [email protected] (B.S.).
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      Orcidhttp://orcid.org/0000-0003-4860-501X
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    ACS Catalysis

    Cite this: ACS Catal. 2020, 10, 3, 2088–2099
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    https://doi.org/10.1021/acscatal.9b04481
    Published January 8, 2020
    Copyright © 2020 American Chemical Society
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    Abstract

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    Defect engineering is a strategy that has been widely used to design active semiconductor photocatalysts. However, understanding the role of defects, such as oxygen vacancies, in controlling photocatalytic activity remains a challenge. Here, we report the use of chemically triggered fluorogenic probes to study the spatial distribution of active regions in individual tungsten oxide nanowires using super-resolution fluorescence microscopy. The nanowires show significant heterogeneity along their lengths for the photocatalytic generation of hydroxyl radicals. Through quantitative, coordinate-based colocalization of multiple probe molecules activated by the same nanowires, we demonstrate that the nanoscale regions most active for the photocatalytic generation of hydroxyl radicals also possess a greater concentration of oxygen vacancies. Chemical modifications to remove or block access to surface oxygen vacancies, supported by calculations of binding energies of adsorbates to different surface sites on tungsten oxide, show how these defects control catalytic activity at both the ensemble and single-particle levels. These findings reveal that clusters of oxygen vacancies activate surface-adsorbed water molecules toward photo-oxidation to produce hydroxyl radicals, a critical intermediate in several photocatalytic reactions.

    Copyright © 2020 American Chemical Society

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    • Additional experimental details on the synthesis of tungsten oxide nanowires, their oxidation, PVP functionalization, and photoirradiation; additional details on methods used to characterize the structure and morphology of the nanowires; methods used to characterize ensemble catalytic activity; preparation of samples and instrumentation for single-molecule fluorescence microscopy; analysis and processing of super-resolution images and colocalization analysis;  computational methods; supporting tables detailing the measurement conditions used for ensemble fluorescence microscopy;  binding energies and bond lengths for a PVP monomer adsorbed onto different sites of tungsten oxide; electron binding energies measured from XPS; peak positions measured from FT-IR; the burst number, photon count, and on-time measurement for different nanowires using single-molecule fluorescence microscopy; supporting figures providing characterization of different nanowire samples by XRD, XPS, TEM, absorption spectroscopy, FT-IR spectroscopy, and Raman spectroscopy; ensemble fluorescence spectra for different photocatalytic transformations; schemes for different reactions catalyzed by tungsten oxide nanowires; calculated binding configurations of a PVP monomer to tungsten oxide; statistics showing the residual background photons after temporal quantile filtering; additional super-resolution images of tungsten oxide nanowires; region-of-interest selection for extracting single-molecule bursts; quantitative characterization of APF and furfuryl alcohol blinking events; colocalization analysis of additional nanowires; and correlation between SEM and fluorescence microscopy images (PDF)

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    ACS Catalysis

    Cite this: ACS Catal. 2020, 10, 3, 2088–2099
    Click to copy citationCitation copied!
    https://doi.org/10.1021/acscatal.9b04481
    Published January 8, 2020
    Copyright © 2020 American Chemical Society
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