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Decoupling Through-Tip Illumination from Scanning in Nanoscale Photo-SECM
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    Decoupling Through-Tip Illumination from Scanning in Nanoscale Photo-SECM
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    • Gaukhar Askarova
      Gaukhar Askarova
      Department of Chemistry and Biochemistry, Queens College, Flushing, New York 11367, United States
      The Graduate Center of CUNY, New York, New York 10016, United States
    • Mahdi Hesari
      Mahdi Hesari
      Department of Chemistry and Biochemistry, Queens College, Flushing, New York 11367, United States
      More by Mahdi Hesari
    • Chen Wang
      Chen Wang
      Department of Chemistry and Biochemistry, Queens College, Flushing, New York 11367, United States
      The Graduate Center of CUNY, New York, New York 10016, United States
      More by Chen Wang
    • Michael V. Mirkin*
      Michael V. Mirkin
      Department of Chemistry and Biochemistry, Queens College, Flushing, New York 11367, United States
      Advanced Science Research Center at The Graduate Center, CUNY, New York, New York 10031, United States
      * E-mail: [email protected]. Fax: 718-997-5531.
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    Analytical Chemistry

    Cite this: Anal. Chem. 2022, 94, 20, 7169–7173
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    https://doi.org/10.1021/acs.analchem.2c00753
    Published May 9, 2022
    Copyright © 2022 American Chemical Society

    Abstract

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    The use of scanning electrochemical microscopy (SECM) for nanoscale imaging of photoelectrochemical processes at semiconductor surfaces has recently been demonstrated. To illuminate a microscopic portion of the substrate surface facing the SECM probe, a glass-sealed, polished tip simultaneously served as a nanoelectrode and a light guide. One issue affecting nanoscale photo-SECM experiments is mechanical interactions of the rigid optical fiber with the tip motion controlled by the piezo-positioner. Here we report an improved experimental setup in which the tip is mechanically decoupled from the fiber and light is delivered to the back of the tip capillary using a complex lens system. The advantages of this approach are evident from the improved quality of the approach curves and photo-SECM images. The light intensity delivered from the optical fiber to the tip is not changed significantly by their decoupling.

    Copyright © 2022 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.analchem.2c00753.

    • Additional voltammogram of oxygen reduction and photo-SECM experiments, including Figures S1 and S2 (PDF)

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    This article is cited by 8 publications.

    1. Tianyu Bo, Debjit Ghoshal, Logan M. Wilder, Elisa M. Miller, Michael V. Mirkin. High-Resolution Mapping of Photocatalytic Activity by Diffusion-Based and Tunneling Modes of Photo-Scanning Electrochemical Microscopy. ACS Nano 2025, 19 (3) , 3490-3499. https://doi.org/10.1021/acsnano.4c13276
    2. Gaukhar Askarova, Mahdi Hesari, Koushik Barman, Michael V. Mirkin. Visualizing Overall Water Splitting on Single Microcrystals of Phosphorus-Doped BiVO4 by Photo-SECM. ACS Applied Materials & Interfaces 2023, 15 (40) , 47168-47176. https://doi.org/10.1021/acsami.3c13099
    3. Partha Saha, Md. Maksudur Rahman, Caleb M. Hill. Electrocatalysis at Individual Colloidal Nanoparticles: A Quantitative Survey of Four Geometries via Electrochemical Cell Microscopy. The Journal of Physical Chemistry C 2023, 127 (19) , 9059-9066. https://doi.org/10.1021/acs.jpcc.3c01427
    4. Carla Santana Santos, Bright Nsolebna Jaato, Ignacio Sanjuán, Wolfgang Schuhmann, Corina Andronescu. Operando Scanning Electrochemical Probe Microscopy during Electrocatalysis. Chemical Reviews 2023, 123 (8) , 4972-5019. https://doi.org/10.1021/acs.chemrev.2c00766
    5. Gaukhar Askarova, Chengcan Xiao, Koushik Barman, Xiang Wang, Lihua Zhang, Frank E. Osterloh, Michael V. Mirkin. Photo-scanning Electrochemical Microscopy Observation of Overall Water Splitting at a Single Aluminum-Doped Strontium Titanium Oxide Microcrystal. Journal of the American Chemical Society 2023, 145 (11) , 6526-6534. https://doi.org/10.1021/jacs.3c00663
    6. Je Hyun Bae. A critical review: Advanced electrochemical analysis based on nanoscale scanning electrochemical microscopy. Sensors and Actuators Reports 2024, 8 , 100243. https://doi.org/10.1016/j.snr.2024.100243
    7. Hao Zhang, Hui Jiang, Xiaohui Liu, Xuemei Wang. A review of innovative electrochemical strategies for bioactive molecule detection and cell imaging: Current advances and challenges. Analytica Chimica Acta 2024, 1285 , 341920. https://doi.org/10.1016/j.aca.2023.341920
    8. Chloe L. Tolbert, Declan M. McDonald, Caleb M. Hill. Electrochemical techniques for visualizing photoelectrochemical processes at the nanoscale. Current Opinion in Electrochemistry 2023, 37 , 101164. https://doi.org/10.1016/j.coelec.2022.101164

    Analytical Chemistry

    Cite this: Anal. Chem. 2022, 94, 20, 7169–7173
    Click to copy citationCitation copied!
    https://doi.org/10.1021/acs.analchem.2c00753
    Published May 9, 2022
    Copyright © 2022 American Chemical Society

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