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Operando Methods for the Mechanistic Elucidation of an Electrochemically Driven Structural Transformation

  • E. Martínez-Periñán
    E. Martínez-Periñán
    Departamento de Química Analítica, Universidad Autónoma de Madrid, 28049 Madrid, Spain
    More by E. Martínez-Periñán
    Orcidhttp://orcid.org/0000-0003-3122-3381
  • , 
  • M. Revenga-Parra
    M. Revenga-Parra
    Departamento de Química Analítica  and  Institute for Advanced Research in Chemical Sciences (IAdChem), Universidad Autónoma de Madrid, 28049 Madrid, Spain
    Instituto Madrileño de Estudios Avanzados en Nanociencia (IMDEA Nanociencia), Cantoblanco, 28049 Madrid, Spain
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  • , 
  • J. Pastore
    J. Pastore
    Department of Chemistry and Chemical Biology, Cornell University, Ithaca, New York 14853, United States
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  • , 
  • F. Pariente
    F. Pariente
    Departamento de Química Analítica  and  Institute for Advanced Research in Chemical Sciences (IAdChem), Universidad Autónoma de Madrid, 28049 Madrid, Spain
    More by F. Pariente
  • , 
  • F. Zamora
    F. Zamora
    Departamento de Química Inorgánica  and  Institute for Advanced Research in Chemical Sciences (IAdChem), Universidad Autónoma de Madrid, 28049 Madrid, Spain
    Instituto Madrileño de Estudios Avanzados en Nanociencia (IMDEA Nanociencia), Cantoblanco, 28049 Madrid, Spain
    More by F. Zamora
    Orcidhttp://orcid.org/0000-0001-7529-5120
  • , 
  • O. Castillo
    O. Castillo
    Departamento de Química Inorgánica, Universidad del País Vasco, Apartado 644, E-48080 Bilbao, Spain
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  • , 
  • E. Lorenzo
    E. Lorenzo
    Departamento de Química Analítica  and  Institute for Advanced Research in Chemical Sciences (IAdChem), Universidad Autónoma de Madrid, 28049 Madrid, Spain
    Instituto Madrileño de Estudios Avanzados en Nanociencia (IMDEA Nanociencia), Cantoblanco, 28049 Madrid, Spain
    More by E. Lorenzo
    Orcidhttp://orcid.org/0000-0001-8432-9652
  • , and 
  • H. D. Abruña*
    H. D. Abruña
    Department of Chemistry and Chemical Biology, Cornell University, Ithaca, New York 14853, United States
    *E-mail: [email protected]. Tel: +1 (607) 255-4720. Fax: +1 (607) 255-9864.
    More by H. D. Abruña
Cite this: J. Phys. Chem. C 2018, 122, 23, 12377–12383
Publication Date (Web):May 21, 2018
https://doi.org/10.1021/acs.jpcc.8b03851
Copyright © 2018 American Chemical Society
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    Abstract

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    We present the use of operando methods for the mechanistic dilucidation of an electrochemically driven structural transformation of a Ni(II) thioacetate complex. Specifically, we employed operando Raman spectroscopy and electrochemistry, along with X-ray diffraction to characterize the electrochemically induced conversion of a paddle-wheel tetrakis–acetate dinickel(II) complex into the related dinickel acetate. Successive Raman spectra were obtained from the surface of a gold electrode immersed in an electrochemical cell containing the dinuclear complex [Ni2(CH3COS)4·EtOH] under a constant applied potential, to oxidize the complex, and effects its conversion/transformation into the unprecedented [Ni(CH3COO)2]n electrodeposited onto the electrode surface as microstructures. The crystal structure of the new electrogenerated compound [Ni(CH3COO)2]n was also examined by synchrotron X-ray diffraction. The observation of a disulfide species, generated during the electrochemical process via Raman spectroscopy was consistent with and served to confirm the proposed mechanism. These approaches can be readily applied to numerous electrode potential-induced transformations.

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    The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.jpcc.8b03851.

    • Table containing unit cell parameters of some anhydrous divalent transition metal acetates (PDF)

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    Cited By

    This article is cited by 5 publications.

    1. Sujoy Sarkar, Xiang Wang, Mahdi Hesari, Peng Chen, Michael V. Mirkin. Scanning Electrochemical and Photoelectrochemical Microscopy on Finder Grids: Toward Correlative Multitechnique Imaging of Surfaces. Analytical Chemistry 2021, 93 (13) , 5377-5382. https://doi.org/10.1021/acs.analchem.1c00358
    2. Xiaoju Yang, Bingjun Xu, Jingguang G. Chen, Xuan Yang. Recent Progress in Electrochemical Nitrogen Reduction on Transition Metal Nitrides. ChemSusChem 2023, 16 (5) https://doi.org/10.1002/cssc.202201715
    3. Libo Sun, Vikas Reddu, Xin Wang. Multi-atom cluster catalysts for efficient electrocatalysis. Chemical Society Reviews 2022, 51 (21) , 8923-8956. https://doi.org/10.1039/D2CS00233G
    4. Jingkun Li, Jinlong Gong. Operando characterization techniques for electrocatalysis. Energy & Environmental Science 2020, 13 (11) , 3748-3779. https://doi.org/10.1039/D0EE01706J
    5. Emiliano Martínez-Periñán, Iria Bravo, Mónica Mediavilla, Mónica Revenga-Parra, Eva Mateo-Martí, Félix Pariente, Encarnación Lorenzo. Spectroelectrochemical operando method for monitoring a phenothiazine electrografting process on amide functionalized C-nanodots/Au hybrid electrodes. Electrochimica Acta 2019, 298 , 950-959. https://doi.org/10.1016/j.electacta.2018.12.106
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