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Post-Synthesis Heat Treatment of Doped PtNi-Alloy Fuel-Cell Catalyst Nanoparticles Studied by In-Situ Electron Microscopy

  • Katherine E. MacArthur*
    Katherine E. MacArthur
    Ernst Ruska-Centre for Microscopy and Spectroscopy with Electrons, Peter Grünberg Institute, Forschungszentrum Jülich, 52425 Jülich, Germany
    *Email: [email protected]
  • Shlomi Polani
    Shlomi Polani
    Electrochemical Energy, Catalysis, and Material Science Laboratory, Department of Chemistry, Technical University Berlin, 10623 Berlin, Germany
  • Malte Klingenhof
    Malte Klingenhof
    Electrochemical Energy, Catalysis, and Material Science Laboratory, Department of Chemistry, Technical University Berlin, 10623 Berlin, Germany
  • Nina Gumbiowski
    Nina Gumbiowski
    Inorganic Chemistry and Center for Nanointegration Duisburg-Essen (CENIDE), University of Duisburg-Essen, Universitaetsstr. 5-7, 45117 Essen, Germany
  • Tim Möller
    Tim Möller
    Electrochemical Energy, Catalysis, and Material Science Laboratory, Department of Chemistry, Technical University Berlin, 10623 Berlin, Germany
    More by Tim Möller
  • Paul Paciok
    Paul Paciok
    Ernst Ruska-Centre for Microscopy and Spectroscopy with Electrons, Peter Grünberg Institute, Forschungszentrum Jülich, 52425 Jülich, Germany
    More by Paul Paciok
  • Jiaqi Kang
    Jiaqi Kang
    Electrochemical Energy, Catalysis, and Material Science Laboratory, Department of Chemistry, Technical University Berlin, 10623 Berlin, Germany
    More by Jiaqi Kang
  • Matthias Epple
    Matthias Epple
    Inorganic Chemistry and Center for Nanointegration Duisburg-Essen (CENIDE), University of Duisburg-Essen, Universitaetsstr. 5-7, 45117 Essen, Germany
  • Shibabrata Basak
    Shibabrata Basak
    Institute of Energy and Climate Research (IEK9), Forschungszentrum Jülich, 52425 Jülich, Germany
  • Rüdiger-A. Eichel
    Rüdiger-A. Eichel
    Institute of Energy and Climate Research (IEK9), Forschungszentrum Jülich, 52425 Jülich, Germany
  • Peter Strasser
    Peter Strasser
    Electrochemical Energy, Catalysis, and Material Science Laboratory, Department of Chemistry, Technical University Berlin, 10623 Berlin, Germany
  • Rafal E. Dunin-Borkowski
    Rafal E. Dunin-Borkowski
    Ernst Ruska-Centre for Microscopy and Spectroscopy with Electrons, Peter Grünberg Institute, Forschungszentrum Jülich, 52425 Jülich, Germany
  • , and 
  • Marc Heggen
    Marc Heggen
    Ernst Ruska-Centre for Microscopy and Spectroscopy with Electrons, Peter Grünberg Institute, Forschungszentrum Jülich, 52425 Jülich, Germany
    More by Marc Heggen
Cite this: ACS Appl. Energy Mater. 2023, 6, 11, 5959–5967
Publication Date (Web):May 16, 2023
https://doi.org/10.1021/acsaem.3c00405
Copyright © 2023 American Chemical Society

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    Abstract

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    Octahedral-shaped PtNi-alloy nanoparticles are highly active oxygen reduction reaction catalysts for the cathode in proton exchange membrane fuel cells. However, one major drawback in their application is their limited long-term morphological and compositional stability. Here, we present a detailed in situ electron microscopy characterization of thermal annealing on octahedral-shaped PtNi catalysts as well as on doped octahedral PtNi(Mo) and PtNi(MoRh) catalysts. The evolution of their morphology and composition was quantified during both ex situ and in situ experiments using energy dispersive X-ray spectroscopy in a scanning transmission electron microscope under a hydrogen atmosphere and in vacuum. Morphological changes upon heating, i.e., a gradual loss of the octahedral shape and a continuous rounding of the particles, were observed, as well as evidence for increased alloying. Furthermore, the evolution of the shape of the PtNi(Mo) nanoparticles was quantified using in situ experiments under hydrogen atmosphere in a transmission electron microscope. The shape change of the particles was quantified using segmentation maps created by a neural network. It has been demonstrated that morphological changes crucially depend on the composition and surface doping: doping with Mo or Mo/Rh significantly stabilizes the structure, allowing for persistence of a truncated octahedral shape during heat treatments.

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    The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acsaem.3c00405.

    • Exact details of the heating profiles used, tracking of the atoms in the in situ EDX heating experiments and additional images and EDX maps, and in situ videos can also be provided upon request (PDF)

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    Cited By

    This article is cited by 1 publications.

    1. Natalie Wolff, Kateryna Loza, Marc Heggen, Torsten Schaller, Felix Niemeyer, Peter Bayer, Christine Beuck, Cristiano L. P. Oliveira, Oleg Prymak, Claudia Weidenthaler, Matthias Epple. Ultrastructure and Surface Composition of Glutathione-Terminated Ultrasmall Silver, Gold, Platinum, and Alloyed Silver–Platinum Nanoparticles (2 nm). Inorganic Chemistry 2023, 62 (42) , 17470-17485. https://doi.org/10.1021/acs.inorgchem.3c02879