3D atomic-scale imaging of mixed Co-Fe spinel oxide nanoparticles during oxygen evolution reaction

Weikai Xiang, Nating Yang, Xiaopeng Li, Julia Linnemann, Ulrich Hagemann, Olaf Ruediger, Markus Heidelmann, Tobias Falk, Matteo Aramini, Serena DeBeer, Martin Muhler, Kristina Tschulik and Tong Li ()
Additional contact information
Weikai Xiang: Ruhr-Universität Bochum
Nating Yang: CAS Key Laboratory of Low-Carbon Conversion Science and Engineering, Shanghai Advanced Research Institute (SARI), Chinese Academy of Sciences (CAS)
Xiaopeng Li: Donghua University
Julia Linnemann: Ruhr-Universität Bochum
Ulrich Hagemann: University of Duisburg-Essen
Olaf Ruediger: Max Planck Institute for Chemical Energy Conversion
Markus Heidelmann: University of Duisburg-Essen
Tobias Falk: Ruhr-Universität Bochum
Matteo Aramini: Diamond Light Source, Harwell Science and Innovation Campus, Chilton
Serena DeBeer: Max Planck Institute for Chemical Energy Conversion
Martin Muhler: Ruhr-Universität Bochum
Kristina Tschulik: Ruhr-Universität Bochum
Tong Li: Ruhr-Universität Bochum

Nature Communications, 2022, vol. 13, issue 1, 1-14

Abstract: Abstract The three-dimensional (3D) distribution of individual atoms on the surface of catalyst nanoparticles plays a vital role in their activity and stability. Optimising the performance of electrocatalysts requires atomic-scale information, but it is difficult to obtain. Here, we use atom probe tomography to elucidate the 3D structure of 10 nm sized Co2FeO4 and CoFe2O4 nanoparticles during oxygen evolution reaction (OER). We reveal nanoscale spinodal decomposition in pristine Co2FeO4. The interfaces of Co-rich and Fe-rich nanodomains of Co2FeO4 become trapping sites for hydroxyl groups, contributing to a higher OER activity compared to that of CoFe2O4. However, the activity of Co2FeO4 drops considerably due to concurrent irreversible transformation towards CoIVO2 and pronounced Fe dissolution. In contrast, there is negligible elemental redistribution for CoFe2O4 after OER, except for surface structural transformation towards (FeIII, CoIII)2O3. Overall, our study provides a unique 3D compositional distribution of mixed Co-Fe spinel oxides, which gives atomic-scale insights into active sites and the deactivation of electrocatalysts during OER.

Date: 2022
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DOI: 10.1038/s41467-021-27788-2

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