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Elucidation of Structure-Activity Correlations in a Nickel Manganese Oxide Oxygen Evolution Reaction Catalyst by Operando Ni L-Edge X-ray Absorption Spectroscopy and 2p3d Resonant Inelastic X-ray Scattering

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Al Samarai,  Mustafa
Research Department DeBeer, Max Planck Institute for Chemical Energy Conversion, Max Planck Society;

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Hahn,  Anselm W.
Research Department DeBeer, Max Planck Institute for Chemical Energy Conversion, Max Planck Society;

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Beheshti Askari,  Abbas
Research Department DeBeer, Max Planck Institute for Chemical Energy Conversion, Max Planck Society;

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Rüdiger,  Olaf
Research Department DeBeer, Max Planck Institute for Chemical Energy Conversion, Max Planck Society;

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DeBeer,  Serena
Research Department DeBeer, Max Planck Institute for Chemical Energy Conversion, Max Planck Society;

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Citation

Al Samarai, M., Hahn, A. W., Beheshti Askari, A., Cui, Y.-T., Yamazoe, K., Miyawaki, J., et al. (2019). Elucidation of Structure-Activity Correlations in a Nickel Manganese Oxide Oxygen Evolution Reaction Catalyst by Operando Ni L-Edge X-ray Absorption Spectroscopy and 2p3d Resonant Inelastic X-ray Scattering. ACS Applied Materials and Interfaces, 11(42), 38595-38605. doi:10.1021/acsami.9b06752.


Cite as: https://hdl.handle.net/21.11116/0000-0005-A91B-F
Abstract
Herein, we report the synthesis and electro-chemical oxygen evolution experiments for a graphene-supported Ni3MnO4 catalyst. The changes that occur at the Ni active sites during the electrocatalyic oxygen evolution reaction (OER) were elucidated by a combination of operando Ni L-edge X-ray absorption spectroscopy (XAS) and Ni 2p3d resonant inelastic X-ray scattering (RIXS). These data are compared to reference measurements on NiO, beta-Ni(OH)(2), beta-NiOOH, and gamma-NiOOH. Through this comparative analysis, we are able to show that under alkaline conditions (0.1 M KOH), the oxides of the Ni3MnO4 catalyst are converted to hydroxides. At the onset of catalysis (1.47 V), the beta-Ni(OH)(2)-like phase is oxidized and converted to a dominantly gamma-NiOOH phase. The present study thus challenges the notion that the beta-NiOOH phase is the active phase in OER and provides further evidence that the gamma-NiOOH phase is catalytically active. The ability to use Ni L-edge XAS and 2p3d RIXS to provide a rational basis for structure-activity correlations is highlighted.