Proceedings of MATSUS Spring 2024 Conference (MATSUS24)
DOI: https://doi.org/10.29363/nanoge.matsus.2024.240
Publication date: 18th December 2023
Water splitting is emerging as a promising route for generating hydrogen in a more sustainable way compared to conventional production methods. Finding affordable and scalable catalysts for the anodic half-reaction, the oxygen evolution reaction (OER), could help with its industrial widespread implementation. Nonetheless, the electrocatalysts’ near-surface structure during OER is still largely unknown, which hampers knowledge-driven optimization. Here, we provide quantitative near-surface structural insights into oxygen-evolving CoOX(OH)Y clusters and nanoparticles by tracking their size-dependent catalytic activity from 4 atom clusters to 50 nm particles and their structural adaptation to OER conditions combining operando X-ray absorption spectroscopy (XAS) and density functional theory calculations. We uncover a superior intrinsic OER activity of 1-5 nm nanoparticles and a size-dependent oxidation leading to a near-surface Co-O bond contraction and charge redistribution during OER.
Moreover, I will also report on the role of Fe in the performance of Co- and Ni-oxide-based electrocatalysts. I will discuss the catalytic performance of epitaxial Co3O4, Co1+δFe2-δO4 (|δ|<=0.2), and Fe3O4 thin film electrocatalysts with (111) and (100) surface orientations. Under OER conditions, all three oxides are covered by oxyhydroxide, but the characteristics of this overlayer, including its thickness, stability, structural and chemical evolution were found to strongly depend on the Fe content and the initial surface structure of the pre-catalyst. Similar investigations carried out for epitaxial NiO(001) and Ni0.75Fe0.25Ox(001) thin films with operando Raman and grazing Incidence XAS will also be presented to demonstrate the generality of the findings obtained for the CoOx thin films. Finally, the observed compositional, structural, and electronic properties of each system will be correlated with their electrochemical performance.
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