Time-resolved spectroscopy uncovers deprotonation-induced reconstruction in oxygen-evolution NiFe-based (oxy)hydroxides

Dan Wu, Longfei Hu, Xiaokang Liu, Tong Liu, Xiangyu Zhu, Qiquan Luo, Huijuan Zhang, Linlin Cao (), Jinlong Yang, Zheng Jiang () and Tao Yao ()
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Dan Wu: University of Science and Technology of China
Longfei Hu: University of Science and Technology of China
Xiaokang Liu: University of Science and Technology of China
Tong Liu: University of Science and Technology of China
Xiangyu Zhu: University of Science and Technology of China
Qiquan Luo: Anhui University
Huijuan Zhang: University of Science and Technology of China
Linlin Cao: University of Science and Technology of China
Jinlong Yang: University of Science and Technology of China
Zheng Jiang: University of Science and Technology of China
Tao Yao: University of Science and Technology of China

Nature Communications, 2025, vol. 16, issue 1, 1-8

Abstract: Abstract Transition-metal layered double hydroxides are widely utilized as electrocatalysts for the oxygen evolution reaction (OER), undergoing dynamic transformation into active oxyhydroxides during electrochemical operation. Nonetheless, our understanding of the non-equilibrium structural changes that occur during this process remains limited. In this study, utilizing in situ energy-dispersive X-ray absorption spectroscopy and machine learning analysis, we reveal the occurrence of deprotonation and elucidate the role of incorporated iron in facilitating the transition from nickel-iron layered double hydroxide (NiFe LDH) into its active oxyhydroxide. Our findings demonstrate that iron substitution promotes deprotonation process within NiFe LDH, resulting in the preferential removal of protons from the specific bridged hydroxyl group (Ni2+-OH-Fe3+) linked to edge-sharing [NiO6] and [FeO6] octahedron. This deprotonation behavior drives the formation of high-valence Ni3+δ species (0

Date: 2025
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DOI: 10.1038/s41467-025-56070-y

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