Publication date: 15th December 2025
NiFe-layered double hydroxides (LDH) are state-of-the-art electrocatalysts for the oxygen evolution reaction (OER) under alkaline conditions. While intrinsic catalyst properties are crucial for their activity, the interaction between the LDH catalyst and the electrolyte can significantly influence the electrocatalytic performance. It has been shown that increasing electrolyte cation size (CsOH > KOH > NaOH > LiOH) enhances the NiFe-LDH OER performance. This is hypothesized to be related to the intercalation of the cation and the following changes in LDH layer spacing.[1] Operando X-ray diffraction (XRD) and X-ray total scattering with Pair Distribution Function (PDF) analysis are powerful structural characterization techniques, which allow us to follow changes in catalyst structure during operation.[2] By measuring operando XRD and PDF quasi-simultaneously, we directly probe how electrolyte-mediated structural dynamics are coupled to the electrochemical behavior. This dual approach captures both long-range and local changes during cycling, revealing links between structure and electrocatalytic performance. Leveraging the high brilliance and time resolution of synchrotron radiation enables us to track these transformations in real time, providing unique insight into the dynamic nature of active catalyst phases. Such operando measurements are essential for disentangling the interplay between structure, electrolyte environment, and catalytic function under realistic working conditions. We demonstrate that the interlayer distance of NiFe-LDHs changes reversibly with applied potential, contracting during Ni oxidation and expanding back to larger d-spacings upon reduction. This reversible behavior is further influenced by the identity of the electrolyte cation, with variations observed across different alkaline environments. At the local structural level, both metal–metal and metal–oxygen bond distances in the NiFe layers shorten as Ni is oxidized and relax back when Ni is reduced. In the OER region, these effects become particularly important and evident, as different alkali cations exert distinct influences on the catalyst’s structural dynamics and the catalytic activity, emphasizing the critical importance of studying the electrode–electrolyte interactions under operando conditions.
We are grateful for support from the Danish National Research Foundation Center for High Entropy Alloy Catalysis (DNRF 149), the Novo Nordisk Foundation (NNF23OC0085722), and the Danish Agency for Science, Technology, and Innovation for covering travel expenses concerning the synchrotron experiments (DanScatt). We acknowledge MAX IV Laboratory for time on Beamline DanMAX under Proposal 20240494. The authors would like to thank Mads Ry Jørgensen, Innokenty Kantor, and Frederik Holm Gjørup for the support during the experiments. Research conducted at MAX IV is supported by the Swedish Research council under contract 2018, the Swedish Governmental Agency for Innovation Systems under contract 2018, and Formas under contract 2019. DanMAX is funded by the NUFI grant no. 4059-00009B. We acknowledge the European Synchrotron Radiation Facility (ESRF) for provision of synchrotron radiation facilities under proposal number CH7147 and the authors would like to thank Dr. Jakub Drnec for assistance and support in using beamline ID31. The raw data associated with this work are available through the ESRF data repository at https://doi.esrf.fr/10.15151/ESRF-ES-1941858325
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