TY - JOUR
T1 - Structural Changes of NiFe Layered Double Hydroxides During the Oxygen Evolution Reaction
T2 - A Diffraction and Total Scattering Operando Study
AU - Aalling-Frederiksen, Olivia
AU - Schlegel, Nicolas
AU - Punke, Stefanie
AU - Anker, Andy S.
AU - Wiberg, Gustav K.h.
AU - Wang, Baiyu
AU - Edelvang-Pejrup, Jens
AU - Holde, Freja B.
AU - Salinas-Quezada, María Paula
AU - Magnard, Nicolas P.L.
AU - Graversen, Laura G.
AU - Arenz, Matthias
AU - Pittkowski, Rebecca K.
AU - Jensen, Kirsten M.Ø.
N1 - Funding Information:
The authors are grateful for funding from the Carlsberg Foundation (CF21\u20100278). The authors are grateful for financial support from Villum Foundation through a Villum Young Investigator grant (VKR00015416). Funding from the Danish Ministry of Higher Education and Science through the SMART Lighthouse is acknowledged. The authors acknowledge support from the Danish National Research Foundation Center for High Entropy Alloy Catalysis (DNRF 149). The Danish Research Council is acknowledged for covering travel expenses concerning the synchrotron experiments through DanScatt. The authors acknowledge MAX IV Laboratory for time on Beamline DanMAX under Proposal 20221432. The authors would like to thank Mads Ry J\u00F8rgensen, Innokenty Kantor, and Frederik Holm Gj\u00F8rup 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\u201000009B. The authors acknowledge the European Synchrotron Radiation Facility (ESRF) for provision of synchrotron radiation facilities under proposal number CH\u20106559 and the authors would like to thank Andrea Sartori for assistance and support in using beamline ID31. The authors would like to acknowledge DESY, Hamburg, Germany, a member of the Helmholtz Association HGF for experimental facilities for the ex situ total scattering. The authors are grateful for the beamline support by scientist Henrik Jeppesen.
Publisher Copyright:
© 2025 The Author(s). Small published by Wiley-VCH GmbH.
PY - 2025
Y1 - 2025
N2 - NiFe-layered double hydroxides (LDHs) are promising electrocatalysts for the oxygen evolution reaction (OER) in alkaline media. Here, operando X-ray diffraction (XRD) and X-ray total scattering are used with Pair Distribution Function (PDF) analysis to investigate the atomic structure of the catalytically active material and follow structural changes under operating conditions. XRD shows an interlayer contraction under applied oxidative potential, which relates to a transition from the α-LDH to the γ-LDH phase. The phase transition is reversible, and the α-LDH structure is recovered at 1.3 VRHE. However, PDF analysis shows an irreversible increase in the stacking disorder under operating conditions, along with a decrease in the LDH sheet size. The analysis thus shows that the operating conditions induce a breakdown of the particles leading to a decrease in crystallite size.
AB - NiFe-layered double hydroxides (LDHs) are promising electrocatalysts for the oxygen evolution reaction (OER) in alkaline media. Here, operando X-ray diffraction (XRD) and X-ray total scattering are used with Pair Distribution Function (PDF) analysis to investigate the atomic structure of the catalytically active material and follow structural changes under operating conditions. XRD shows an interlayer contraction under applied oxidative potential, which relates to a transition from the α-LDH to the γ-LDH phase. The phase transition is reversible, and the α-LDH structure is recovered at 1.3 VRHE. However, PDF analysis shows an irreversible increase in the stacking disorder under operating conditions, along with a decrease in the LDH sheet size. The analysis thus shows that the operating conditions induce a breakdown of the particles leading to a decrease in crystallite size.
KW - layered compounds
KW - nanostructures
KW - operando experiments
KW - oxygen evolution reaction
KW - pair distribution function analysis
U2 - 10.1002/smll.202411211
DO - 10.1002/smll.202411211
M3 - Journal article
C2 - 39981961
SN - 1613-6810
VL - 21
JO - Small
JF - Small
IS - 12
M1 - 2411211
ER -