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Topochemical exfoliation of metal oxyhydroxides for the electrolytic oxygen evolution reaction

Nature Synthesis volume 4, pages 1308–1318 (2025)Cite this article

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Abstract

Thin nanosheets of metal oxyhydroxides (MOOHs) are promising for a range of applications, including electronics, optics, electrochemistry and catalysis. However, their synthesis remains challenging. Here we address this by introducing a topochemical oxidizing approach that enables the production of stable aqueous colloids of four different MOOH nanosheets. Chemically implanted active oxygen species are shown to facilitate the exfoliation of bulk MOOHs with an efficiency strongly dependent on their abundance. Spectroscopic analysis combined with theoretical calculations reveals that alkali cations stabilize negatively charged active oxygen species through electrostatic interactions, regulating the repulsive forces between the layers, and thereby facilitating effective exfoliation. As-produced Cs+-CoFeOOH nanosheets have high electrocatalytic performances for the oxygen evolution reaction, achieving 1 A cm−2 at a cell voltage of 1.62 V in an anion-exchange membrane water electrolyser. This work presents an alternative strategy for exfoliating MOOHs and may open new avenues for fabricating two-dimensional materials from delamination-resistant layered compounds.

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Fig. 1: Schematic of the topochemical exfoliation process.
Fig. 2: Characterizations of CoOOH nanosheets.
Fig. 3: Characterization of binary metal oxyhydroxide nanosheets.
Fig. 4: Atomic and electronic structures of A+-CoOOH nanosheets.
Fig. 5: Electrochemical and AEMWE performance of MOOH nanosheets.

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All data are available in the main text or the Supplementary Information, and are also available from the corresponding authors upon request. Source data are provided with this paper.

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Acknowledgements

This work was supported by the National Natural Science Foundation of China (grant number 22479097, F.S.), the Shanghai Science and Technology Committee (Grant numbers 23ZR1433000 and 22511100400, F.S.), the National High-Level Talent Program for Young Scholars (F.S.), the Start-up Fund (F.S.) from Shanghai Jiao Tong University, the Shanghai Jiao Tong University 2030 Initiative (D.Z.), and the Nano·Materials Technology Development program (RS-2023-00235295, Y.M.L.) through the NRF funded by the Ministry of Science and ICT of South Korea. H.M.C. acknowledges support from the National Science and Technology Council, Taiwan (contract numbers NSTC 113-2123-M-002-005 and 113-2639-M-002-009-ASP). We also acknowledge the Shanghai Jiao Tong University Instrument Analysis Centre and the SJTU-HPC computing facility for the measurements and computational hours.

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Authors and Affiliations

  1. State Key Laboratory of Metal Matrix Composites, School of Materials Science and Engineering, Shanghai Jiao Tong University, Shanghai, China

    Sihong Wang, Qu Jiang, Haoyue Zhang, Ruohan Feng, Chaoran Zhang, Cuiping Guo, Di Zhang & Fang Song

  2. Department of Energy Engineering, College of Engineering, Hanyang University, Seoul, Republic of Korea

    Chuan Hu & Young Moo Lee

  3. Department of Chemistry and Center for Emerging Materials and Advanced Devices, National Taiwan University, Taipei, Taiwan

    Chia-Shuo Hsu & Hao Ming Chen

  4. National Synchrotron Radiation Research Center, Hsinchu, Taiwan

    Hao Ming Chen

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Contributions

F.S. conceived the idea and led the project. S.W. synthesized the catalysts, did the structural characterizations and tested the electrochemical performances, with the assistance of Q.J. H.Z., R.F. and C.Z. assisted with Raman and AFM measurements and contributed to data interpretation. C.H. synthesized the polymers, and fabricated the membranes and AEMWEs under the supervision of Y.M.L. S.W. conducted the DFT calculations. C.-S.H. and H.M.C. did the XAS measurements. D.Z. provided resources for material characterizations and theoretical calculations. C.G. discussed the possible exfoliation mechanism. All authors analysed the data. F.S. and S.W. wrote the paper, with input from all the other authors.

Corresponding authors

Correspondence to Hao Ming Chen or Fang Song.

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Competing interests

F.S., S.W. and C.G. are named as inventors on a patent (ZL 2021 1 0728470.X) filed by Shanghai Jiao Tong University related to the exfoliation technology described in this paper. The other authors declare no competing interests.

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Nature Synthesis thanks Pawin Iamprasertkun, Chuan Zhao and the other, anonymous, reviewer(s) for their contribution to the peer review of this work. Primary Handling Editor: Alexandra Groves, in collaboration with the Nature Synthesis team.

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Wang, S., Jiang, Q., Hu, C. et al. Topochemical exfoliation of metal oxyhydroxides for the electrolytic oxygen evolution reaction. Nat. Synth 4, 1308–1318 (2025). https://doi.org/10.1038/s44160-025-00837-0

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