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Mesoporous high-entropy alloys (HEAs) represent a promising advancement in mesoporous metal, showing great potential for various applications. Their unique multimetallic uniformity, strong structural features, and high surface-active site exposure contribute to their practical catalytic ability. The catalytic efficiency of metal nanostructures depends on both their elemental compositions and crystallinity, with single-crystalline structures generally outperforming polycrystalline ones. However, synthesizing single-crystalline HEA nanostructures with defined mesoporosity remains challenging due to the complex fabrication process. This study introduces a block copolymer micelle-assisted soft-chemical strategy to create single-crystalline mesoporous HEAs (SCPHEAs). These structures feature uniformly sized mesopores that permeate throughout, maximizing the exposure of high-entropy alloy active sites, enhancing material utilization, and facilitating efficient mass and charge transport. The optimized SCPHEAs exhibit excellent electrocatalytic performance in methanol oxidation reactions, surpassing polycrystalline mesoporous HEAs, commercial Pt-C, and various recently reported precious metal-based HEAs and conventional alloy electrocatalysts. This superior performance is attributed to a synergistic effect that results from surface charge redistribution among different atomic entities, which enhances the adsorption of methanol and water molecules and mitigates intermediate CO poisoning. Our synthesis method enables the designing of a wide range of mesoporous HEAs with controllable morphology and crystallinity tailored for various catalytic applications and beyond.

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• In Copyright
  

  This document is the Accepted Manuscript version of a Published Work that appeared in final form in Journal of the American Chemical Society, copyright © 2025 American Chemical Society after peer review and technical editing by the publisher. To access the final edited and published work see https://doi.org/10.1021/jacs.5c01260.

Keyword: High Entropy Alloy, Electrocatalysis, Machine Learning, Mesoporous Metal, Nanoparticle

Date published: 2025-06-04

Publisher: American Chemical Society (ACS)

Journal:

• Journal of the American Chemical Society (ISSN: 00027863) vol. 147 issue. 22 p. 18651-18661

Funding:

• Exploratory Research for Advanced Technology JPMJER2003
• Japan Society for the Promotion of Science 20K05453
• Japan Society for the Promotion of Science 24K17694
• Japan Society for the Promotion of Science P220632

Manuscript type: Author's version (Accepted manuscript)

MDR DOI: https://doi.org/10.48505/nims.5751

First published URL: https://doi.org/10.1021/jacs.5c01260

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Updated at: 2026-02-16 18:06:09 +0900

Published on MDR: 2026-05-27 08:33:24 +0900