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Herein, we propose a facile immiscible\u2010metal\u2010induced surface\u2010segregation strategy to construct a core\u2013shell Bi\u2013PtMn catalyst that simultaneously achieves outstanding MOR performance and high selectivity toward the CO\u2010free pathway. Exploiting the immiscibility between Mn and Bi enables precise regulation of surface\u2010segregated Bi, leading to a well\u2010defined core\u2013shell structure with an ordered L1\n                    <jats:sub>0<\/jats:sub>\n                    \u2010PtMn core and a PtBi shell. The catalyst delivers benchmark mass activity of 61.81 A mg\n                    <jats:sub>Pt<\/jats:sub>\n                    <jats:sup>\u22121<\/jats:sup>\n                    , 4.0 and 16.2 times that of Bi\u2010Pt and Pt\/C, respectively. Furthermore, as a practical anodic electrocatalyst for direct methanol fuel cells, the catalyst achieves a peak power density of 294.21\u00a0mW cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    at an ultralow Pt loading of 0.5 mg\n                    <jats:sub>Pt<\/jats:sub>\n                    cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    . Mn lowers the barrier of the rate\u2010determining step by facilitating C\u2500H bond cleavage, as corroborated by theoretical calculations and kinetic isotope effect (KIE) measurements. This work provides a design principle based on immiscible metal thermodynamics for atomic\u2010level surface engineering of electrocatalysts.\n                  <\/jats:p>","DOI":"10.1002\/adma.74062","type":"journal-article","created":{"date-parts":[[2026,7,15]],"date-time":"2026-07-15T11:02:01Z","timestamp":1784113321000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Immiscible Metal\u2010Regulated Surface Segregation Enables Core\u2013Shell Bi\u2013PtMn Catalysts With Benchmark Performance in Direct Methanol Fuel Cells"],"prefix":"10.1002","volume":"38","author":[{"ORCID":"https:\/\/orcid.org\/0009-0008-1514-5524","authenticated-orcid":false,"given":"Shao","family":"Ye","sequence":"first","affiliation":[{"name":"The Key Laboratory of Fuel Cell Technology of Guangdong Province School of Chemistry and Chemical Engineering South China University of Technology  Guangzhou China"},{"name":"Department of Materials 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