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A series of composition\u2010controlled PtCo\/C alloy catalysts is synthesized. In situ XRD analysis provided clear evidence of the structural transformation from the Pt\u2010Co\u2010PVP composite to the PtCo alloy during calcination under a H\n                    <jats:sub>2<\/jats:sub>\n                    \/Ar atmosphere. The process began at 300\u00a0\u00b0C with the concurrent formation of two distinct populations of alloy nanoparticles with high and low Pt\/Co ratios. With increasing temperature, the high\u2010ratio nanoparticles are gradually converted into those with a lower ratio. The Pt\/Co ratios in these catalysts demonstrated a remarkable consistency with the predetermined ratios in the mother solution. The Co\/Pt mass ratio can span a wide range from 0 to 150%. As for a case application for electrocatalytic methanol oxidation reaction, the optimized Pt\n                    <jats:sub>1<\/jats:sub>\n                    Co\n                    <jats:sub>0.8<\/jats:sub>\n                    \/C alloy catalyst achieved a mass activity of 1.8 A\/mg(Pt), which is 2.4 times that of a commercial PtCo\/C\u2010TKK catalyst, 2.2 and 4.4 times that of Pt\n                    <jats:sub>1<\/jats:sub>\n                    Co\n                    <jats:sub>0.8<\/jats:sub>\n                    \/C\u2010Im and Pt\/C\u2010Im catalysts prepared via impregnation. The aerosol\u2010microdroplet confinement strategy also enables the composition\u2010precise synthesis of other alloy catalysts.\n                  <\/jats:p>","DOI":"10.1002\/smll.202511541","type":"journal-article","created":{"date-parts":[[2025,11,25]],"date-time":"2025-11-25T11:22:25Z","timestamp":1764069745000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["A Composition\u2010Precise Synthesis of Porous PtCo Alloy Catalysts Mediated by Aerosol\u2010Microdroplet Confinement"],"prefix":"10.1002","volume":"22","author":[{"given":"Qiao","family":"Qiao","sequence":"first","affiliation":[{"name":"School of Chemical and Environmental Engineering Anhui Laboratory of Clean Catalytic Engineering Anhui Laboratory of Functional Coordinated Complexes for Materials Chemistry and Application, Hydrogen Energy Technology Research Center of Wuhu Anhui Polytechnic University  Beijng Middle Road Wuhu 241000 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