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In this study, we propose a microemulsion\u2010mediated semi\u2010confined method for synthesis of covalent organic framework (COF) nanosheets featured by the concurrent implementation of uniform size, high crystallinity and yield, and excellent scalability, which is virtually impossible for the dominant interfacial polymerization and phase\u2010transfer polymerization methods. The versatility of this method is demonstrated by synthesizing a range of COF nanosheets, including TpPa\u2010SO\n                    <jats:sub>3<\/jats:sub>\n                    H, TpBd\u2010(SO\n                    <jats:sub>3<\/jats:sub>\n                    H)\n                    <jats:sub>2<\/jats:sub>\n                    , and TpTG. The resulting TpBd\u2010(SO\n                    <jats:sub>3<\/jats:sub>\n                    H)\n                    <jats:sub>2<\/jats:sub>\n                    COF nanosheets are assembled into self\u2010standing COF membranes, achieving the highest proton conductivity (1.76 S cm\n                    <jats:sup>\u22121<\/jats:sup>\n                    ), high mechanical strength (92.1\u00a0MPa), and negligible swelling ratio (&lt;5%). In practical PEM water electrolysis, the TpBd\u2010(SO\n                    <jats:sub>3<\/jats:sub>\n                    H)\n                    <jats:sub>2<\/jats:sub>\n                    COF membrane yields a current density of 3.0 A\u00a0cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    at 2.3\u00a0V and 60\u00a0\u00b0C, outperforming the commercial Nafion membrane (3.0 A\u00a0cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    at 2.7\u00a0V) under identical conditions. Our work develops an alternative platform method for COF nanosheet synthesis and marks the first application of self\u2010standing COF membranes in PEM water electrolysis, unlocking their great potential for high\u2010efficiency energy conversion.\n                  <\/jats:p>","DOI":"10.1002\/anie.3468299","type":"journal-article","created":{"date-parts":[[2026,2,4]],"date-time":"2026-02-04T06:23:05Z","timestamp":1770186185000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":7,"title":["Proton Exchange Membranes from Microemulsion\u2010Synthesized COF Nanosheets for Water Electrolysis"],"prefix":"10.1002","volume":"65","author":[{"given":"Xu","family":"Dong","sequence":"first","affiliation":[{"name":"School of Chemical Engineering and Technology Tianjin University  Tianjin 300072 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Shiyi","family":"Zhu","sequence":"additional","affiliation":[{"name":"School 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