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However, the range of available precursors and materials is relatively limited, and the correlation between precursor structure and the resulting morphology remains largely unexplored. Herein, we design a water\u2010soluble, ammonium\u2010functionalized aggregation\u2011induced emission luminogen (AIEgen) that serves dual roles as a crosslinkable building block and an auxiliary fluorescence probe. Co\u2011assembled with Pluronic F127 in an emulsion, this system yields an asymmetric\u2011wall nanoporous polymer capsule (ANPC) with a mesoporous outer shell and a dense inner layer, a morphology rarely achieved in polymer\u2011based systems. Multi\u2010scale characterizations, spanning fluorescence monitoring, precursor structure variation, electron microscopy, crystallographic and computational analyses, collectively reveal that AIEgen\u2011solvent and AIEgen\u2011F127 interactions cooperatively govern this architecture evolution. Benefiting from its hollow cavity and nanoporous shell that promote mass transport and site accessibility, the cobalt phthalocyanine\u2010loaded ANPC catalyst achieves an impressive methanol Faradaic efficiency of 44.2% in acidic CO\n                    <jats:sub>2<\/jats:sub>\n                    electroreduction, markedly outperforming nonporous bulk (6.8%), nonporous capsules (14.8%), mesoporous nanospheres (17.5%), and sparse\u2010porous capsules (28.5%). Ultimately, this work establishes a rational co\u2010assembly strategy for engineering porous architectures, highlighting how precursor design dictates morphology and how such structural uniqueness directly boosts electrocatalytic performance.\n                  <\/jats:p>","DOI":"10.1002\/adma.75033","type":"journal-article","created":{"date-parts":[[2026,9,16]],"date-time":"2026-09-16T06:48:30Z","timestamp":1789541310000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Asymmetric\u2010Wall Nanoporous Polymer Capsules via AIEgen\u2011Assisted Assembly as High\u2011Performance Electrocatalytic Carriers"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0009-0009-8129-3549","authenticated-orcid":false,"given":"Guokang","family":"He","sequence":"first","affiliation":[{"name":"Department of Chemistry and the Hong Kong Branch of Chinese National Engineering Research Center for Tissue Restoration and 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