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However, bottom\u2010up construction of reactive interfaces for controlled synthesis of crystalline porous materials still remains a substantial challenge. Here, we constructed a stable, morphology\u2010tunable reactive interface by spontaneous self\u2010assembly of amphiphilic moiety derived from Schiff base reactions, featuring the surfactant\u2010free stabilization and versatile interface morphology readily adjusted by hydrophobic chain length (C4\u2013C12) of aliphatic amines. Such interface confinement lowers nucleation barriers while the localized monomer enrichment speeds reactions, thus enabling a mild, facile, and controlled synthesis of covalent organic frameworks (COFs) with diverse mesoscopic architectures (spherical\/ribbon\/sheet). Further introducing colloidal SiO\n                    <jats:sub>2<\/jats:sub>\n                    nanospheres on the interfaces can co\u2010assemble and form stable nanoscale Pickering emulsions, yielding hierarchical porous COFs with tunable, large mesopores (17\u201040\u00a0nm) beyond the intrinsic pore size limitation. The resulting asymmetric hemispherical hollow mCOF\n                    <jats:sub>PEA<\/jats:sub>\n                    (BET surface area of 561.9 m\n                    <jats:sup>2<\/jats:sup>\n                    g\n                    <jats:sup>\u22121<\/jats:sup>\n                    ) as a potential iodine host (30.18\u00a0wt.% loading) delivered remarkable electrochemical performance with an initial capacity of 202.9 mAh g\n                    <jats:sup>\u22121<\/jats:sup>\n                    (96.16% of theoretical value) and retained 132.8 mAh g\n                    <jats:sup>\u22121<\/jats:sup>\n                    after 2500 cycles, profited from their mesoporosity and asymmetric morphology with an increased surface area, exposed more active sites and enhanced ion transport ability.\n                  <\/jats:p>","DOI":"10.1002\/anie.202517356","type":"journal-article","created":{"date-parts":[[2026,1,12]],"date-time":"2026-01-12T14:26:57Z","timestamp":1768228017000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":4,"title":["Amphiphilic Reactive Interfaces Enable Controlled Synthesis of Mesoscopic Covalent Organic Frameworks"],"prefix":"10.1002","volume":"65","author":[{"given":"Hao","family":"Chen","sequence":"first","affiliation":[{"name":"Engineering Research Center of Nanophotonics &amp; Advanced Instrument (Ministry of Education) School of Physics East China Normal University  Shanghai 200241 P.R. 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