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However, it is challenging to prepare COF membranes with a molecular sieving property for gas separation due to their relatively large pore size. In this work, we develop the MOF\u2010in\u2010COF concept for vacuum\u2010assisted synthesis of metal\u2013organic framework (MOF) ZIF\u20108 inside the pores of TB\u2010COF formed from trihydroxy\u2010benzene\u2010tricarbaldehyde (T) and diamino\u2010biphenyl\u2010disulfonic acid (B), thus constructing a novel ZIF\u20108@TB\u2010COF membrane. Attributing to the formation of a well\u2010defined one\u2010dimensional (1D) nanoscale transport channel, the ZIF\u20108@TB\u2010COF membrane displays a high hydrogen permselectivity. At 100\u2009\u00b0C and 200\u2005kPa, the mixture separation factors of H\n                    <jats:sub>2<\/jats:sub>\n                    \/CO\n                    <jats:sub>2<\/jats:sub>\n                    , H\n                    <jats:sub>2<\/jats:sub>\n                    \/CH\n                    <jats:sub>4<\/jats:sub>\n                    and H\n                    <jats:sub>2<\/jats:sub>\n                    \/C\n                    <jats:sub>3<\/jats:sub>\n                    H\n                    <jats:sub>8<\/jats:sub>\n                    are 21.9, 63.1 and 134.4, respectively, which are much higher than those of the pristine TB\u2010COF membrane due to the precise size sieving channels brought about by the incorporated MOF. The synthesis of ZIF\u201067@TB\u2010COF membrane demonstrates the versatility of the synthesis strategy.\n                  <\/jats:p>","DOI":"10.1002\/anie.202419946","type":"journal-article","created":{"date-parts":[[2024,12,5]],"date-time":"2024-12-05T11:29:12Z","timestamp":1733398152000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":24,"title":["Vacuum\u2010Assisted Confined Growth of MOF@COF Composite Membranes with Enhanced Hydrogen Permselectivity"],"prefix":"10.1002","volume":"64","author":[{"given":"Siqi","family":"Li","sequence":"first","affiliation":[{"name":"State Key Laboratory of Molecular &amp; Process Engineering Shanghai Key Laboratory of Green Chemistry and Chemical Processes School of Chemistry and Molecular Engineering East China Normal University, 500  Dongchuan Road Shanghai 200241 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