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Herein, a binary meso\u2010reconstruction strategy to develop biomimetic sub\u2010nanoporous engineered aerogel molecular sieves (NAMSs) with reversible nanogating channels is demonstrated, in which sub\u20101 nm pores (\u22487 \u00c5) provide coupling size\u2010thermodynamic gated functions that enable molecule discrimination and trapping in a reversible manner. The NAMSs show polarity\u2010reversible adsorption in which adsorbate molecules are discriminated by each gate\u2010admission sponge\u2010fiber molecular sieve, facilitating size\/interface synergistically induced selective separation of 1,3,5\u2010trimethyl benzene\/ethylene glycol with high separation factor and fast adsorption rate. The nanogating aerogel molecular sieves with molecularly defined sub\u20101\u00a0nm nanoporous architecture (\u22487 \u00c5), Murray's law hierarchical channels, ultrahigh surface area (686 m<jats:sup>2<\/jats:sup> g<jats:sup>\u22121<\/jats:sup>), and robust self\u2010supporting characteristics define a new benchmark for both aerogels and molecular sieves, exhibiting great potential in diversified on\u2010demand molecular separations that are prevalent in chemical, energy, and environmental processes.<\/jats:p>","DOI":"10.1002\/smll.202202173","type":"journal-article","created":{"date-parts":[[2022,5,24]],"date-time":"2022-05-24T12:18:56Z","timestamp":1653394736000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":22,"title":["Sub\u2010Nanoporous Engineered Fibrous Aerogel Molecular Sieves with Nanogating Channels for Reversible Molecular Separation"],"prefix":"10.1002","volume":"18","author":[{"given":"Feng","family":"Zhang","sequence":"first","affiliation":[{"name":"State Key Laboratory for Modification of Chemical Fibers and Polymer Materials, College of Textiles Donghua University  Shanghai 201620 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8716-0549","authenticated-orcid":false,"given":"Yang","family":"Si","sequence":"additional","affiliation":[{"name":"State Key Laboratory for Modification of Chemical Fibers and Polymer Materials, College of Textiles Donghua University  Shanghai 201620 China"},{"name":"Innovation Center for Textile Science and Technology Donghua University  Shanghai 200051 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jianyong","family":"Yu","sequence":"additional","affiliation":[{"name":"State Key Laboratory for Modification of Chemical Fibers and Polymer Materials, College of Textiles Donghua University  Shanghai 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