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We report here a very simple and fast route to very high surface area, mechanically robust, hydrophobic polymer gels prepared by fluoride\u2010catalyzed hydrolysis of mixtures of MeSi(OEt)<jats:sub>3<\/jats:sub> and bis\u2010triethoxysilylethane (BTSE) at room temperature. These materials offer specific surface areas up to 1300\u2005m<jats:sup>2<\/jats:sup>\u2009g<jats:sup>\u22121<\/jats:sup>, peak pore sizes of 0.8\u2005nm and thermal stabilities above 200\u2009\u00b0C. The gelation times and surface areas can be controlled by adjusting the solvent volume (dichloromethane), percent fluoride (as <jats:italic>n<\/jats:italic>Bu<jats:sub>4<\/jats:sub>NF or TBAF) and the BTSE contents. Polymers with other corners and linkers were also explored. These materials will further expand the materials databank for use in vacuum insulation panels and as thermally stable release and capture media.<\/jats:p>","DOI":"10.1002\/chem.201704941","type":"journal-article","created":{"date-parts":[[2017,10,20]],"date-time":"2017-10-20T09:52:46Z","timestamp":1508493166000},"page":"274-280","source":"Crossref","is-referenced-by-count":7,"title":["High Surface Area, Thermally Stable, Hydrophobic, Microporous, Rigid Gels Generated at Ambient from MeSi(OEt)<sub>3<\/sub>\/(EtO)<sub>3<\/sub>SiCH<sub>2<\/sub>CH<sub>2<\/sub>Si(OEt)<sub>3<\/sub> Mixtures by F<sup>\u2212<\/sup>\u2010Catalyzed Hydrolysis"],"prefix":"10.1002","volume":"24","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-7040-0793","authenticated-orcid":false,"given":"Joseph C.","family":"Furgal","sequence":"first","affiliation":[{"name":"Department of Chemistry University of Michigan  Ann Arbor MI 48109 USA"},{"name":"Department of Chemistry &amp; Center for Photochemical Sciences Bowling Green State University  Bowling Green OH 43403 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Honami","family":"Yamane","sequence":"additional","affiliation":[{"name":"Department Polymer Chemistry Kyoto University  Kyoto Kyoto 606-8501 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Timothy R.","family":"Odykirk","sequence":"additional","affiliation":[{"name":"Department of Materials Science and Engineering University of Michigan  Ann Arbor MI 48109 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Eongyu","family":"Yi","sequence":"additional","affiliation":[{"name":"Department of Materials Science and Engineering University of Michigan  Ann Arbor MI 48109 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yoshiki","family":"Chujo","sequence":"additional","affiliation":[{"name":"Department Polymer Chemistry Kyoto University  Kyoto Kyoto 606-8501 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4939-3514","authenticated-orcid":false,"given":"Richard M.","family":"Laine","sequence":"additional","affiliation":[{"name":"Department of Materials Science and Engineering University of Michigan  Ann Arbor MI 48109 USA"},{"name":"Department of Macromolecular Science &amp; Engineering University of Michigan  Ann Arbor MI 48109 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2017,11,29]]},"reference":[{"key":"e_1_2_2_1_1","doi-asserted-by":"publisher","DOI":"10.1021\/ar970151f"},{"key":"e_1_2_2_2_1","doi-asserted-by":"publisher","DOI":"10.1021\/ja9916658"},{"key":"e_1_2_2_3_1","doi-asserted-by":"publisher","DOI":"10.1002\/(SICI)1521-3773(19990115)38:1\/2<56::AID-ANIE56>3.0.CO;2-E"},{"key":"e_1_2_2_3_2","doi-asserted-by":"publisher","DOI":"10.1002\/(SICI)1521-3757(19990115)111:1\/2<58::AID-ANGE58>3.0.CO;2-3"},{"key":"e_1_2_2_4_1","doi-asserted-by":"publisher","DOI":"10.1002\/1521-4095(200010)12:19<1403::AID-ADMA1403>3.0.CO;2-X"},{"key":"e_1_2_2_5_1","doi-asserted-by":"publisher","DOI":"10.1021\/cm011030j"},{"key":"e_1_2_2_6_1","doi-asserted-by":"publisher","DOI":"10.1021\/ar000034b"},{"key":"e_1_2_2_7_1","doi-asserted-by":"publisher","DOI":"10.1021\/cr0200062"},{"key":"e_1_2_2_8_1","doi-asserted-by":"publisher","DOI":"10.1021\/cr300014x"},{"key":"e_1_2_2_9_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.200703871"},{"key":"e_1_2_2_9_2","doi-asserted-by":"publisher","DOI":"10.1002\/ange.200703871"},{"key":"e_1_2_2_10_1","doi-asserted-by":"publisher","DOI":"10.1021\/jo061779j"},{"key":"e_1_2_2_11_1","doi-asserted-by":"publisher","DOI":"10.1021\/ma981839q"},{"key":"e_1_2_2_12_1","doi-asserted-by":"publisher","DOI":"10.1039\/C2CS35072F"},{"key":"e_1_2_2_13_1","doi-asserted-by":"publisher","DOI":"10.1021\/ja9808853"},{"key":"e_1_2_2_14_1","doi-asserted-by":"publisher","DOI":"10.1021\/ma101597h"},{"key":"e_1_2_2_15_1","doi-asserted-by":"publisher","DOI":"10.1021\/ja102453s"},{"key":"e_1_2_2_16_1","doi-asserted-by":"publisher","DOI":"10.1002\/marc.201200835"},{"key":"e_1_2_2_17_1","doi-asserted-by":"publisher","DOI":"10.1039\/c3ta12324c"},{"key":"e_1_2_2_18_1","doi-asserted-by":"publisher","DOI":"10.1002\/chem.201303759"},{"key":"e_1_2_2_19_1","doi-asserted-by":"publisher","DOI":"10.1039\/C3TA14746K"},{"key":"e_1_2_2_20_1","volume-title":"Sol-Gel Science: The Physics and Chemistry of Sol-Gel Processing","author":"Brinker C. 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