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Inspired by nature's disulfide bonds, which stabilize proteins and enable redox activity, this study introduces a hierarchically porous poly(aryl thioether) photocatalyst via dual disulfide and thioether linkages formed by polycondensation. Thiolate intermediates undergo partial oxidation in air, yielding a micro\/mesoporous polymer with a 757\u00a0m\n                    <jats:sup>2<\/jats:sup>\n                    \u00a0g\u207b\u00b9 surface area, comparable to its microporous counterpart synthesized in N\u2082. This structure exhibits enhanced adsorption capacity, as demonstrated by tests with volatile organic compounds and mercury ions. The disulfide\u2010functionalized pore walls enable thiyl radical formation under visible light, achieving outstanding diphenylacetylene oxidation performance. This heterogeneous photocatalyst surpasses homogeneous systems, showing &gt;99% conversion efficiency with 3.5% apparent quantum yield at 440\u00a0nm. This study pioneers a linker engineering strategy to integrate hierarchical porous structure and photoactive radical generation in a single porous polymer photocatalyst.\n                  <\/jats:p>","DOI":"10.1002\/smll.202501398","type":"journal-article","created":{"date-parts":[[2025,3,11]],"date-time":"2025-03-11T21:43:38Z","timestamp":1741729418000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["Hierarchically Porous Poly(aryl thioether)s Through Dynamic Linker Engineering for Thiyl Radical Photocatalysis"],"prefix":"10.1002","volume":"21","author":[{"given":"Sunil","family":"Kumar","sequence":"first","affiliation":[{"name":"Water Cycle Research Center Korea Institute of Science and Technology (KIST)  Seoul 02792 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Doyun","family":"Kim","sequence":"additional","affiliation":[{"name":"Department of Chemical and Biomolecular Engineering Korea Advanced Institute of Science and Technology (KAIST)  291 Daehak\u2010ro, Yuseong\u2010gu Daejeon 34141 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Youngdong","family":"Song","sequence":"additional","affiliation":[{"name":"Department of Chemical and Biomolecular Engineering Korea Advanced Institute of Science and Technology (KAIST)  291 Daehak\u2010ro, Yuseong\u2010gu Daejeon 34141 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Bolormaa","family":"Bayarkhuu","sequence":"additional","affiliation":[{"name":"Water Cycle Research Center Korea Institute of Science and Technology (KIST)  Seoul 02792 Republic of Korea"},{"name":"Division of Energy and Environment Technology KIST\u2010School University of Science and Technology  Seoul 02792 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jueun","family":"Park","sequence":"additional","affiliation":[{"name":"Water Cycle Research Center Korea Institute of Science and Technology (KIST)  Seoul 02792 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Donghee","family":"Hoh","sequence":"additional","affiliation":[{"name":"MSU\u2010DOE Plant Research Laboratory Michigan State University  East Lansing Michigan 48824 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Cafer T.","family":"Yavuz","sequence":"additional","affiliation":[{"name":"Oxide &amp; Organic Nanomaterials for Energy &amp; Environment Laboratory Chemistry Program Physical Science &amp; Engineering (PSE) King Abdullah University of Science and Technology (KAUST)  Thuwal 23955 Saudi Arabia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1548-2017","authenticated-orcid":false,"given":"Jeehye","family":"Byun","sequence":"additional","affiliation":[{"name":"Water Cycle Research Center Korea Institute of Science and Technology (KIST)  Seoul 02792 Republic of Korea"},{"name":"Division of Energy and Environment Technology KIST\u2010School University of Science and Technology  Seoul 02792 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2025,3,3]]},"reference":[{"key":"e_1_2_8_1_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.chemrev.6b00439"},{"key":"e_1_2_8_2_1","doi-asserted-by":"publisher","DOI":"10.1002\/adma.202210082"},{"key":"e_1_2_8_2_2","doi-asserted-by":"publisher","DOI":"10.1126\/science.1221383"},{"key":"e_1_2_8_3_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.chempr.2024.05.022"},{"key":"e_1_2_8_3_2","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-024-49379-7"},{"key":"e_1_2_8_4_1","doi-asserted-by":"publisher","DOI":"10.1002\/adma.201806254"},{"key":"e_1_2_8_5_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.accounts.2c00262"},{"key":"e_1_2_8_5_2","doi-asserted-by":"publisher","DOI":"10.1002\/anie.201610914"},{"key":"e_1_2_8_6_1","doi-asserted-by":"publisher","DOI":"10.1002\/advs.202400626"},{"key":"e_1_2_8_6_2","doi-asserted-by":"publisher","DOI":"10.1039\/D0CS00049C"},{"key":"e_1_2_8_7_1","doi-asserted-by":"publisher","DOI":"10.1021\/cb3005269"},{"key":"e_1_2_8_8_1","doi-asserted-by":"crossref","unstructured":"M. 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