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However, the design and synthesis of three\u2010dimensional (3D) sp<jats:sup>2<\/jats:sup>\u2010carbon\u2010conjugated COPs, along with their photocatalytic performances, remain underexplored. Here, we synthesized two novel vinylene\u2010linked fully conjugated 3D COPs (BUCT\u2010COP\u201050 and BUCT\u2010COP\u201051) through the saddle\u2010shaped building blocks. Under visible\u2010light irradiation, both materials demonstrated efficient hydrogen peroxide\u00a0(H<jats:sub>2<\/jats:sub>O<jats:sub>2<\/jats:sub>) generation, with BUCT\u2010COP\u201051 (thiophene\u2010enriched) achieving a remarkable production rate of 3.21\u00a0mmol g<jats:sup>\u22121<\/jats:sup> h<jats:sup>\u22121<\/jats:sup> in pure water, higher than BUCT\u2010COP\u201050 (benzene\u2010modified, 2.16\u00a0mmol g<jats:sup>\u22121<\/jats:sup> h<jats:sup>\u22121<\/jats:sup>). Mechanistic investigations revealed that the H<jats:sub>2<\/jats:sub>O<jats:sub>2<\/jats:sub> generation predominantly proceeded via the indirect two\u2010electron oxygen reduction reaction pathway. The superior performance for BUCT\u2010COP\u201051 could attributed to its narrower bandgap, broader light absorption range, and higher conductivity. This work illustrates that vinylene linked fully conjugated 3D COPs could be as promising semiconductors in environmental and energy\u2010related fields.<\/jats:p>","DOI":"10.1002\/chem.202501480","type":"journal-article","created":{"date-parts":[[2025,6,12]],"date-time":"2025-06-12T02:09:36Z","timestamp":1749694176000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":7,"title":["Vinylene\u2010Linked Fully Conjugated 3D Covalent Organic Polymers for Photocatalytic H<sub>2<\/sub>O<sub>2<\/sub> Production"],"prefix":"10.1002","volume":"31","author":[{"given":"Rui","family":"Zhang","sequence":"first","affiliation":[{"name":"State Key Laboratory of Organic\u2010Inorganic Composites Beijing University of Chemical Technology  Beijing 100029 P. R. 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