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Here, we have designed a functional 3D COF (DPP\u2010TAM\u2010COF) and successfully modulated it into diverse nano\u2010architectures, including nano\u2010ring, hollow\u2010sphere, and nano\u2010urchin, through a solvent\u2010driven tuning strategy. The produced nano\u2010architectures possess bifunctional groups, well\u2010tuned morphology, high porosity, and photothermal properties that can be applied in efficient photothermal biomass valorization coupled with hydrogen peroxide production. Specifically, they can realize the furfuryl alcohol conversion into furoic acid with an optimal generation efficiency of 39.0 mmol\/g coupled with the efficient hydrogen peroxide production, which is superior to the majority of reported materials. Based on various characterizations and theoretical calculations, the functions of nano\u2010architectures and bifunctional groups have been validated in the coupling reaction. Aiming at extending the application regimes of 3D COFs, this work might give new insights into the structure or morphology study of 3D COFs.<\/jats:p>","DOI":"10.1002\/anie.2408330","type":"journal-article","created":{"date-parts":[[2026,8,7]],"date-time":"2026-08-07T13:08:01Z","timestamp":1786108081000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Solvent\u2010Driven Modulation of Covalent\u2010Organic Framework Nano\u2010Architectures for Photothermal\u2010Catalytic Biomass Valorization and Hydrogen Peroxide Production"],"prefix":"10.1002","volume":"65","author":[{"given":"Yi\u2010Lu","family":"Yang","sequence":"first","affiliation":[{"name":"Guangdong Provincial Key Laboratory of Carbon Dioxide Resource Utilization School of Chemistry South China Normal University  Guangzhou P. R. 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