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Published on Web 08/10/2006 Triconstituent Co-assembly to Ordered Mesostructured PolymerSilica and CarbonSilica Nanocomposites and Large-Pore Mesoporous Carbons with High Surface Areas Ruili Liu,† Yifeng Shi,† Ying Wan,†,‡ Yan Meng,† Fuqiang Zhang,† Dong Gu,† Zhenxia Chen,† Bo Tu,† and Dongyuan Zhao*,†,§,# Contribution from the Department of Chemistry, Shanghai Key Laboratory of Molecular Catalysis and Innoatie Materials, Key Laboratory of Molecular Engineering of Polymers, and Adanced Materials Laboratory, Fudan Uniersity, Shanghai 200433, People’s Republic of China, and Department of Chemistry, Shanghai Normal Uni ersity, Shanghai 200234, People’s Republic of China Received May 14, 2006; E-mail: dyzhao@ Abstract: Highly ordered mesoporous polymersilica and carbonsilica nanocomposites with interpenetrat- ing networks have been successfully synthesized by the evaporation-induced triconstituent co-assembly method, wherein soluble resol polymer is used as an organic precursor, prehydrolyzed TEOS is used as an inorganic precursor, and triblock copolymer F127 is used as a template. It is proposed for the first time that ordered mesoporous nanocomposites have “reinforced concrete”-structured frameworks. By adjusting the initial mass ratios of TEOS to resol, we determined the obtained nanocomposites possess continuous composition with the ratios ranging from zero to inf