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Abstract

Homogeneous integration of nanomaterials into mesoporous metal oxides (MMOs) remains a long-standing challenge, as conventional solvent evaporation–driven block copolymer self-assembly often leads to phase segregation and structural inhomogeneity, thereby hindering the realization of synergistic effects between MMOs and nanomaterials. Herein, we introduce an ultrafast condensation-induced self-assembly (CISA) strategy that leverages the rapid condensation of metal alkoxides in block copolymer solutions to trigger self-assembly within seconds. This rapid solution-phase process enables the uniform incorporation of 1D/2D nanomaterials into mesostructured MMOs. The resulting nanocomposites exhibit enhanced lithium-ion battery performance over their MMO counterparts. Furthermore, as CISA process avoids solvent evaporation and employs a green solvent (acetone), it allows complete solvent recovery through a simple purification step, enhancing the environmental sustainability. In addition, by introducing condensation instead of evaporation as a new driving force for block copolymer self-assembly, CISA offers a versatile platform for the green synthesis of MMOs and their nanocomposites with broad applications in energy storage, catalysis, and sensing.