Swelling‐agent‐free synthesis of mesocellular foam (MCF)‐like silica mesophases by a pH‐dependent structural transformation using carboxy‐terminated triblock copolymer Pluronic P123 has been discovered. The structural properties of the MCF‐like silica materials can be modulated by controlled calcination or post‐synthesis treatment with sulfuric acid, and either closed‐cell or open‐cell mesostructures have been prepared. The MCF‐like silica mesophases have also been applied as hard templates to prepare MCF‐like carbon materials via a nanocasting route. Furthermore, the swelling‐agent‐free synthesis has been found to be less sensitive to the presence of organosilanes, and the cocondensation syntheses of functional MCF‐like materials with carboxyethyl, iodopropyl, or mercaptopropyl groups have also been demonstrated.

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