Supramolecular assemblies of surfactant molecules are often used to synthesize mesoporous silica (MPS). However, elimination of the surfactant molecules by conventional thermocalcination after MPS film synthesis often leads to film distortion or breakage. Here the effective removal of surfactant molecules at room temperature is described in which the hexagonal mesostructure of the film is preserved. The technique used-photocalcination-is based on the photochemical decomposition of organic molecules under irradiation with vacuum ultraviolet light.