Both powder-type and film-type mesoporous silica materials have been prepared by using a sol-gel process in highly acidic, solvent-rich and mild conditions by solvent evaporation method. Powder mesoporous silica which has hexagonal arrays was well synthesized within only 10 minutes, and mesoporous film was formed on the glass plate within only several seconds by supramolecular interactions between the silicate species and surfactant-templates. In particular, the synthesis time was very short compared with that of hydrothermal synthesis owing to the solvent evaporation. This method has some characteristics different from the hydrothermal method such as the following. There is no precipitation because particles do not form in the solution before solvent evaporation, bulk powder is rigid, whereas that of hydrothermal synthesis is very soft and mesoporous materials are synthesized in acidic condition. Solvent evaporation method for the synthesis of mesoporous materials is promising because the method is very simple and time-saving.