We synthesized the highly ordered mesoporous thin films with alkyltrimethyl-ammonium (CnTMA+). The arrangement of mesopores was depend on the Si/surfactant ratio. The hexagonal(P6mm) arrangement was observed, when Surfactant/Si ratio was 1/10. Increasing the Surfactant/Si ratio to 1.6/10, the cubic (Pm3n) arrangements were observed. A steel vessel for the measurement of the nitrogen adsorption isotherms of thin film on the substrate was designed. It was found that mesopore arrangements in the film is more regular than that in the powder samples prepared by the same acidic synthesis conditions.