Microporous and mesoporous materials have found great utility as catalysts and adsorption media because of their large internal surface area. Since the discovery of surfactant-templated mesoporous silica materials in 1992, the new developing periodic mesoporous organosilica material (PMO) has received much attention. In this present work, a PMO material, amino-functionalized mesoporous silica thin films with 3D hexagonal structure, were synthesized by self-assembly co-condensation of tetraethoxy silane (TEOS) and 3-aminopropyltriethoxysiliane (APTES) precursors in various ratios, in the presence of cetyltrimethyl ammonium bromide acting as the structure-directing agent. The thin films were characterized by small-angle X-ray diffraction, grazing incidence small angle X-ray scattering, Fourier transform infrared, transmission electron microscope, thermogravimetric analysis, and N-2 adsorption. Results show that when the APTES/(TEOS+APTES) ratio was 0.10, the mesoporous organosilica thin film has high degree of order, an average pore size of 2.16 nm, a large BET-specific surface area of 1560 m(2)/g and a large pore volume of 0.76 cm(3)/g.