Semiconductor-organic composite films built up of titania and surfactants (e.g. C 1 6 TAB, C 1 4 TAB, C 1 2 TAB) have been prepared on glass substrates at 50 o C in air and under hydrothermal conditions, respectively. XRD, SEM, TEM and UV-VIS diffuse reflectance spectra studies indicate that a lamellar mesostructure with d spacing of 34 Å is obtained and the thickness of the titania layer intercalated between organic layers is less than 1 nm.