Since mesoporous materials can be prepared by combining the sol-gel chemistry and the structuring effect of surfactants, they have attracted attention for application in various high technology fields. The present work deals with the analyses of the mechanisms involved in the formation of SiO₂ and TiO₂ highly organised 2D-hexagonal meso-structured films using Brij 58 as surfactant. The preparation of such films by dip-coating involves rapid evaporation which makes the different steps difficult to control. Simultaneous in-situ SAXS (synchrotron) and interferometry analyses have been performed to get a first understanding of the self-assembly process. SiO₂ and TiO₂ materials have a different chemical reactivity (kinetics and coordination aspects). However, we show that the mechanisms involved during dip-coating are quite similar : The self-assembly leading to the organised phase takes place at a final stage of the drying process, involves the formation of a disorganised intermediate phase and depends also on the presence of micellar interfaces in addition to film/air and film/substrate interfaces.

The preparation and characterization of optically uniform mesoporous TiO thin films that present a high regularity in the pore mesostructure and orientation is reported. In addition, these films of optical quality are crack-free as confirmed on the nanometer and micrometer scales by electron microscopy. These films showed overall good optical quality as well as a high degree of organization before and after removal of the organic template and consolidation of the inorganic network.