In this work, we synthesized and characterized mesoporous thin films of SiO2 and NiTiO3 structured by a surfactant called Brij58. These films were fabricated by the method of dip coating and the best conditions for well-structured thin films were investigated as a function of surfactant concentration and different types of substrates. These films have been characterized by X-ray reflectivity which was calculated using the matrix formalism. We demonstrated that the silicon substrate had a great effect on the structure and porosity of the fabricated films for both SiO2 and NiTiO3. Furthermore, we found that mesoporosity has been increased as a function of the surfactant concentration in the solution. This experimental procedure allows also to produce NiTiO3 powders which have been characterized by X-ray diffraction. The XRD coupled to the crystallographic software Maudshows that the samples are constituted by 98, 2% NiTiO3 powders.