Zirconium-stannate titanate Zr 1−x Sn x TiO 4 (ZTS) thin films, undoped and doped with Sb, Ta and Nb, were prepared by a polymeric precursor technique. The ZTS films were deposited on the multilayered substrates (Pt/Ti/SiO 2 /Si) by means of multiple spin-coating. After this deposition, the samples were heated at different temperatures (300-700• C). The chemical composition of these films and bulk ZTS samples was investigated by using x-ray photoelectron spectroscopy and selected-area XPS depth profiling. A partial surface segregation of Sn IV and the presence of Sn 0 , Ti II and Ti III species in the films were revealed from XPS depth profiles. An optimized ZTS deposition process, where an oxidizing agent (H 2 O 2 ) is added to the gel, is proposed.