International audienceThin films of thulium and ytterbium-doped titanium oxide were grown by metal-organic spray pyrolysis deposition from titanium(IV)oxide bis(acetylacetonate), thulium(III) tris(2,2,6,6-tetramethyl-3,5-heptanedionate) and ytterbium(III) tris(acetylacetonate). Deposition temperatures have been investigated from 300 to 600 A degrees C. Films have been studied regarding their crystallinity and doping quality. Structural and composition characterisations of TiO2:Tm,Yb were performed by electron microprobe, x-ray diffraction, and Fourier transform infrared spectroscopy. The deposition rate can reach 0.8 mu m/h. The anatase phase of TiO2 was obtained after synthesis at 400 A degrees C or higher. Organic contamination at low deposition temperature is eliminated by annealing treatments