Abstract: Ultrafine powder （UFP） TiO₂ doped with ZnO and NiO were prepared by sol-gel method in CH₃CH₂OH solvent. The doped TiO₂ UFP were character ized by TG-DTA、XRD and TEM. The experimental results showed that Stable anatase phase solid solution UFP which was doped with 10mol%, 15mol% ZnO or NiO were obtained, TEM photographs showed that amorphous ZnO or NiO was absorbed on the surface of TiO₂ solid solution particles when doped amount is more than 20mol%, The experimental results also showed that, the crystalline temperature from amorphous to anatase phase went up and stability of solid solution of anatase phase lowered with increament of doped cations amounts, and the crystalline temperature of samples doped with NiO is higher than that of samples doped with ZnO in the same doped amount, but the temperature of solid state reaction of the former is lower than that of the latter.