Fe doped TiO2 nanoparticles were prepared under high temperature and pressure conditions by mixture of metal nitrate solution and TiO2 sol. Fe doped TiO2 particles were reacted in the temperature range of 170 to 200˚C for 6 h. The microstructure and phase of the synthesized Fe doped TiO2 nanoparticles were studied by SEM (FE-SEM), TEM, and XRD. Thermal properties of the synthesized Fe doped TiO2 nanoparticles were studied by TG-DTA analysis. TEM and X-ray diffraction pattern shows that the synthesized Fe doped TiO2 nanoparticles were crystalline. The average size and distribution of the synthesized Fe doped TiO2 nanoparticles were about 10 nm and narrow, respectively. The average size of the synthesized Fe doped TiO2 nanoparticles increased as the reaction temperature increased. The overall reduction in weight of Fe doped TiO2 nanoparticles was about 16% up to ~700˚C; water of crystallization was dehydrated at 271˚C. The transition of Fe doped TiO2 nanoparticle phase from anatase to rutile occurred at almost 561˚C. The amount of rutile phase of the synthesized Fe doped TiO2 nanoparticles increased with decreasing Fe concentration. The effects of synthesis parameters, such as the concentration of the starting solution and the reaction temperature, are discussed.