A comparative study of TiO 2 powders prepared by precipitation and sol-gel methods was conducted. Titanium tetrachloride and titanium tetraisopropoxide were used as the starting materials for the precipitation and sol-gel processes, respectively. The effects of the two different drying methods, freeze drying and normal drying at 100°C, of the precipitates on the properties of the prepared TiO 2 powders were also investigated. The effects of the synthesis methods on phase, surface area, crystallite size, and photodegradation of methylene blue were studied by XRD, SEM, TEM, BET, and UV/ Vis techniques. It was found that the major phase of the synthesized TiO 2 was anatase, but small amounts of the brookite phase (Ͻ10 %) were found in some samples. The synthesized anatase TiO 2 with no pretreatment was found to be stable up to 600°C for the samples prepared by the precipitation