In this study, nanoscale photocatalyst TiO 2 powders were synthesized via sol-gel and flame spray pyrolysis (FSP). Phase structures and ratios were analyzed by X-ray diffractometer (XRD). Size, specific surface area, and morphologies were determined using particle size analyzer, Brunauer-Emmett-Teller theory, and scanning electron microscope, respectively. Anatase phase with some rutile together was obtained in XRD analysis. The degradation rates of aqueous methylene blue (MB) by TiO 2 nanopowders were calculated using UV-vis spectrophotometer. It was found that MB decomposition was successfully achieved with significantly high efficiencies for both sol-gel and FSP-derived powders with small differences.