Highly photocatalytically active anatase TiO 2 were synthesized by a solvothermal method using tetrabutyl titanate (TBT), citric acid, and ethanol as row material. The morphology and photocatalytic activity of titanium oxide have changed significantly with the presence of surfactants, such as cetyltrimethylammonium bromide (CTAB), sodium dodecylbenzenesulfonate (SDBS), and diethanolamine (DEA). Scanning electron microscope and X-ray powder diffraction results show that the synthesized products are anatase TiO 2 spherical particles with a micronanostructure. The crystal type of TiO 2 has no obvious change with the addition of different surfactants, but the morphology, size, and dispersion of the TiO 2 particles have changed to some extent. Among the three surfactants, CTAB is beneficial to reduce TiO 2 particle size and improve TiO 2 dispersion and agglomeration. DEA is favor to self-assembly the nanocrystals into spherical particles. Degradation of methyl orange photocatalyzed by TiO 2 prepared with CTAB as surfactant reaches 95.4% under ultraviolet light for 100 min. After five recycles, the catalyst did not exhibit significant loss of photocatalytic activity, confirming that the photocatalyst is essentially stable. This work indicates that the surfactant-assisted solvothermal method is an effective approach to improve the structure, morphology, and photocatalytic performance of TiO 2 . Moreover, the surfactants with various types can interact with the precursors of TiO 2 in different ways.