A naosized TiO2 powder was successfully prepared by the hydrolysis of titanium isopropoxide through sol-gel process. The microstructure of TiO2 powder was investigated by transmission electron microscopy and X-ray diffraction. Both anatase and rutile phases were found in TiO2 powder annealed for 1 hour at 600 degrees C. The characteristics of X-ray photoelectron spectra and infrared spectra could be affected by the size and aggregation state of the microsrystalc constituting the TiO2 powder.