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TiO2 nanoparticles with different phases are prepared by hydrolysis of titanium tetrabutoxide in the presence of HCl. The composition and microstructure of the resulting samples are studied by XRD and TEM. These results show that the range of particle size of TiO2 is from 20 to 30 nm. The mechanism of TiO2 photocatalysis reaction has been discussed extensively. Photocatalytic activities of nanometer TiO2 are also evaluated by degradation of the crystal violet solution. Experimental results indicate that the synergistic action of H2O2 and ultrasonic wave greatly enhances photo-catalytic reaction of TiO2.