Abstract: A series of nanocomposite of TiO2 thin films and multi-walled carbon nanotubes (MWCNTs) in different forms were prepared by sol-gel methods. The surface morphologies of the nanocomposite films were characterized via scanning electron microscopy (SEM). The effects of inducing MWCNTs into TiO2 thin film on the structure and absorption properties of TiO2 were characterized by X-ray diffraction (XRD) and UV-Vis spectrophotometer methods. The nanocomposite films were also characterized by photoelectrochemical methods. The results showed that the MWCNTs/TiO2 nanocomposite films were porous and rough and the absorption edge can extend to visible light region. The photoelectrochemical properties of TiO2 could be evidently enhanced by bottom distribution mode, or otherwise, decreased by surface distribution mode and uniform distribution mode. The effects of composite modes on the photoelectrochemical activities were discussed in terms of separation of charge carriers. MWCNTs distributed in bottommode within the nanocomposite filmcould improve electron-collecting efficiency and reduce recombination.