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A new hierarchical structure of TiO2-ZnO nanorod-nanosheet was prepared by two-step hydrothermal method without any seed layers. A spin-coating assisted successive ionic layer reaction method (SC-SILR) was used to deposit the CdS nanocrystals into the TiO2 nanorod array and the TiO2-ZnO hierarchical nanostructure to form the CdS/TiO2 and CdS/TiO2-ZnO nanocomposite films. Different analysis methods, such as SEM, TEM, XRD, UV-Vis and transient photocurrent, were utilized to characterize the morphologies, structures of the samples and investigate the light absorption properties, the photoelectric conversion performance of the electrodes. The results indicated that the transient photocurrent of the TiO2-ZnO hierarchical nanostructure film was apparently superior to the TiO2 nanorod array film after depositing the photosensitive layer of CdS and showed an evident enhancement at wavelength of 500 nm. Hybrid solar cells were assembled using P3HT as p- type polymer materials. Photovoltaic measurement results indicated that the energy conversion efficiency of the hybrid solar cell based on the hierarchical structure of P3HT/CdS/TiO2-ZnO composite film could reach 0.65%, which revealed an increasing of 58% compared with that of the hybrid solar cell based on the P3HT/CdS/ TiO2 composite film. [ABSTRACT FROM AUTHOR]