TiO2 nanotubes with outer diameters of similar to 10 nm and lengths of several hundreds nanometer were synthesized by the hydrothermal method. The morphology of the nanotubes was thoroughly examined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM), The composition and structure of tubular materials were determined by energy dispersive x-ray spectroscopy, selected area electron diffraction pattern, and x-ray diffraction (XRD). XRD results confirmed that the nanotubes are composed of pure anstase TiO2. Both TEM and the Barrett-Joyner-Halenda methods indicated that the inner diameters of the nanotubes are around 7 run, In addition, the hybrid of poly(3-hexylthiophene) and TiO2 nanotube were prepared by the oxidative polymerization of 3-hexylthiophene in the presence of TiO2 nanotubes. The obtained composites were characterized by SEM, Fourier transformed infrared spectroscopy, and thermal gravmetric analysis. (c) 2005 American Vacuum Society.