Ti 3+ self-doped titanium-zinc hybrid oxides with different phase compositions and morphologies were successfully synthesized using Zn powder as the reductant and Zn source by a chemical-reduction precipitation method with subsequent thermal treatment. The fabricated Ti 3+ self-doped TiO 2 (A)/TiO 2 (R), TiO 2 (A)/TiO 2 (R)/ZnTiO 3 , and TiO 2 (A)/ZnO heterojunctions were characterized by X-ray diffraction, transmission electron microscopy, high-resolution transmission electron microcopy, X-ray photoelectron spectroscopy, and UV-Vis diffuse reflectance spectroscopy. The effects of various Ti/Zn molar ratios and preparation processes on the structural, morphological, optical, photocurrent and photocatalytic properties of the resultant samples were investigated systematically. Results reveal that Ti 3+ self-doping enhances the photoabsorption capability of titanium-zinc hybrid oxides in the visible-light region. Moreover, different processes and Ti/Zn molar ratios play great influences on the structure, morphology, optical, photocurrent and photocatalytic properties of the final products. Ti 3+ self-doped titanium-zinc hybrid oxides exhibit excellent photocurrent and photocatalytic