Nanostructured NiTiO3 and NiTiO3-TiO2 nanocomposite were prepared by a low temperature modified sal-gel method. A calcination temperature of 600 degrees C determined by thermal gravimetric analysis was applied for converting prepared gel to oxide materials. X-ray differactometry and transmission electron microscopy were used for characterization of crystal structure and morphology of prepared materials. A crystallite size of 20-30 nm for nickel titanate and a nanoparticle size smaller than 50 nm were obtained for prepared samples. Brunauer-Emmett-Teller analysis showed the behavior of mesoporous materials with small adsorbate-adsorbent interaction potentials. By using UV-Vis diffuse reflectance spectroscopy and Mott-Schottky analysis, the energy band structures of nanostructured NiTiO3 and NiTiO3-TiO2 nanocomposite were determined and forward bias of cyclic voltammograms of samples were interpreted in terms of their energy band structure. (C) 2014 Elsevier Ltd. All rights reserved.