Nanocrystalline TiO2 powders have been selectively prepared by the simple combustion reaction method using urea as a fuel. The crystalline powder was obtained using a silica basin heated directly on a hot plate at 500 °C until self-ignition occurred. After combustion process, the calcined products were obtained by heating the as-prepared powders for 1 h in air atmosphere at various sintering temperatures [500–900 °C]. The obtained nanopowder materials were systematically characterized by X-day diffraction (XRD), micro-Raman, UV–visible absorption (UV–vis), and Fourier transform infrared (FT-IR) spectroscopics. Powder XRD pattern shows the good agreement rutile phase structured TiO2 and the sharp diffraction peaks indicates good for crystallinity. The size of a symmetry of the nanoparticles have been measured with aid of a scanning electron microscopy (SEM), high resolution transmission electron microscopy (HR-TEM), and Brunauer, Emmett and Teller (BET) surface studies. The crystallinity of the powders was found to increase with respect to calcination temperatures. The average specific surface area of the particle was probed using gas adsorption–desorption measurements. Raman spectroscopy experiment was performed to ascertain the nature of TiO2 powder quality. UV–vis absorption spectra results showed the changes in the absorption edges of TiO2 report to increasing the calcinations temperatures.