Sphere-like rutile TiO2 nanocrystals have been synthesized by sol-gel method followed by hydrolysis of titanium tetrachloride in deionized water in the presence of ammonium hydroxide as hydrolysis catalyst. The as-prepared TiO2 nanoparticles have single rutile phase with average diameter approximately 26.4 nm. The results show that the temperature has a great influence on the particle size distribution and also crystalline phase (rutile) of TiO2 nanoparticles is consistent with the temperature. Characterization of the as-prepared nanocrystalline powder was carried out by different techniques such as powder X-ray diffraction (XRD), field emission transmission electron microscopy (FE-TEM) and Raman spectroscopy.