The first part of this thesis is the preparation and characterization of the metal-doped TiO2 nanoparticles. The preparation method was based on a nonaqueous sol-gel route using benzyl alcohol as solvent and titanium tetrachloride together with other metallic compound as metal precursors. The obtained metal-doped TiO2 materials were characterized by ICP-AES, XRD, TGA-DSC, UV-Vis, XPS and TEM. The results indicated that these materials were in the nanometer scale and were with highly crystalline and pure anatase phase. The tin-doped TiO2 and cobalt-doped TiO2 nanoparticles both showed higher photocatalytic activity as compared to undoped TiO2 nanoparticles. The second part of this thesis is the preparation and characterization of the TiO2/SnO2 nanocomposites. The nanocomposites were synthesized by a seed-mediated growth approach, using SnO2 nanocrystals as seeds and a mixture of TiCl4 and benzyl alcohol as a growth solution. The XRD and TEM characterizations indicated that the TiO2/SnO2 nanocomposites exhibited a flower-like morphology with uniform size, and the two metal oxides were with rutile and cassiterite phases, respectively.