KeywordsSemiconductors, Sol-Gel Chemistry, X-ray Diffraction, Transmission Electron Microscopy (TEM), Catalytic Properties TiO 2 and ZrO 2 /TiO 2 composite microsphere particles were synthesized using the sol-gel method. Photoactivity of TiO 2 and ZrO 2 /TiO 2 were compared. Particles were characterized using X-ray diffraction (XRD), infrared spectroscopy (FTIR), scanning electron microscopy (SEM) of X-ray (EDAX), and transmission electron microscopy (TEM). The study revealed that TiO 2 particles were microspheres. The decorating of ZrO 2 particles on TiO 2 surface was successfully carried out that was proved by SEM and TEM analyzes. The photo-catalytic activity of TiO 2 and ZrO 2 /TiO 2 composite microsphere particles was examined using methylene blue (MB) as reference material under UV lamp. Our findings showed that ZrO 2 /TiO 2 was more active than TiO 2 . These findings suggest a new TiO 2 -based catalyst structure to synthesize and to emphasize the importance of the shape of the catalyst.