TiO2(1-.ZrO2. (.=- 0.2, 0.4, 0.6 and 0.8) composite powders having a homogeneous distribution and nanocrystalline were successfully synthesized by sol-gel process using titanium iso-propoxide as precursor. The particle sizes of TiO2-ZrO2 powders calcined at 600°C were measured ranging from 10nm to 19nm by XRD and TEM. For the comparison of photocatalytic activity, TiO2-ZrO2 composite powders were tested in the degradation of phenol and the photoreduction of inorganic pollutants. The degradation of phenol increased with increase the content of anatase TiO2 phase.