In this work, visible light responsive (VLR)ZrTiO4/Bi2O3 photocatalysts were successfully synthesized by a hydrothermal method. The prepared ZrTiO4/Bi2O3 photocatalysts were characterized by X-ray diffraction studies (XRD), X-ray photoelectron spectroscopy (XPS), diffuse reflectance spectroscopy (DRS), photoluminescence (PL) and transmission electron microscopy (TEM) analyses. DRS results revealed that the extent of light absorption towards the visible region of the spectrum increased with an increase in the calcination temperature of the catalysts up to 450 degrees C and then started to decrease. The decrease in absorption at high temperatures was mainly due to the formation of polycrystalline ZrTiO4/Bi2O3 from the tetragonal Bi2O3 pure oxide particles. All the metals present in the ZrTiO4/Bi2O3 composite nano-particles also exhibited corresponding oxide states. Particle sizes of about 7 nin were obtained during this combined method of preparation, especially with the catalysts calcined at 450 degrees C. The photocatalytic activity of the catalysts was measured using 4-chlorophenol as a model pollutant for these environmental remediation studies. Among the catalysts calcined at different temperatures, the samples calcined at 450 degrees C showed the most remarkable degradation of 4-chlorophenol, higher than not only the other calcined catalysts but also the commercially available Degussa P-25. This is due to the formation of smaller particle sizes, a higher surface area and stronger absorption in the visible light irradiation for these catalysts calcined at 450 degrees C. Thus, such new VLR photocatalysts can be expected to work effectively under visible light regions as an applicable alternative photocatalyst for commercial scale use. (C) 2010 Elsevier B.V. All rights reserved.