Fe(III) doped TiO2 with mole ratio of 0.1 was prepared by solvothermal method in the presence of isopropyl alcohol using PEG as a template. Characterization of prepared catalysts by TGA-DTA, XRD, SEM, surface area, UV-DRS, XRF, Zeta potential and XANES was investigated. Catalyst calcined at 500°C exhibited pure phase of anatase nanoparticles with high surface area (52m2/g), while higher calcination temperature generated a trace amount of pseudobrookite (Fe2TiO5) and finally transformed anatase TiO2 to rutile decreasing the surface area. Red shift phenomenon due to substitution of Fe(III) in the TiO2 crystal lattice was found in all catalysts. Fe(III)-TiO2 calcined at 500°C showed significantly higher degradation of methyl orange under visible light compared to those calcined at higher calcination temperatures. However, it showed little better performance compared to the commercial TiO2. © 2010 Taiwan Institute of Chemical Engineers.