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The Fe3+-doped and undoped TiO2 nanoparticles have been prepared employing sol-gel method with hydrolysis mechanism. The nanoparticles were characterized with powder X-ray diffraction and scanning electron microscopy. The experimental results showed that Fe3+-doped TiO2 possess the average particle size in the nanoscale range. The photocatalytic performance of the nanoparticles was observed for degradation of phenol in aqueous dispersion under UV light as a function of calcined temperature. The most favorable photodegradation efficiency of Fe3+-doped TiO2 occurs at 450degC.