Co-doped TiO 2 nanoparticles containing 0.0085, 0.017, 0.0255, 0.034, and 0.085 mol % Co(III) ion dopant were synthesized via sol-gel and dip-coating techniques. The effects of metal ion doping on the transformation of anatase to the rutile phase have been investigated. Several analytical tools, such as X-ray diffraction (XRD), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS), and energy dispersive X-ray analysis (EDAX) were used to investigate the nanoparticle structure, size distribution, and composition. Results obtained revealed that the rutile to anatase concentration ratio increases with increase of the cobalt dopant concentration and annealing temperature. The typical composition of Co-doped TiO 2 was Ti 1−x Co x O 2 , where x values ranged from 0.0085 to 0.085. The activation energy for the phase transformation from anatase to rutile was measured to be 229, 222, 211, and 195 kJ/mole for 0.0085, 0.017, 0.0255, and 0.034 mol % Co in TiO 2 , respectively.