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In order to study the ion effect on titania phase structure, crystallite size, and photocatalytic activity, Rb+-doped TiO2 nanoparticles were prepared via a modified sol-gel method and characterized by means of X-ray diffraction, Energy Dispersive X-rays spectroscopy and transmission electron microscopy. The photocatalytic activity of the elaborated powders was studied following the degradation of methyl orange. The results indicate that doping Rb+ increases the BET surface area of TiO2 crystals, decreases the crystal size, reduces the diminishing rates of surface area with increasing calcinations temperature, raises the temperature at which anatase changes into rutile phase, and so significantly increases the photocatalytic activity of TiO2. The kinetics of the methyl orange degradation fits Langmuir-Hinshelwood kinetics model well.