Developing new semiconductor materials with improved photocatalytic activity is a promising technology for the remedy of environmental pollution. Here we report on the synthesis of Yb containing TiO2 nanoparticles and their catalytic activity under visible light. Highly monodispersed, spherical TiO2 and TiO2 :Yb nanoparticles of 27- 40 nm size range were prepared through controlled hydrolysis of titanium tetrabutoxide (TTB) and characterized by X-ray diffraction (XRD), energy dispersion spectroscopy (EDS), high-resolution transmission electron microscopy (HRTEM), high angle annular dark field (HAADF), and ultraviolet-visible diffuse reflectance spectroscopy (UV-vis DRS) techniques. Average size of the nanoparticles was found to decrease with the increase of Yb doping concentration. The photocatalytic activity of Yb doped TiO2 was evaluated by measuring the degradation rates of methylene blue (MB) under UV and visible lights. Doping with ytterbium ions enhanced significantly the photocatalytic activity of TiO2 nanoparticles for MB oxidation under visible light.