A titania photocatalyst co-doped with boron and zirconium was prepared by mechanical ball milling. The resulting powder was characterized by XRD, XPS, SEM, and EDS. The photocatalytic performance of the powder was evaluated by degradation of methylene blue (MB) solution under UV illumination. XRD patterns were refined by Rietveld analysis to obtain accurate lattice parameters and positions of the atoms in the crystal structure of the photocatalyst. XRD, XPS, and Rietveld analysis results indicated that mechanical ball milling successfully weaved the dopant elements into the crystal structure and distorted the lattice of TiO2. Also, SEM micrographs confirmed that mechanical ball milling led to a decrease in average particle size of the photocatalyst. Boron and zirconium co-doped TiO2 particles exhibited a better visible light response and photocatalytic activity than those of the mono-element doped TiO2 (i.e. B-TiO2 and Zr-TiO2) and undoped TiO2 particles. The enhanced photocatalytic activity is attributed to the synergistic effects of boron zirconium co-doping and particle size reduction. (C) 2013 Elsevier Ltd and Techna Group S.r.l. All rights reserved.