Monodispersed C, Ag co-modified TiO2 microspheres were successfully synthesized through a two-step method. Firstly, monodisperse spherical TiO2 particles were obtained via controlled hydrolysis of TBOT (tetrabutyltitanate) in ethanol. Secondly, the C, Ag co-modified TiO2 microspheres were prepared through a simple calcination process, in which the AgNO3 and citric acid was used as Ag and C source, respectively. The physical and chemical properties of C, Ag co-modified TiO2 microspheres were carefully studied by using XRD, SEM, TEM, Raman, PL spectra and UV-vis diffuse reflectance spectra (DRS), while the chemical states of C and Ag were discussed via EDS (energy dispersive spectrometer) and XPS. The photocatalytic activity of the as-prepared products was evaluated by photocatalytic decolorization of Rhodamine B (Rh B) aqueous solution at ambient temperature under UV and visible-light irradiation. The photocatalytic activity research shows that, with the cooperation of two modified materials, C, Ag co-modified TiO2 microspheres exhibit enhanced photocatalytic activity both in ultraviolet and visible-light region compared with that of pure TiO2 and single Ag modified TiO2 microspheres. (C) 2013 Elsevier B.V. All rights reserved.