A series of Er3+-TiO2, Yb3+-TiO2 and Er3+/Yb3+-TiO2 photocatalysts were obtained via sal gel method, using lanthanides precursor ranging from 0.25 to 10 mol%. The experiments demonstrated that phenol in aqueous solutions was successfully degraded under visible light (lambda > 450 nm) using Er/Yb-TiO2. The as-prepared samples were characterized by X-ray diffraction (XRD), X-ray photoelectron emission spectroscopy (XPS), UV-vis absorption measurement, BET surface area analysis and luminescent spectroscopy. XPS analysis revealed that erbium and ytterbium were present in the form of oxides. The sample showing the highest photoactivity was in the form of anatase, its surface area equalled to 125 m(2)/g, average crystals size was 13 nm, and it was prepared introducing 1 mol% of Yb3+ into reaction medium. 3 h of irradiation resulted in 89% of phenol degradation under visible light. Action spectra analysis performed for the selected Er/Yb-TiO2 samples, revealed that irradiation from 420 to 475 nm is responsible for visible light photoactivity. (C) 2014 Elsevier B.V. All rights reserved.