Abstract: A series of Eu³⁺ and Y³⁺ doped TiO₂ nanopowders were prepared by sol-gel method.The microstructures and properties of the samples were characterized by means of XRD,BET,SEM,UV-Vis and fluorescence spectra.It is indicated that the doping of Eu³⁺ and Y³⁺ together in TiO₂ can inhibit the phase transformation of nano TiO₂,increase the specific surface area and induce the blue shifting in the UV-Vis spectra.All the systems co-doped with Eu³⁺ and Y³⁺ show the characteristic fluorescence spectra of Eu³⁺,and the emission intensity of Eu³⁺ increases with Y³⁺ replacing Eu³⁺.The photocatalytic activities of TiO₂ nanopowders co-doped with Eu³⁺ and Y³⁺ were tested for degradation of methyl blue solutions.The results show that the doping of Eu³⁺ and Y³⁺ together,compared with the doping of Eu³⁺ or Y³⁺ respectively,can increase the photocatalytic activities of TiO₂ nanopowders and the best molar ratio of Eu³⁺∶Y³⁺ is 1∶4.