Abstract: The Dy³⁺/TiO₂ photocatalyst with different amount of Dy³⁺ doped and different calcination temperatures were synthesized by sol-gel method, and characterized by SEM, XRD, FT-IR and photocatalytic activity. The results showed that the obtained powder was anatase TiO₂. With the Dy³⁺ doped, it showed that Yb³⁺-Er³⁺ doped rare earth can refine the grain. The photocatalytic experiments of methylene blue degraded showed that the degradation rate could be 81.19% when calcined at 500 ℃, Dy³⁺/TiO₂ molar ratio of 0.2%, 1 mL H₂O₂(30%), irradiated without lighting for 6h