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In this work, we proposed to synthesize CuFe2O4/Fe2O3 core-shell materials with different Fe2O3 contents in order to create new and efficient photo-Fenton-like catalysts for the degradation of methylene blue with oxalic acid as a radical-producing source. The catalysts were prepared through two stages: first, CuFe2O4 was prepared by a hydroxide coprecipitation – annealing method and then, Fe2O3 was immobilized on CuFe2O4 surface by a simple impregnation – annealing procedure. According to the experimental results, our CuFe2O4/Fe2O3 core-shell materials exhibit high photo-Fenton-like catalytic activity for the degradation of methylene blue under both UVA light and visible light, as well as good ferromagnetic properties, which allows them to be easily separated from the solution by a magnet. Among them, the catalyst prepared with the molar CuFe2O4/Fe2O3 ratio of 1:2 showed the best catalytic performance with the rate constant of 2.103 h–1 under UVA light and 0.542 h–1 under visible light, which were 2 times higher than CuFe2O4 sample. The enhanced catalytic activities of our core-shell materials can be attributed to the high content of surface Fe3+ species, high specific surface area and the presence of rod-like Fe2O3 particles on their surface.