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In this paper，ZnFeZ OQ and Zn0/ZnFeZ OQ were synthesized by precipitation method. The structure and appearance of the synthesized nanoparticles were characterized by XRD and SEM. The results show that ZnFeZ OQ and Zn0/ZnFeZ OQ can be successfully prepared by XRD;we can find that the ZnFeZ04 is irregular, and the Zn0/ZnFeZ OQ is the ball type and the small particles are attached. A study on the photocatalytic performance of the simulated wastewater(Methylene blue)with Zn0/ZnFeZ OQ under the simulated sunlight showed that the highest degradation rate could reach to 89.2%.