The superparamagnetic Fe 3 O 4 is synthesized by solvothermal method, in which the glycol as reducing agent and medium using FeCl 3 as the Fe sources. The superparamagnetic Fe 3 O 4 @SiO 2 was synthesized by the system which is composed by ethanol, water, ammonia and ethyl orthosilicate. The property of the Fe 3 O 4 , Fe 3 O 4 @SiO 2 and Fe 3 O 4 @SiO 2 @ZnO is characterized by XRD, TEM, Vsm and UV/vis spectrum. The TEM results indicate that spheres structure of Fe 3 O 4 and Fe 3 O 4 @SiO 2 are synthesized. These nanoparticles are detected by Vsm detection for superparamagnetic property. The inverse spinel structure of Fe 3 O 4 is polycrystalline, which is constructed by Ostwald ripening effect. The photocatalytic activity of Fe 3 O 4 @SiO 2 @ZnO was characterized by degraded methylene blue under the visible light-driven. The results show that the photocatalytic property of Fe 3 O 4 @SiO 2 @ZnO is enhanced after visible light irradiated for degrading methylene blue. The Fe 3 O 4 and Fe 3 O 4 @SiO 2 nanomaterials are recycled and reused because of the superparamagnetic property. The Fe 3 O 4 @SiO 2 @ZnO nanomaterials show high catalytic activity and excellent stability according to the decomposition of methylene blue after recycled and reused several times.