A magnetic Fe 3 O 4 @ZnO nanocomposite (NC) was successfully synthesized by a wet milling method using a high energy milling (HEM) machine. The magnetic Fe 3 O 4 @ZnO NC was characterized by an X-ray Diffractometer (XRD), scanning and transmission electron microscopes (SEM and TEM), and a vibrating sample magnetometer (VSM @ZnO NC under UV irradiation were quantified by the degradation of a methylene blue (MB) dye solution. The result reveals that the photodegradation efficiency of Fe 3 O 4 @ZnO NC is favorable at pH neutral (pH = 7) reaching 100%. By increasing the MB dye concentration from 10 ppm to 40 ppm, the photodegradation efficiency decreases from 100% to 52%. The Fe 3 O 4 @ZnO NC can be easily collected by an external magnet. The magnetic Fe 3 O 4 @ZnO NC could be extended to various potential applications, such as purification processes, catalysis, separation, and photodegradation.