Mg 0.7 Zn 0.3 Fe 2 O 4 (MZF) powder was prepared by a solid-state mixed oxide using ballmilling technique. The phase identification of calcined powders was performed using X-ray diffraction technique (XRD). It has been found that MZF powders were successfully obtained for calcination conditions of 800 o C for milling times of 36 h, whereas milling times of 12 h, unreacted ZnO, Fe 2 O 3 and MgO phases (2θ ~ 54, 57 and 63) are detected from the original mixture up to 900 o C. By increasing the calcination temperature to 1000 o C, a single phase of MZF is formed. Moreover, the microstructure of powder were examined by scanning electron microscopy (SEM) and showed that the particle in size from 58-1200 nm. While, XRD patterns were obtained average size of particle, calculation by Scherrer's equation, between 30.54 -66.59 nm.
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