We report on an investigation to unravel morphological and magnetic-property dependence on sintering temperature for samples of Ni 0.5 Zn 0.5 Fe 2 O 4 synthesized via mechanical alloying. The samples were sintered at various sintering temperatures from 800°C to 1000°C. The morphology of the samples was studied by means of scanning electron microscopy (SEM); hysteresis and permeability measurement were carried out using a BH hysteresisgraph system and an impedance analyzer, respectively. The morphological studies show a microstructural evolution with the increase of sintering temperature. The relationship between ordered magnetism and the microstructure of the samples show that the important grain-size threshold for the appearance of significant ordered magnetism (mainly ferromagnetism) is about ≥0.3 µm. We found that two factors sensitively influenced the samples content of ordered magnetism, their ferrite-phase crystallinity degree and the number of grains above the critical grain size.