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In this study, nanocrystalline Ni 0?64 Zn 0?36 Fe 2 O 4 powders were prepared using a planetary ball mill. The evolution of the microstructure and magnetic properties during the milling were studied by Xray diffraction technique, scanning electron microscopy, transmission electron microscopy and vibrating sample magnetometre. It is revealed from the results of the phase analysis that nanocrystalline Ni 0?64 Zn 0?36 Fe 2 O 4 ferrite with average crystallite size of 6?18 nm and non-uniform lattice strain of 0?33% has been formed after 60 h of milling time. A progressive increase of saturation magnetisation and a dramatic decrease in coercivity were also observed with increasing milling time.