Ni 0.6 Zn 0.4 Fe 2 O 4 prepared using solid state reaction and sol-gel methods were compared for their structural and magnetic properties. Due to the much higher annealing temperature used in solid state reaction, the crystalline size was much larger than that of the nanoparticles prepared by sol-gel. The saturation magnetization of sol-gel nanoparticles was higher, and the coercivity was about 2 times larger, compared to the solid state reaction sample. By analyzing the integration intensity of x-ray diffraction peaks (220) and (222), we proposed that the difference in the saturation magnetization might be due to the inversion of cation distribution caused by the different preparation techniques used.