In this study, nanocrystalline ferrite powders with the composition Ni0.5Zn0.5Fe2O4 were prepared by the autocombustion method. The obtained powders were sintered at 800^oC, 900^oC and 1,000^oC for 4 h in air
atmosphere. The as-prepared and the sintered powders were characterized by X-ray diffraction (XRD),
Fourier transform infrared (FT-IR) spectroscopy, and magnetization studies. An increase in the crystallite size and a slight decrease in the lattice constant with sintering temperature were observed, whereas microstrain was observed to be negative for all the samples. Two significant absorption bands in the wave number range of the 400 cm⁻¹ to 600 cm⁻¹ have been observed in the FT-IR spectra for all samples which is the distinctive feature of the spinel ferrites. The force constants were found to vary with sintering temperature, suggesting a cation redistribution and modification in the unit cell of the spinel. The M-H loops indicate smaller coercivity, which is the typical nature of the soft ferrites. The observed variation in the saturation magnetization and coercivity with sintering temperature has been attributed to the role of surface, inhomogeneous cation distribution, and increase in the crystallite size.