A series of magnesium-doped Ni 0.65−x Mg x Zn 0.35 Fe 2 O 4 (x = 0.00, 0.04, 0.08, 0.10, 0.12, 0.16) ferrites have been synthesized using sol-gel and solid-state techniques. Sol-gel-synthesized ferrites were sintered at 1000 • C/2 h whereas solid-state-prepared ferrites were sintered at 1250 • C/2 h. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) studies confirm the spinel phase, and cation ion distribution has been estimated for both the batches using these studies. Magnetic measurements indicate the increase of saturation magnetization (M s ) up to x < 0.10 and decreases for further increase in concentration of magnesium. The Curie temperature of the samples was found to be decreasing with increase in concentration of Mg 2+ ions in both the batches.