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Co 0.5 Mn 0.5– x Ni x Fe 2 O 4 (0.0≤ x ≤0.3) precursor is obtained by solvothermal method at 160 °C in glycol–water. Cubic Co 0.5 Mn 0.5– x Ni x Fe 2 O 4 is obtained by calcining the precursor from 600 °C to 800 °C in air. The precursor and its calcined products are characterized by thermogravimetry and differential scanning calorimetry, X-ray powder diffraction, scanning electron microscopy, and vibrating sample magnetometer. A high-crystallized rod-like Co 0.5 Mn 0.5– x Ni x Fe 2 O 4 with a cubic structure is obtained when the precursor is calcined at 800 °C in air for 2 h. Lattice parameters decrease with the increase of Ni 2+ addition amount. The magnetic properties of Co 0.5 Mn 0.5– x Ni x Fe 2 O 4 depend on Ni 2+ doped amount and calcination temperature. Co 0.5 Mn 0.3 Ni 0.2 Fe 2 O 4 obtained at 800 °C has the highest specific saturation magnetization value, 63.51 emu/g. However, Co 0.5 Mn 0.3 Ni 0.2 Fe 2 O 4 obtained at 600 °C has the highest coercivity value, 1204.02 Oe. [ABSTRACT FROM AUTHOR]