Ni0.5Co0.5Fe₂O₄ (NCF) powders were obtained employing two alternative synthesis routes: solid-state reaction and Pechini’s methods. The ceramic powders were pressed and sintered in the temperature range of 1100∘C to 1250∘C. Microstructural and structural properties were evaluated by SEM, XRD, and Raman spectroscopy. Magnetic hysteresis loops of sintered samples were also recorded. A secondary phase was observed in samples synthesized by Pechini’s method, whereas samples obtained by the solid-state reaction method, with the mechanochemical activation of the reagents, only produced the spinel structure. Magnetic properties of samples obtained by the solid-state method displayed higher magnetic saturations and lower coercive fields than those obtained from the Pechini’s method.Ni0.5Co0.5Fe₂O₄ (NCF) powders were obtained employing two alternative synthesis routes: solid-state reaction and Pechini’s methods. The ceramic powders were pressed and sintered in the temperature range of 1100∘C to 1250∘C. Microstructural and structural properties were evaluated by SEM, XRD, and Raman spectroscopy. Magnetic hysteresis loops of sintered samples were also recorded. A secondary phase was observed in samples synthesized by Pechini’s method, whereas samples obtained by the solid-state reaction method, with the mechanochemical activation of the reagents, only produced the spinel structure. Magnetic properties of samples obtained by the solid-state method displayed higher magnetic saturations and lower coercive fields than those obtained from the Pechini’s method.