Ferrites Ni 0.75 Zn 0.25 Fe 2 O 4 were obtained by polymeric precursor method and calcined in a short time with microwave energy to assess the morphological and microstructural characteristics. Samples were calcined at 500, 650, 800, and 950°C for 30 min in a microwave oven. The resulting powders were characterized by thermal analysis (TG/DSC), X-ray diffraction (XRD), Fourier transform infrared spectrometer, field-emission gun scanning electron microscope (FEG-SEM), and energy-dispersive X-ray spectroscopy. The XRD results showed the formation of single ferrite phase at temperature of 500°C for 30 min. The FEG-SEM analysis showed agglomerated particles with formation of non-dense longitudinal plates, with interparticle porosity and agglomerated fine particles. The rapid calcination by microwave energy demonstrated satisfactory results in relatively low temperature of 500°C for 30 min and appeared to be a promising technique for obtaining nickel-zinc ferrite powders.