The present paper examines the relation between different developed microstructures and the microwave electromagnetic properties in Ni-Zn-Co ferrite. To this end, the Ni0.25Zn0.25Co0.5Fe2O4composition has been prepared with the conventional ceramic process with varied prefiringTP(750°C, 1000°C) and sinteringTStop temperatures (1200°C, 1250°C). When lower temperatures are applied in these production stages, incomplete microstructures with low density, higher porosity, or finer grains are achieved. On account of these features, the contributions of domain wall motion and spin rotation to the complex permeabilityμ⁎(f)move to higher frequencies, whereas microwave dielectric permittivityε⁎(f)is decreased. In particular in conjunction with the high Co content, the wall relaxation and spin resonance are interestingly forced to occur at 850 MHz and 8.05 GHz, respectively. Regarding the electromagnetic wave attenuation, the ferrite annealed at lower temperatures exhibits strong return loss peaks at higher frequencies, but without other performance improvement. We should notice that the variations in sintering temperatureTSyield the maximum changes in the recorded parameters, including the coercive field,μ⁎(f),andε⁎(f), indicating the inferior role of prefiringTPin Ni-Zn ferrite.