Microwave dielectric ceramics have great potential applications in the fields of modern communication technology. However, the effects of processing of solid reaction on the crystal structure and properties of NiZrNb2O8 has not been reported. In this paper, the NiZrNb2O8 ceramic was prepared using different raw materials. The solid state reaction process, crystal structure, and dielectric properties of the NiZrNb2O8 ceramics were investigated. The X-ray diffractometer (XRD) results showed that the solid state reaction of NiZrNb2O8 could be divided into two steps using NiO, ZrO2 and Nb2O6 as raw materials. Scanning electron microscope (SEM) analysis results showed that the surface of NiZrNb2O8 prepared from NiNb2O6 and ZrO2 was more compact. The optimal density of the samples reached 99.28% of the theoretical value. And the dielectric constant (εr), quality factor (Q×f), temperature coefficient of resonant (τf) reached 23.6, 37237 GHz, -7.796 ppm/°C, respectively.