In order to improve deficiencies of NiFe2O4 spinel used as matrix of inert anode in aluminium electrolysis, NiFe2O4/SiCp were prepared by the solid state reaction for the first time. Microstructural changes were observed by scanning electronic microscope and phase was determined with X-ray detector. Effect of sintering temperature and times on density, porosity and microstructure were researched, and the reasons that caused the difference were discussed deeply. At the same time the thermodynamical compatibility of NiFe2O4 and SiC was proved under 1200℃ by DTA.The results showed that the microstructure was more homogeneous when the sintering temperature reached 1 180℃and the density attained their maximum about 6 h sintering. The appropriate sintering technique of NiFe2 O4/SiCw composite materials was 1180℃× 6 h.