NiAl2O4-metal composite material is an effective candidate for anodes used in industrial production of aluminium as a substitute for graphite anodes. NiAl2O4-Cu-Ni anode was prepared by spark plasma sintering in present paper. According to the density and electrical conductivity of the anodes, the optimal process parameters were given and the result showed that sintering temperature had the most significant influence on the properties of the inert anodes. Moreover, NiO was added to the inert anodes. The results showed that adding NiO will highly increase electrical conductivity of the inert anodes. SEM and optical microscope were applied to study the mechanism of the effect of NiO on the inert anodes.