Spinel nickel aluminate is an important industrial material, has been synthesized by a solid state reaction method from nano powders ?- Al2O3 and NiO represented as a theoretical batch. Sintering the raw materials was done at rate heating 4 OC/min in 1500 OC. The sintered specimens were investigated employing by X-ray diffraction (XRD), Energy-dispersive X-ray spectroscopy (EDS) and scanning electron microscopy techniques (SEM). It is that the formation nickel aluminate spinel was completed in 1500 oC, at the following percent (20 wt % NiO and 30wt% NiO and 50 wt% NiO), thermal properties have been also investigated for sintered specimens. The new composite materials it high thermal expansion stability and resistant to thermal shock at 1200oC, especially with 30 wt % NiO.