Spinel type metal aluminates, MAl2O4 (M = Ni, Co, Zn, Mg, Ca, Sr), have potential applications in different fields e.g. anodes for solid oxide fuel cells for their immobilized characteristics. NiAl2O4, a spinel type material, was successfully synthesized by standard solid-state reaction method and characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and thermogravimetric analysis (TGA). Rietveld analysis using Fullprof software shows that the crystallographic phase is cubic in space group Fd-3m with cell parameter a = 8.03990(5) Å. The refinement converged in a very good goodness-of-fit, χ2 = 0.991. Microstructural study shows a porous structure suitable for electrode materials. TGA shows a slight weight loss in the range room temperature to 440 °C (about 0.022 wt%) the loss of water molecules from the structure. Above 440 °C the weight gradually increases until 900 °C (about 0.052 wt%) which is mainly related to the fill-up of oxygen vacancies in the unit cell and change in valence states of transition metals. [ABSTRACT FROM AUTHOR]