Single-phase bulk Ti 2 AlN was prepared by spark plasma sintering (SPS) at 1200°C of Ti/Al/TiN powders in stoichiometric proportion. Investigated by X-ray diffraction (XRD) of samples and the sintering process parameter, the reaction procedure could be analyzed. Scanning electron microscopy (SEM) and electron probe micro-analysis (EPMA) coupled with energy-dispersive spectroscopy (EDS) were utilized to investigate the morphology characteristics. When sintered at 1200°C, Ti 2 AlN phase was well developed with a close and lamellated structure. The distribution of Ti 2 AlN grains was homogeneous.