| Summary: | In the present study, high-purity ternary-phase nitride (Ti<sub>2</sub>AlN) powders were synthesized through microwave sintering using TiH<sub>2</sub>, Al, and TiN powders as raw materials. X-ray diffraction (XRD), differential scanning calorimetry (DSC), transmission electron microscopy (TEM), and scanning electron microscopy (SEM) were adopted to characterize the as-prepared powders. It was found that the Ti<sub>2</sub>AlN powder prepared by the microwave sintering of the 1TiH<sub>2</sub>/1.15Al/1TiN mixture at 1250 °C for 30 min manifested great purity (96.68%) with uniform grain size distribution. The formation mechanism of Ti<sub>2</sub>AlN occurred in four stages. The solid-phase reaction of Ti/Al and Ti/TiN took place below the melting point of aluminum and formed Ti<sub>2</sub>Al and TiN<sub>0.5</sub> phases, which were the main intermediates in Ti<sub>2</sub>AlN formation. Therefore, the present work puts forward a favorable method for the preparation of high-purity Ti<sub>2</sub>AlN powders.
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