Synthesis of Nanostructured TiN Using a Two‐Step Transition Metal Halide Approach

A two‐step transition metal halide approach has been developed for synthesizing uniform ultra‐fine titanium nitride (TiN) nano‐crystallites (<10 nm) at relatively low temperatures of 400°C. The nano‐sized TiN crystallites were obtained by reacting liquid titanium tetrachloride dissolved in anhydrous chloroform with anhydrous NH 3 gas at room temperature followed by heat treatment under ultra‐high‐purity Ar, N 2 , and anhydrous NH 3 atmosphere. The synthesized TiN nano‐crystallites were characterized by X‐ray diffraction, Brunauer–Emmett–Teller, pycnometer, differential thermal analysis/thermo‐gravimetric analysis, and high‐resolution transmission electron microscopy. The effect of the heat treatment temperature and atmosphere (Ar, N 2 , and NH 3 ) on the specific surface area, density, crystal structure, and composition is discussed.