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) nanocrystallites (< 10 nm) at relatively low temperatures of 400 degrees C. The nano-sized TiN crystallites were obtained by reacting liquid titanium tetrachloride dissolved in anhydrous chloroform with anhydrous NH3 gas at room temperature followed by heat treatment under ultra-high-purity Ar, N-2, and anhydrous NH3 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 NH3) on the specific surface area, density, crystal structure, and composition is discussed.