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 NH3 gas at room temperature followed by heat treatment under ultra-high-purity Ar, N2, 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, N2, and NH3) on the specific surface area, density, crystal structure, and composition is discussed.
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Document Type: Research Article
Department of Materials Science and Engineering, Carnegie Mellon University, Pittsburgh, Pennsylvania 15213
Department of Materials Science and Engineering and Department of Biomedical Engineering, Carnegie Mellon University, Pittsburgh, Pennsylvania 15213
Publication date: 2005-08-01