RI 9406 - Vapor-Phase Reactions To Prepare Titanium Nitride Powder

The U.S. Bureau of Mines conducted research on preparing submicrometer titanium nitride (TiN) powder as a substitute for tungsten carbide (WC) in cutting tools and wear-resistant parts. Earlier research on a small scale was expanded to include a larger reactor. The TiN powder was produced by contacting titanium tetrachloride (TiCI4) with anhydrous ammonia (NH3) in the presence of Mg at 1,100° C. The powder was collected in an electrostatic precipitator (ESP) filled with ultra-high-purity (UHP) Ar. All collected powder was thermal vacuum distilled to remove Mg and magnesium chloride (MgCl2), leaving the purified TiN. Powder handling and purification procedures were conducted to assure low oxygen content in the powder product. Oxygen content in the distilled TiN powder product was as low as 0.40 wt pct. Nitrogen averaged near 22.0 wt pet with a high of 22.4 wt pct. The purified powder product had an average median particle diameter of 0.14 µm with a standard deviation of 0.09 µm.