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Production of Titanium Nitride, Carbide, and Carbonitride Powders.

Davidson-CF; Shirts-MB; Harbuck-DD
U S Pat 4 812 301 1989 Mar; :
A process for producing substantially oxygen-free titanium carbide, nitride, or carbonitride in powder form comprises treating a gas phase reaction mixture of titanium halide, desirably ticl4, a reductant vapor, desirably sodium or magnesium, and a reactive gas capable of furnishing carbon, nitrogen or mixtures thereof at the reaction temperature, desirably, nitrogen, methane, or ammonia, to a temperature in the range from 500 deg to 1,250 deg c, preferably 800 deg to 1,100 deg c, whereby the titanium halide is substantially simultaneously reduced and carbided, nitrided, or carbonitrided. The process may also be practiced using volatile metal halides of metals such as zirconium, hafnium, vanadium, niobium, tantalum, and silicon for forming substantially oxygen-free carbides, nitrides, or carbonitrides thereof in powder form. Thus, magnesium vapor at 0.51 G/min was reacted with ticl4 vapor at 5.1 G/min at 1,000 deg c in a vertical stainless steel tube reactor. Argon was used as a carrier gas for the magnesium and ticl4. Nitrogen was fed into the furnace at four times the stoichiometric amount to react with titanium. The reaction products were carried through the reactor into a scrubber where they were collected in a 10-pct hcl solution. The powder mixture was then filtered and leached three times in water to remove mgcl2. The powder was identified as tin by x-ray diffraction. A similar experiment with methane at four times the stoichiometric amount instead of nitrogen gave a product identified as tic. A similar experiment with ticl4 at 3.06 G/min, sodium vapor at 0
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PAT 4,812,301
NIOSH Division
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U.S. Pat. 4,812,301, Mar. 14, 1989