RI 8079 Nitride Intermediates in the Preparation of Columbium, Vanadium, and Tantalum Metals (In Two Parts) 1. Nitride Preparation

The Federal Bureau of Mines has studied the reaction of oxides of columbium, vanadium, and tantalum with ammonia in vertical, gas-solids reactors at temperatures ranging from 300° to 1,300° C with the goal of preparing nitride intermediates for subsequent preparation of the metals by a thermal-decomposition step. The best nitride conversions were obtained in nonmetal reactors. With Cb205, V2O3, and V205 , low-temperature maxima in reaction rates occurred at 800°,800°, and 450° C, respectively, during oxynitride formation (in A1203) at 1 atm of pure ammonia. Conversion of the oxynitride, in a second step, to the mononitride was optimum at 1,200° C for columbium and 1,050° C for vanadium. In the case of Ta205, the rate of reaction to form Ta3N5 (in a single step) was highest at 900° C, where the presence of up to 5 percent methane was found to be beneficial; improved results were obtained by conducting the nitriding in a rotary kiln. Optimum space velocities (in the vertical Al203 reactor) ranged from 5,280 hr-1 for Cba205 to 7,950 hr-1 for V203. Oxide particle size had little effect upon reaction rates. Under fully optimized conditions, products containing less than 1 percent oxygen were readily obtained in under 6 hours.