RI 8053 Electrolytic Preparation of Titanium and Zirconium Diborides From Their Oxides and Mineral Concentrates

The Bureau of Mines investigated electrolytic techniques for preparing diborides of the group IV B metals. TiB2, ZrB2, and HfB2 were electro-deposited from their respective oxides dissolved in borate-chloride-cryolite electrolytes. Titanium diboride was also electrodeposited from rutile (Ti02) dissolved in a Na2,B4O7-Na2C03-Na3A1F6-NaC1 electrolyte at 1,050° C; 14 kW-hr were required to produce 1 pound of TiB2. Major impurities in the TiB2 produced in a 10-deposition cycle experiment, in weight-percent, were Al, 0.2; Cr, 0.3; Fe, 0.1; V, 0.3; C, 1.4; and 0, 1.0. Zirconium diboride was electro-deposited from zircon (ZrSiO4) dissolved in a Na2B407-NaOH-Na3A1F6-NaCl-NaF electrolyte at 1,050° C. The ZrB2 produced in a 10-deposition cycle experiment contained the following impurities in weight-percent; Fe, 0.1; Si, 0.5; C, 0.3; and 0, 0.6. Energy required to produce 1 pound of ZrB2 was 9.3 kW-hr.