Preparation of Zirconium Powder Through ZrCl4 Bubbling in Mg-MgCl2 Bath

Abstract

An alternative process has been studied for zirconium production through chemical reaction between ZrCl4 bubbles and magnesium melt floating on molten MgCl2 salt. The preparation of pure zirconium in the form of powder was successfully accomplished by cleaning process consisting of washing with distilled water and pickling with hydrochloric acid solution. The purity of zirconium powder increased with dense concentration of hydrochloric acid solution and longer pickling time by removing residual magnesium, MgCl2 and other impurities except for zirconium. The sufficiently high level of purity was achieved by pickling for 6 hours using 3 mass% of hydrochloric acid solution. It was noteworthy that purity of zirconium powder was deteriorated with the formation of intermetallic compounds when alumina or iron was used for apparatus material. Meanwhile, a sound quality without any intermetallic compound and high purity were achieved when MgO material was used. It was found that there were no significant differences in purity and morphology of zirconium powder depending on reaction temperature. However, mean particle size was increased by increasing reaction temperature.