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采用超重力旋转填料床一段H2O2选择性氧化-真空蒸馏分离锇.在分离锇后的一次氯钌酸盐酸蒸馏余液中加入H2SO4和Na Cl O3,二段氧化-真空蒸馏分离钌和残留锇.氧化蒸馏出的Ru O4经盐酸吸收还原所得精制氯钌酸盐酸吸收液中加入适量H2O2,再经NH4Cl结晶沉淀得到氯钌酸铵,在氢气气氛下煅烧还原制得海绵钌.王水与HF混合煮洗、水洗干燥,所制钌粉纯度达99.999%以上,符合钌溅射靶材的原料要求.分析了锇、钌分步氧化蒸馏分离机理.
Separation of osmium by a H2O2 selective oxidation-vacuum distillation in a super gravity rotary packed bed was carried out by adding H2SO4 and NaClO3 to the primary ruthenium hydrochloric acid distillate after the separation of osmium. The second stage oxidation-vacuum distillation separated ruthenium and residual osmium Oxidatively distilled Ru O4 is absorbed and reduced by hydrochloric acid to obtain a purified hydrochloric acid ruthenic acid acid absorbing solution, adding an appropriate amount of H2O2, and then precipitating ammonium chloride ammonium ruthenate by NH4Cl to obtain a ruthenium sponge ruthenium under calcination in a hydrogen atmosphere. HF was mixed and washed and washed with water, and the purity of ruthenium powder was over 99.999%, which was in line with the raw material requirements of ruthenium sputtering targets.The separation mechanism of osmium and ruthenium by step oxidation distillation was analyzed.