靶用钌粉的制备  

Preparation of Ruthenium Powder as Sputtering Target Material

作　　者：章德玉[1] 雷新有[1] 张建斌[1] 

机构地区：[1]天水师范学院化学工程与技术学院,甘肃天水741001

出　　处：《过程工程学报》2015年第2期324-329,共6页The Chinese Journal of Process Engineering

摘　　要：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.Osmium was separated from ruthenium hydrochloric acid absorption by H2O2 selective oxidation and vacuum distillation in a supergravitational rotating packed bed in the first stage. Ruthenium and residual osmium were separated in the stage. And with addition of NaClO3 and H2SO4, the residual solution was further treated by oxidation and vacuum distillation in the second stage. Ruthenium tetroxide （RuO4）, which formed in the oxidation and vacuum distillation, was absorbed in a hydrochloric acid solution, and pure ruthenium hydrochloric acid absorption solution obtained. A suitable amount of I-I202 was added in the absorption solution, and the ammonium ruthenate chloride in crystalline form was obtained by crystallization and precipitation of the pure ruthenium hydrochloric acid absorption solution with ammonium chloride. The sponge ruthenium powder was prepared by calcining the resultant ruthenium salt under the optimum conditions of the calcination and reduction in hydrogen atmosphere. The sponge ruthenium powder product was washed firstly by a mixed solution of aqua regia and hydrofluoric acid, and further washed by water before drying. The high-purity ruthenium could be obtained with the purity of at least 99.999%, excluding gaseous ingredient elements, which could be used for preparing high-purity ruthenium sputtering target materials. The separation mechanism of osmium with ruthenium by selective oxidation and vacuum distillation was analyzed.

关 键 词：超重力旋转填料床 钌 锇 氧化 蒸馏 分离 

分 类 号：O658.3[理学—分析化学]