固态电迁移提纯金属镨的研究  

Purification of Praseodymium by Solid State Electrotransport

作　　者：付松[1] 李宗安[1] 张志琦[1] 陈德宏[1] 苗睿瑛[1] 王志强[1] 

机构地区：[1]北京有色金属研究总院稀土材料国家工程研究中心有研稀土新材料股份有限公司,北京100088

出　　处：《稀有金属》2015年第11期1018-1023,共6页Chinese Journal of Rare Metals

基　　金：国家科技部重点基础研究发展计划(973计划)项目(2012CBA01207);国家科技部高技术研究发展计划(863计划)项目(2011AA03A409)资助

摘　　要：采用固态电迁移法对金属镨进行了提纯研究。在1×10^(-6)Pa真空环境下,分别在790,810和890℃下对工业纯电解镨进行固态电迁移处理85 h,对金属镨中主要杂质O,C,Fe,Cu,Al等元素含量进行测试,采用电感耦合等离子体质谱法(ICP-MS),辉光放电质谱法(GDMS),高频燃烧-红外法与惰气脉冲-红外热导法进行最终产品金属La的成分分析。结果表明:主要杂质O,C,Fe沿料棒向阳极迁移,Cu,Al向阴极迁移;镨的晶型转变对主要杂质O,C的迁移速率有很大影响,当电迁移温度超过镨的晶型转变点795℃,镨由dhcp结构转变为bcc结构后,表现为O,C在镨中的残余率迅速下降,且温度越高,O,C残余率越低。并以钙热还原制得金属镨为原料,经真空蒸馏提纯后,在890℃温度下进行电迁移处理216 h,在料棒阴极端区域B取样分析了78个杂质元素,金属镨纯度达到99.9929%,在国内首次制得绝对纯度高于4N的金属镨。The purification of praseodymium （Pr） metal was studied by solid state electrotransport, in which commercially pure electrolyzed Pr was electrotransported at temperatures of 790,810 and 890 ℃ for 85 h under a dynamic vacuum of 1 × 10 ^-6 Pa, respectively. The main content of impurity elements such as O, C, Fe, Cu, Al, etc. , was analyzed. The electrodeposited Pr metal was analyzed with scanning electron microscopy （SEM）, inductively coupled plasma-mass spectrometry （ICP-MS）, glow discharge-mass spectrometry （GD-MS）, high frequency combustion-infrared absorption method and inert gas fusion infrared absorption/thermal conductivity method. The results showed that main impurities O, C, Fe were anode-migrating, and meanwhile Cu, Al were cathode-migrating and the electromigration of main impurities O, C was greatly influenced by crystal transformation, namely, the residue rates of O, C in Pr decreased rapidly after the crystal structure turned to bce from dhcp at the temperature of 〉 795 ℃, and the higher temperature could lead to the lower residue rates. To get purer metal Pr, Pr was firstly reduced by Ca and then refined by vacuum distilling, and was electrotransported for 216 h at the temperature of 890℃. The analysis results showed that the purity of Pr in Zone B was up to 99. 9929% with 78 impurity elements detected. The Pr with the absolute purity of more than 4N was firstly obtained domestically.

关 键 词：镨 固态电迁移 提纯 稀土 

分 类 号：TF804[冶金工程—有色金属冶金]