摘要
开发一种基于黏性蒸馏-气相分离的高纯碲材料制备方法。通过调节冷凝器结构和冷凝温度,达到黏性蒸馏、控制碲优势冷凝区的目的,使挥发性差的物质留在残留物中,而硒在气相中与碲分离,实现冶金级粗碲的提纯。研究饱和蒸气压、碲分子平均自由程、不同冷凝位置的杂质分布特征以及冷凝物形貌。500 g级的实验结果表明,在5 Pa、773 K和90 min的最佳实验条件下,碲的直收率为83.40%,纯度高于99.9996%,碲优势冷凝区冷凝物中硒含量降低至2.76×10^(-4)%(质量分数)。
A method for preparing high-purity tellurium based on viscous distillation and gas-phase separation was developed.By adjusting the condenser structure and condensing temperature to achieve viscous distillation,the dominant condensation zone for tellurium was controlled;hence,poorly volatile substances remained in the crucible,while selenium was separated from tellurium in the gas phase to achieve the purification of metallurgical-grade crude tellurium.Specifically,the saturated vapor pressure,mean free path of tellurium,impurity distribution,and morphologies of the condensate at different locations were investigated in detail.The results for a 500 g upscaled experiment showed that the direct yield of Te was 83.40%,the purity of Te reached higher than 99.9996 wt.%and the selenium content in the dominant condensation zone was reduced to 2.76×10^(-4) wt.%under the optimal experimental conditions of 5 Pa,773 K and 90 min.
作者
黄大鑫
蒋文龙
徐宝强
查国正
杨斌
Da-xin HUANG;Wen-long JIANG;Bao-qiang XU;Guo-zheng ZHA;Bin YANG(National Engineering Research Center of Vacuum Metallurgy,Kunming University of Science and Technology,Kunming 650093,China;State Key Laboratory of Complex Non-ferrous Metal Resources Clean Utilization,Kunming University of Science and Technology,Kunming 650093,China;Faculty of Metallurgical and Energy Engineering,Kunming University of Science and Technology,Kunming 650093,China)
基金
the National Key R&D Program (No. 2022YFC2904900)
the National Natural Science Foundation of China (No. U1902221)
the Construction of High-level Talents of Kunming University of Science and Technology,China (No. 20210172)
the Leading Talents of Industrial Technology in Ten Thousand Talents Plan of Yunnan Province,China
the Scientist Studio of Yunnan Province,China。
关键词
高纯碲
除硒
提纯
平均自由程
优势冷凝区
high-purity tellurium
selenium removal
refinement
mean free path
dominant condensation zone