第32卷第3期 2017年3月
文章编号：1000-324X(2017)03-0281-06
无机材料学报 Journal of Inorganic Materials
Vol. 32 No. 3 Mar.,2017
DOI: 10.15541/jim20160324
冶金法制备太阳能级多晶硅的耦合除杂研究
李鹏廷1,2，王凯1,2，姜大川1,2，任世强1,2，谭毅1,2，安广野3，
张磊，郭校亮，王峰3
(1.大连理工大学材料科学与工程学院，大连116024;2.大连理工大学辽宁省太阳能光伏系统重点实验室，大连116024; 3.大工(青岛)新能源材料技术研究院有限公司，青岛266200)
摘要：以工业硅为原料，利用介质熔炼、定向凝固和电子束熔炼三种熔体处理技术对工业硅中的B、P和金属杂质进行了去除，制备出了99.9999%级多晶硅材料，其中，杂质B和P的含量分别低于0.20ppmw（partspermillion(weight)，百万分之一质量），金属杂质总含量（TM）低于0.23ppmw。研究发现，介质熔炼去除杂质B的过程中，熔体中发生氧化还原反应可以有效去除大部分的杂质AI和Ca：电子束熔炼过程中，利用饱和蒸气压原理可以有效去除挥发性杂质P、AI、Ca，同时降束诱导多晶硅定向凝固，可将其他金属杂质进一步去除。本研究通过各技
术间的耦合除杂，减少了冶金法提纯多晶硅的工序，为连续化、规模化生产提供了技术支撑。关键词：工业硅；介质熔炼；定向凝同；电子束熔炼
中图分类号：TF89
文献标识码：A
Couplingof MetallurgicalMethodtoRemoveImpuritiesinSolarGrade
Polycrystalline Silicon
LI Peng-Ting'-2, WANG Kai'-2, JIANG Da-Chuan'2, REN Shi-Qiang'2, TAN-Yi'-2, AN Guang-Ye,
ZHANG Leis, GUO Xiao-Liang', WANG Feng
(1. School of Materials Science and Engineering, Dalian University of Technology, Dalian 116024, China; 2. Key Laboratory for Solar Energy Photovoltaic System of Liaoning Province, Dalian 116024, China; 3. New Energy Materials and Technology Institute Co. Ltd. of Dalian University of Technology (Qingdao), Qingdao 266200, China)
Abstract: Preparation of 6N grade polycrystalline silicon materials using raw materials of industrial silicon was explored by medium melting, directional solidification and electron beam melting. The contents of impurities B and P in the samples are both lower than 0.20 ppmw, while the total content of metal impurity (TM) is less than 0.23 ppmw. Dur-ing the process of removing B by medium melting, a large proportion of Al and Ca is simultaneously removed through the redox reaction, During the process of electron beam melting, volatile impurities including P, Al and Ca are fur-ther effectively removed by using saturated vapor pressure. Meanwhile, other metal impurities are removed by de-creasing beam power, which induces the occurrence of directional solidification. Coupling of metallurgical methods reduces the purification process of polycrystalline silicon, and provides the technical support for continuous and large-scale production
Key words: industrial silicon; medium melting; directional solidification; electron beam melting 收稿日期：2016-05-17；收到修改稿日期：2016-07-05
基金项目：国家自然科学基金(51404053)；中国博士后科学基金(2014M551076)
National Natural Science Foundation of China (51404053); China Postdoctoral Science Foundation (2014M551076)
作者简介：李鹏廷（1986)，男，博士，E-mail:ptli@dlut.edu.cn 通讯作者：谭毅，教投.E-mail:tanyi@dlut.edu.cn
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