湿法冶金去除太阳能级硅中硼的研究

Abstract

湿法提纯作为冶金法制备太阳能级硅的前处理工序,可以去除大部分金属和硼杂质。研究了以氢氟酸-硫酸混合酸为浸出剂,有机溶剂甲醇作为后处理剂,去除硅粉中硼杂质的方法。采用电感耦合等离子体发射光谱仪(ICP)等对产品进行表征。酸浸过程优化工艺条件:硫酸质量分数为55%,氢氟酸质量分数为7%,酸浸温度为70℃、酸浸时间为4 H、液固质量比为8∶1。酸浸后可使硅粉中的硼杂质质量分数由6.893x10-6降至3.867x10-6,去除率为41.9%。在酸浸基础上采用有机溶剂甲醇作为后处理剂,杂质硼质量分数降至3.84x10-6,去除率为44.29%。从硼酸浸后形成的产物入手探索提高硼去除率的方法,实验验证了该方法的可行性,为研究湿法冶金预处理太阳能级硅提供了新的参考。

As a pretreatment unit for preparing solargrade silicon(SG-Si) by metallurgic method,wet purification could remove most metallic impurities and nonmetallic impurities,such as boron.Experiment researched a new method to remove boron from SG-Si with mixed hydrofluoric acid-sulfuric acid as leaching agent and with organic solvent methanol as posttreatment agent.Samples were characterized by ICP and other analysis methods.When SG-Si powder had been leached at optimized conditions as follows:mass fraction of sulfuric acid was 55%,mass fraction of hydrofluoric acid was 7%,reaction temperature was 70 ℃,reaction time was 4 h,and liquid-solid mass ratio 8∶1,it was found that mass fraction of impurity boron in SG-Si was reduced to 3.867×10-6 from 6.893×10-6 and the removal rate was 41.9% after acid leaching;on the basis of the former procedure,mass fraction of impurity boron was reduced to 3.84×10-6 and the removal rate was 44.29% when treated with organic solvent.Experiment proved the feasibility of the method and provided a new reference for researching on the pretreatment of SG-Si by hydrometallurgy.