电感耦合等离子体原子发射光谱法测定太阳能级硅中硼

Determination of boron in solar grade silicon by inductively coupled plasma atomic emission spectrometry

研究了用电感耦合等离子体原子发射光谱仪(ICP-AES)测定太阳能级硅(SOG-Si)中硼的方法。试验发现,在110℃左右的温度下,用氢氟酸和硝酸的混合溶液作溶剂,试样在PFA烧杯中能较快溶解,且在溶样时添加0.3mL甘露醇,可有效抑制硼的损失。在1000级洁净室中,用金属氧化物半导体(MOS)级试剂溶解电子级硅(EG-Si),可控制样品空白中硼元素含量小于1μg/L,并能抑制部分基体效应。在仪器最佳工作状态下,选取B 182.641nm作为分析谱线,方法的检出限为18.10μg/L,回收率在92%~108%之间,相对标准偏差(RSD,n=11)不大于7.2%。样品中硼的测定结果与电感耦合等离子体质谱(ICP-MS)法及辉光放电质谱(GDMS)法进行了比对,结果吻合。

The trace boron in solar grade silicon(SOG-Si)was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).The silicon sample was dissolved in mixed solution of nitric acid and hydrofluoric acid under heating in PFA container at about 110 ℃,and 0.3mL of mannitol was added to protect boron.Electronic grade silicon(EG-Si)was dissolved by reagent of metal oxide semiconductor(MOS)level in class 1000 clean room,so the boron in sample blank was less than1μg/L and the silicon matrix effect can be partly inhibited.Under the optimal condition of instrument,the detection limit of method was 18.10μg/L and the recovery was 92%-108% with the relative standard deviation(RSD)not more than 7.2%(n=11)at the spectra line of B 182.641 nm.The found results were consistent with those of inductively coupled plasma mass spectrometry(ICP-MS)and glow discharge mass spectrometry(GDMS).