Determination of oxygen in silicon materials by inert gas fusion-thermal conductivity method
SUN Haifeng, ZHOU Haishou, CHEN Caixia
General Research Institute for Nonferrous Metals Guobiao (Beijing) Testing & Certification Co., Ltd., Beijing 100088, China
摘要：采用惰性气体熔融-热导法测定硅材料中杂质氧的含量。经试验确定了仪器的最佳分析条件：称样量为0.05～0.15 g，分析功率为4 500 W，使用镍助熔剂、座坩埚；采用（30+40）s二次腐蚀方法处理助熔剂，以降低助熔剂的空白值。选择与待测试样性质类似、氧含量接近的标准物质校正仪器,氧的质量在0.01～0.30 mg之间与信号积分面积呈良好的线性，线性相关系数r=0.999 8，方法检出限为27 μg/g。对氧含量不同的硅材料试样进行测定，测定结果的相对标准偏差为1.5%～3.4%(n=11)，加标回收率为96.2%～99.2%。该方法操作简单快捷，测定结果准确。
Abstract：The impurity oxygen content in silicon material was determined by inert gas fusion-thermal conductivity method. The optimum analytical conditions were determined on the basis of test, the sample mass was 0.05-0.15 g, the analytical power was 4 500 W, and nickel flux and seat crucible were used. The two etching method(30+40) s was used to pretreat flux in order to reduce the blank value of it. The standard material correctioned instrument with similar properties and close content was chosen. The mass of oxygen was linear with area of signal in the range of 0.01-0.30 mg, the linear correlation coefficient (r) was 0.999 8. The detection limit of the method was 27 μg/g. The samples with different oxygen content were tested. The relative standard deviation of the test results was 1.5%-3.4%(n=11), and the addition recovery rate was 96.2%-99.2%. This method has the characteristics of simple operation and high accuracy.
Keywords：silicon; oxygen content; inert gas fusion-thermal conductivity method; flux; seat crucible
基金：孙海峰-，周海收，陈彩霞.惰性气体熔融－热导法测定硅材料中的氧［J］.化学分析计量，2018，27(5): 48–50. SUN H F，ZHOU H S，CHEN C X. Determination of oxygen in silicon materials by inert gas fusion thermal conductivity method ［J］. Chemical analysis and meterage，2018，27(5): 48–50.