Determination of impurities in silicon/carbon composite anode materials for lithium ion batteries by inductively coupled plasma atomic emission spectrometry
SUN Haifeng, SONG Yiyun, TIAN Jia, XU Qing
Guobiao (Beijing) Testing & Certification Co., Ltd., Beijing 100088, China
摘要：建立电感耦合等离子体发射光谱法测定锂离子电池硅/碳复合负极材料中杂质元素铁，镍，铝，钙的分析方法。采用高温灰化后以硝酸-氢氟酸混合酸消解样品。对比分析了不同灼烧温度对灼烧灰分消解效果和元素检测的影响。仪器工作条件：射频功率1 200 W，雾化器流量为0.75 L/min，观察高度为10 mm。4种元素的质量浓度与谱线强度呈良好的线性关系，线性相关系数均大于0.999 9。当称样质量为0.5 g时，铝，钙，铁，镍的检出限分别为0.000 18%，0.000 13%，0.000 19%，0.000 17%。测定结果的相对标准偏差为2.71%～5.34%(n=11)，各元素的加标回收率为99.6%～107.6%。该方法样品处理简单、快速，检出限低，准确度和精密度高，适合于锂离子电池硅碳负极材料中杂质的测定。
Abstract：A method for determination of impurity elements (Fe, Ni, Al, Ca) in silicon/carbon composite anode materials for lithium ion batteries by inductively coupled plasma-atomic emission spectrometry(ICP-OES) was established. The sample was decomposed by mixed nitric acid-hydrofluoric acid after high temperature ashing. The effects of different burning temperatures on ash digestion and element detection were compared and analyzed. The working conditions of the instrument were as follows: RF power was 1 200 W, atomizer flow rate was 0.75 L/min, and observation height was 10 mm. The mass concentration of the four elements and the spectral line strength had good linear relationship with the linear correlation coefficients of more than 0.999 9. When the sample mass was 0.5 g, the detection limits of Al, Ca, Fe and Ni were 0.000 18%, 0.000 13%, 0.000 19% and 0.000 17%, respectively. The relative standard deviation of the results was 2.71%-5.34%(n=11), and the recovery was 99.6%-107.6%. The method is simple, rapid with low detection limit, high accuracy and precision, which is suitable for the determination of impurities in silicon-carbon anode materials for lithium ion batteries.
Keywords：lithium-ion battery; silicon/carbon composite anode material; high temperature ashing; ICP-OES
孙海峰，宋义运，田佳，等.电感耦合等离子体发射光谱法测定锂离子电池硅/碳复合负极材料中的杂质[J].化学分析计量，2019，28(5)：37-40. SUN H F，SONG Y Y，TIAN J，et al. Determination of impurities in silicon/carbon composite anode materials for lithium ion batteries by inductively coupled plasma atomic emission spectrometry[J]. Chemical analysis and meterage，2019，28(5)：37-40.