摘要
通过选择合适的同位素及分辨率,提出了辉光放电质谱法(GDMS)测定超高纯铜溅射靶材中39种痕量杂质元素的分析方法。对辉光放电过程中的参数进行了优化,条件如下:放电气体流量为450 mL·min^(-1),放电电流为2.00 mA,预溅射时间为20 min。由于高纯铜的GDMS标准样品极难获得,为提高痕量杂质元素的检测准确度,在现有的标准样品条件下,利用高纯铜标准样品只获得了与基体匹配的21种杂质元素的相对灵敏度因子(RSF),其余18种杂质元素的RSF只能按照仪器自带的标准RSF进行计算。参照美国材料与试验协会的标准ASTM F1593-08(2016)的TypeⅢ中的第2种方法计算33种杂质元素的检出限,而其他6种主要杂质元素因其含量高于仪器噪声水平而无法用此法得到检出限。用GDMS对超高纯铜溅射靶材样品进行了检测,主要杂质元素为硅、磷、硫、氯、铁、银,检出量为0.015~0.082μg·g^(-1),杂质总量小于1μg·g^(-1)。除锌、碲、金的检出限在10 ng·g^(-1)级外,其余元素的检出限能够达到ng·g^(-1)级,其中钍、铀的检出限甚至达到了0.1 ng·g^(-1)级,说明方法能够满足GB/T 26017-2010中的6N(99.9999%)超高纯铜溅射靶材的检测要求。
Glow discharge mass spectrometry(GDMS) was proposed for the determination of 39 trace impurity elements in ultra-high purity copper sputtering targets by selecting appropriate isotopes and resolution. The parameters in the glow discharge process were optimized, and the conditions were as follows: the discharge gas flow rate at 450 mL·min^(-1), the discharge current of 2.00 mA, and the pre-sputtering time of 20 min. Because the GDMS standard sample of high purity copper was extremely difficult to get, in order to improve the detection accuracy of trace impurity elements, under the existing standard sample conditions, only the relative sensitivity factors(RSF) of 21 impurity elements matching the matrix were obtained by using the high purity copper standard sample, and those of the remaining 18 impurity elements could only be calculated according to standard RSF of the instrument. The detection limits of 33 impurity elements were calculated according to the second method in type III of American Society for Testing and Materials Standard ASTM F1593-08(2016), while the detection limits of the other six major impurity elements could not be obtained by this method because their contents were higher than the noise level of the instrument. The sputtering target samples of ultra-high purity copper were detected by GDMS. The main impurity elements were Si, P, S, Cl, Fe, and Ag, with the detection amounts in the range of 0.015-0.082 μg·g, and the total amount of impurities was less than 1 μg·g^(-1). The detection limits of Zn, Te, and Au were on level of 10 ng·g^(-1), while the detection limits of other elements could reach ng·glevel, and the detection limits of Th and U were even up to 0.1 ng·g^(-1)level. It was shown that the method could fulfill the detection requirements of 6 N(99.999 9%) ultra-high purity copper sputtering targets in GB/T 26017-2010.
作者
余琼
连危洁
温毅博
马兰
李明利
YU Qiong;LIAN Weijie;WEN Yibo;MA Lan;LI Mingli(Ningbo Branch of China Academy of Ordnance Science,Ningbo 315103,China;Konfoong Materials International Co.,Ltd.,Ningbo 315400,China;Zhejiang Pharmaceutical University,Ningbo 315500,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2022年第9期1049-1055,共7页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
宁波市关键核心技术应急攻关计划项目(2020G009)。
关键词
辉光放电质谱法
超高纯铜
杂质元素
相对灵敏度因子
glow discharge mass spectrometry
ultra-high purity copper
impurity element
relative sensitivity factor
