电子探针法测定超细铜粉中氧含量  

Determination of oxygen content in ultrafine copper powder by electron probe microanalysis

作　　者：刘英[1] 张勋高[1,2] LIU Ying;ZHANG Xungao(Centre for Analysis and Measurement,Wuhan University,Wuhan 430072,China;Centre for Analysis and Measurement,Tarim University,Alaer 843300,China)

机构地区：[1]武汉大学测试中心,湖北武汉430072 [2]塔里木大学分析测试中心,新疆阿拉尔843300

出　　处：《冶金分析》2021年第10期23-28,共6页Metallurgical Analysis

摘　　要：超细铜粉的氧化程度决定其产品性能和应用,快速、准确测定超细铜粉中O含量具有重要实际意义。实验利用自制铝质模具进行粉末压片制样,选择粒径小于10μm的CuO、Cu_(2)O和Cu粉末分别代表O含量高、中、低的超细铜粉,采用电子探针(EPMA)法对超细铜粉中的O进行定量分析。在加速电压为15kV下,考察了O和Cu元素定量分析的束流线性范围,讨论了Cu元素分析线、束流和束斑大小对O元素定量分析的影响。结果表明,Cu Kα线定量优于Lα线,束流线性范围为5~100nA,束斑以50μm为佳。在优化的测量条件下,对铜粉中高、中、低含量O测量的相对标准偏差(RSD,n=9)均不大于3.0%;O元素的检出限为0.042%;Cu_(2)O标准样品中O含量的相对误差为-4.11%;与氢损法测定值相比较,CuO和Cu粉末样品中O含量检测结果的相对误差分别为-5.95%和-7.04%。The degree of oxidation of ultrafine copper powder decides the performance and application of products.Rapid and accurate determination of O content in ultrafine copper powder has important practical significance.In experiments,the sample was prepared by pressed powder pellet method using self-made aluminum mold.The powder of CuO,Cu2 O and Cu with particle size less than 10μm was selected to represent ultrafine copper powder with high,medium,and low content of O,respectively.The content of O in ultrafine copper powder was quantitatively analyzed by electron probe microanalysis(EPMA).The linear range of beam for quantitative analysis of O and Cu was investigated when the acceleration voltage was 15 kV.The effect of analytical line of Cu,beam current,and beam spot size on the quantitative analysis of O was discussed.The results showed that Cu Kαline had better quantitative effect than Lαline.The optimal linear range of beam current and beam spot size were 5-100 nA and 50μm,respectively.Under the optimal measuring conditions,the relative standard deviations(RSD,n=9)of measurement results of high,medium,and low content of O in copper powder were all not more than 3.0%.The limit of detection of O was0.042%.The relative error of O in standard sample of Cu2 O was-4.11%.Compared to the measurement results of hydrogen loss method,the relative error of O in CuO and Cu powder samples was-5.95%and-7.04%,respectively.

关 键 词：超细铜粉 电子探针 粉末压片法 氧 定量分析 

分 类 号：O657[理学—分析化学] TF123.72[理学—化学]