直流辉光放电质谱法测定氧化铝中的杂质元素

Impurities Concentration Detection in Oxide Aluminum by Direct Current Glow Discharge Mass Spectrometry

  • 摘要: 为了探索采用直流辉光放电质谱法(dc-GDMS)测定非导体样品中的杂质含量,建立了dc-GDMS法测定α-Al2O3粉末中杂质元素的方法。以Cu粉作为导电介质,与α-Al2O3粉末混合均匀,压片,考察辉光放电条件(放电电流、放电气体流量、离子源温度)和压片条件(两种粉末的混合比例、压片机压力等因素)对放电稳定性和灵敏度的影响,同时优化了实验条件。尝试将Al、O、Cu的总信号归一化进行计算,并用差减法计算了Al2O3粉末中的杂质含量。方法精密度在54%以内,元素检出限为0.005~0.57 μg/g。该方法的测定结果与直流电弧发射光谱法的测定结果基本吻合。

     

    Abstract: In order to investigate elemental analysis in non-conducting samples by direct current glow discharge mass spectrometry (dc-GDMS), a method for detecting impurities in α-Al2O3 powder was established. Copper powder acted as a kind of conducting host matrix, which was fully mixed with α-Al2O3 powder,and then pressed the mixture into wafers. Effect of glow discharge conditions, such as discharge current, discharge gas flow, ion source temperature, and pressure conditions, such as mixture ratio, pressure, etc. on discharge stability and sensitivity were investigated. The experiment condition was optimized. Total signal of Al, O and Cu normalization was adopted, and the impurities contents in α-Al2O3 powder were calculated in subtraction. The method precision is within 54% and the detection limits are between 0.005 μg/g and 0.57 μg/g. The results coincide with that of direct current spark atomic emission spectrometry.

     

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