惰气熔融–红外吸收/热导法同时测定氮化硅中的低氧高氮  

Simultaneous and Accurate Determination of Low Oxygen and High Nitrogen in Silicon Nitride by the Inert Gas Melting-Infrared Absorption/Thermal Conductivity Method

作　　者：王琳[1] 王楠[1] 任士远 张彬彬[1] WANG Lin;WANG Nan;REN Shiyuan;ZHANG Binbin(Analysis and Measurement Centre,Northeastern University,Shenyang 110819,China)

机构地区：[1]东北大学分析测试中心,沈阳110819

出　　处：《中国陶瓷》2025年第1期20-25,共6页China Ceramics

基　　金：国家重点研发计划项目(No.2017YFB0310300)。

摘　　要：氮化硅是性能优异的陶瓷材料,在航空航天、国防军工等方面有着重要的作用。氮化硅中的杂质元素氧与主元素氮对其制备工艺及高纯化发展至关重要。通过对称样量、脱气功率、分析功率、氧的开始基线时间、助熔剂种类及比例、坩埚选择等因素的探究,建立了惰气熔融–红外吸收/热导法同时测定氮化硅中的低氧高氮,并通过标准物质验证了方法的准确性、精密度与回收率。结果表明,当称样量为0.0700 g、脱气功率为5000 W、分析功率为5500 W、氧的开始基线时间为1 s、助熔剂为0.60 g镍囊、坩埚为石墨套坩埚时,可以得到稳定、准确的测试结果。以此实验条件使用标准物质建立了标准曲线,并进行了加标回收实验和精密度实验,氧、氮标准曲线线性相关系数分别为0.999922、0.999990,加标回收率为96.9%~102.7%,88.2%~97.7%,氧的RSD(n=7)分别为1.99%、0.45%、氮的RSD(n=7)分别为0.63%、0.79%。方法的检出限分别为0.000306%、0.00864%,定量限为0.000102%、0.00881%。该方法可用于快速、准确、同时检测氮化硅中的低氧高氮。Silicon nitride is a ceramic material with excellent performance,which plays an important role in aerospace,national defense,the military industry,etc.The impurity element oxygen and the main element nitrogen of silicon nitride are crucial to the development of its preparation process and high purification.In this paper,the factors such as sample weight,degassing power,analytical power,the beginning time of the baseline of oxygen,the type and proportion of flux,the selection of crucible were investigated.A method for simultaneous determination of low oxygen and high nitrogen in silicon nitride by the inert gas melting-infrared absorption/thermal conductivity method was established,and the accuracy,precision and recovery of the method were verified by standard materials.The results showed that the sample weight was 0.0700 g,degassing power was 5000 W,analysis power was 5500W,the flux was 0.60 g nickel,the beginning time of the baseline of oxygen was 1 s and a graphite sleeve was used.The correlation coefficients were 0.999922 and 0.999990,respectively.The limits of detection were 0.000306%and 0.00864%,and the limits of quantification were 0.000102% and 0.00881%.The RSD(n=7)of oxygen was 1.99%and 0.45%,respectively,and RSD(n=7)of nitrogen was 0.63% and 0.79%,respectively.The recoveries of oxygen were from 96.9% to 102.7%,and those of nitrogen were from 88.2% to 97.7%.The method can be used for rapid,accurate and simultaneous detection of low oxygen and high nitrogen in silicon nitride.

关 键 词：氮化硅 氧 氮 惰气熔融–红外吸收/热导法 

分 类 号：TQ174.75[化学工程—陶瓷工业]