脉冲加热-红外吸收/热导法同时测定碳化硅粉末和纤维中氧和氮  

Simultaneous determination of oxygen and nitrogen in silicon carbide powder and fiber by pulse heating-infrared absorption and thermal conductivity method

作　　者：梁钪 高颂 杨峥 庞晓辉 王桂军 郑松波 LIANG Kang;GAO Song;YANG Zheng;PANG Xiaohui;WANG Guijun;ZHENG Songbo(AECC Beijing Institute of Aeronautical Materials,Beijing Key Laboratory of Aeronautical Materials Testing and Evaluation,Key Laboratory nf Scipncp and Technology on Aeronautical Materials Testing and Evaluation,Aero Engine Corporation of China,Aviation Key Laboratory of Science and Technology on Materials Testing and Evaluation,Beijing 100095)

机构地区：[1]中国航发北京航空材料研究院航空材料检测与评价北京市重点实验室中国航空发动机集团材料检测与评价重点实验室材料检测与评价航空科技重点实验室,北京100095

出　　处：《分析试验室》2021年第9期1085-1089,共5页Chinese Journal of Analysis Laboratory

摘　　要：采用脉冲加热-红外吸收、热导法,通过选择合适的助熔剂、确定分析功率和称样量,建立了同时测定碳化硅粉末和碳化硅纤维中的氧和氮含量的方法。经优化后,称取碳化硅粉末20~100 mg,碳化硅纤维7~10 mg,将粉末或纤维放入0.5 g镍囊中,加1 g镍篮后,在分析功率5.5 k W下进行测定。采用碳化硅和氮化硅标准物质测得氧和氮的校准曲线;碳化硅粉末中氧和氮检出限0.0135%和0.0018%,回收率95.8%和95.6%,相对标准偏差(RSD)均小于2%;碳化硅纤维中氧和氮检出限0.0386%和0.0051%,回收率104.2%和99.7%,RSD均小于5%。本方法同时适用于碳化硅纤维和粉末中氧和氮含量的检测。A method for the simultaneously analysis of oxygen and nitrogen content in silicon carbide powder and silicon carbide fiber was established by pulse heating-infrared absorption and thermal conductivity method,based on the optimizations of flux,analysis power and sample weight.After optimization,20-100 mg Si C powder or7-10 mg SiC fiber was put into a nickel capsule of 0.5 g,adding a nickel basket of 1 g,and determined under the analysis power of 5.5 kW.And the calibration curves for oxygen and nitrogen were performed using silicon carbide and silicon nitride reference materials.For the determination of oxygen and nitrogen in SiC powder,the detection limits were 0.0135%(O)and 0.0018%(N),the recoveries were 95.8%(O)and 95.6%(N),and the relative standard deviations were both less than 2%.For the determination of oxygen and nitrogen in SiC fiber,the detection limits were 0.0386%(O)and 0.0051%(N),the recoveries were 104.2%(O)and99.7%(N),and the relative standard deviations were both less than 5%.It is suitable for the determination of oxygen and nitrogen both in silicon carbide fiber and powder.

关 键 词：脉冲加热-红外吸收/热导法 碳化硅 粉末 纤维 氧 氮 

分 类 号：O659.21[理学—分析化学] O657.33[理学—化学]