脉冲加热惰气熔融-红外/热导法测定镍基高温合金粉末中氧和氮  

Determination of oxygen and nitrogen in nickel-based superalloy powder by pulse heating inert gas fusion infrared absorption/thermal conductivity method

作　　者：陈芳 吴林飞 雷黎 CHEN Fang;WU Linfei;LEI Li(Shenzhen Wedge Central South Reasearch Institute Co.,Ltd.,Shenzhen 518000,China)

机构地区：[1]深圳市万泽中南研究院有限公司,广东深圳518000

出　　处：《冶金分析》2022年第1期71-77,共7页Metallurgical Analysis

基　　金：广东省重点领域研发计划项目(2019B010935001);国家科技重大专项(2017-Ⅵ-0009-0080);深圳市发展和改革委员会项目(SZDRC 20181000)。

摘　　要：镍基高温合金粉末中氧和氮对镍基高温合金综合性能有重要影响。采用氧氮氢联用分析仪对镍基高温合金粉末中氧、氮含量同时测定的方法进行研究。探讨分析功率、助熔剂、石墨坩埚、镍箔质量与称样量组合对测试结果的影响,推荐合适的测试条件。结果表明:分析功率为5.5 kW时,样品完全熔融,释放曲线峰形对称且无拖尾;0.2 g镍箔作为助熔剂时,熔融状态良好,且质软易封装样品;采用石墨套坩埚有利于样品均匀受热,降低熔透率,提高测试结果稳定性;考虑样品需充分熔融并确保测试结果稳定性良好,样品称样量为0.4 g左右时,采用0.2 g镍箔助熔较为合适。最终选定在5.5 kW的分析功率下采用0.2 g镍箔包裹0.4 g样品投入石墨套坩埚进行测试,氧的检出限为0.000 3%,定量限为0.001 0%;氮的检出限为0.000 15%,定量限为0.000 5%。标准样品的氧、氮含量测定值均在标准值扩展不确定度范围内,氧的相对误差小于9%,氮的相对误差小于6%。加标回收实验结果显示:氧的回收率为96%~102%,氮的回收率为95%~105%。测得3组样品中氧、氮含量的相对标准偏差(RSD,n=7)均小于7%。Oxygen and nitrogen in nickel-based superalloy powder has an important influence on the comprehensive properties of nickel-based superalloy. The method for simultaneous determination of oxygen and nitrogen in nickel-based superalloy powder was studied using an oxygen-nitrogen-hydrogen analyzer. The effect of analysis power, flux, graphite crucible, combination of nickel foil mass and sample mass on the test results was discussed. The suitable test conditions were recommended. The results showed that the sample could be completely fused when the analytical power was 5.5 kW. The peak shape of the release curve was symmetrical without tailing. As 0.2 g of nickel foil was used as a flux, the fusion state was good and it was soft to easily seal the sample. The use of duplex graphite crucible was conducive to the uniform heating of the sample, reducing the penetration rate and improving the stability of the test results. Considering that the sample should to be fully fused to ensure good stability of the test results, 0.2 g of nickel foil was used as flux for about 0.4 g of sample. Finally, 0.4 g of sample wrapped with 0.2 g of nickel foil were put into a duplex graphite crucible for testing under the analytical power of 5.5 kW. The limit of detection of oxygen was 0.000 3%, and the limit of quantification was 0.001 0%. The limit of detection of nitrogen was 0.000 15% and the limit of quantification was 0.000 5%. The measurement results of oxygen and nitrogen contents of the standard samples were all within the extended uncertainty range of the standard value. The relative error of oxygen and nitrogen was less than 9% and 6%, respectively. The recoveries of oxygen and nitrogen were 96%-102% and 95%-105%, respectively. The relative standard deviations(RSD, n=7) of the testing results of oxygen and nitrogen contents in three samples were all below 7%.

关 键 词：镍基高温合金粉末 脉冲加热 惰气熔融 红外法 热导法 氧 氮 镍箔 

分 类 号：O659.2[理学—分析化学] TF033[理学—化学]