惰气熔融红外吸收光谱法测定海洋钛合金用铌铝合金中氧量  

Determination of Oxygen in Niobium-Aluminum Alloy for Marine Titanium Alloy by Inert Gas Fusion Infrared Absorption Spectroscopy

作　　者：刘攀 袁晓冬[2] 陈倩倩 张庸 孟秋达 张砚博 张欣耀 LIU Pan;YUAN Xiaodong;CHEN Qianqian;ZHANG Yong;MENG Qiuda;ZHANG Yanbo;ZHANG Xinyao(National Key Laboratory for Marine Corrosion and Protection,Luoyang,Henan 471023,China;Luoyang Ship Material Research Institute,Luoyang,Henan 471023,China;Xiamen Sunrui Material Research Institute Co.,Ltd.,Xiamen,Fujian 361100,China;Liaoning Academy of Materials,Shenyang,Liaoning 110167,China;Chinalco Luoyang Copper Processing Co.,Ltd.,Luoyang,Henan 471039,China;Henan Key Laboratory of Technology and Application of Structural Materials for Ship and Marine Equipment,Luoyang,Henan 471023,China)

机构地区：[1]海洋腐蚀与防护全国重点实验室,河南洛阳471023 [2]洛阳船舶材料研究所(中国船舶集团有限公司第七二五研究所),河南洛阳471023 [3]厦门双瑞材料研究院有限公司,福建厦门361000 [4]辽宁材料实验室,沈阳110167 [5]中铝洛阳铜加工有限公司,河南洛阳471039 [6]河南省船舶及海工装备结构材料技术与应用重点实验室,河南洛阳471023

出　　处：《中国无机分析化学》2025年第5期704-712,共9页Chinese Journal of Inorganic Analytical Chemistry

基　　金：海洋腐蚀与防护全国重点实验室基金资助项目(JS240601);七二五所科技创新项目(LW150602,LW220603)。

摘　　要：铌铝中间合金是重要的钛合金用合金添加剂,具有与金属钛接近的熔点和密度,有利于降低成分偏析,提高钛合金的成分均匀性。氧含量对钛合金的性能有重要影响,是铌铝中间合金等钛合金原料的基本质量特性指标。通过探讨粉碎制样时间、分析功率、助熔剂、样品量、仪器校准等分析条件对测定结果的影响,建立了脉冲加热-惰气熔融-红外吸收光谱法测定铌铝合金中氧量的方法。实验结果表明,铌铝合金原始样品颗粒较大(大于250μm),氧量存在非常大的不均匀性,相对偏差可达80%。短时间的粉碎制样可有效提升检验结果的一致性。使用镍篮作为助熔剂时,过量镍可导致铌铝合金熔体黏稠度升高,阻碍含氧气体的生成和释放,最终采用锡囊、镍箔或镍囊作为样品分析时的助熔剂与承载容器,使用盘式振动研磨仪粉碎制样10~15 s,ONH-2000和ONH-836气体分析仪的分析功率分别设定为5.5 kW和5.0 kW,称取100~200 mg样品,采用钢铁标准样品校准仪器,结果表明,方法的定量限为0.006%~0.011%,重复性精密度(以相对标准偏差表征,n=6)为2.6%~10.4%,钢铁和钛合金标准样品中氧的测定值与证书认定值相符,钢铁有证标准样品中氧的回收率为90.5%~106%。方法适用于铌铝中间合金中氧量的准确、快速检验,并有望在以铌为合金元素的钛合金用新型多元铝基中间合金中得到推广和应用。Niobium-aluminum master alloy,an essential alloy additive,has a melting point and density comparable to titanium.This property is advantageous for minimizing component segregation and enhancing the uniformity of titanium alloys.Oxygen content,a fundamental quality characteristic of niobium-aluminum master alloys and other titanium alloy raw materials,is closely related to the performance of titanium alloys.In this work,a method for determining oxygen in niobium-aluminum master alloy was developed based on the pulse heating inert gas fusion infrared absorption technique.The impacts of various analysis conditions,including preparation time,analysis power,flux type,sample mass,and instrument calibration,on the measurement results were investigated.The large particle size of niobium-aluminum alloy raw materials,exceeding 250μm,leads to substantial inhomogeneity in oxygen content,with a relative deviation reaching up to 80%.Short-term grinding,for 10-15 s,can effectively enhance the consistency of measurement results.When nickel baskets are used as flux,an excessive amount of nickel increases the viscosity of the niobium-aluminum alloy melt,hindering the generation and release of oxygen-bearing gas species.For sample analysis,tin capsules,nickel foil,or nickel capsules are recommended as flux and containment vessels.The optimal analysis conditions are as follows:a sample grinding time of 10-15 s,analytical power of the ONH-2000 and ONH-836 gas analyzers set to 5.5 kW and 5.0 kW respectively,and a sample mass of 100-200 mg.The calibration coefficient is established using steel certified reference materials.The method has a quantification limit of 0.006%-0.011%.When applied to the analysis of actual niobium-aluminum alloy samples,the repeatability precisions(expressed as relative standard deviations,n=6)range from 2.6%to 10.4%.The measured values of steel and titanium certified reference materials are in good agreement with the certified values.The recoveries of oxygen in steel certified reference materials are between

关 键 词：惰气熔融 红外吸收光谱 铌铝 氧 铝基中间合金 海洋钛合金 

分 类 号：O657.33[理学—分析化学] TG115.33[理学—化学]