脉冲熔融-红外/热导法测定钛合金粉末微注射成形脱脂坯中氧氮氢

Determination of Oxygen,Nitrogen and Hydrogen in Micro InjectionMolding of Titanium Alloy Powder about Degrease Billets by ImpulseFusion-Infrared Absorption and Thermal Conductivity Method

准确测定钛合金粉末微注射成形脱脂坯中氧氮氢含量对钛合金的粉末微注射工艺改进有很大指导作用。采用工业镍板经过表面打磨、酸洗、加工成固定质量的镍粒来代替市售的镍助熔剂,通过自制镍粒预先加入设备预脱气减少空白影响的方式建立了脉冲熔融-红外/热导法测定钛合金粉末微注射成形的脱脂坯中氧氮氢含量的方法。实验表明,镍粒助熔剂与石墨坩埚经二次脱气,可确保镍粒助熔剂的空白降至极低值以代替市售的镍篮、镍屑等助熔剂。钛合金粉末微注射成形脱脂坯采用振动磨形式加工至0.178 mm以下,镍粒的加入量为1.5 g,分析功率为5 300 W时,可以获得稳定准确的结果。采用实验方法对脱脂坯实际样品进行测定,其相对标准偏差(RSD,n=6)分别为0.080%~0.47%、0.28%~1.3%和1.6%~2.0%;采用加入钛合金标准样品进行加标回收实验,氧氮氢加标回收率分别在95.7%~104%、97.8%~100%及96.6%~103%。方法满足脱脂坯中的氧氮氢快速检测要求的同时,极大地降低了分析成本。

Accurate determination of oxygen,nitrogen and hydrogen content of titanium alloy powder can greatly guide the improvement of powder microinjection process of titanium alloy.Using industrial nickel plate after surface grinding,pickling,processing into a fixed quality of nickel particles to replace commercial nickel flux,by homemade nickel particles added in advance to reduce the impact of the pulse melting-infrared/thermal conductivity,the method of determination,titanium alloy powder micro injection molding of oxygen and nitrogen hydrogen content method.The test shows that nickel particle flux and graphite crucible after secondary degassing,can ensure that the blank of nickel particle flux drop extremely low value,instead of the market sold nickel basket,nickel chips and other flux.The titanium alloy powder is processed by vibration grinding to less than 80 mm,the amount of nickel particles is 1.5 g,and the analytical power is 5300 W,the stable and accurate results can be obtained.The recovery test of relative standard deviation(RSD,n=6)is 0.080%—0.047%,0.28%—1.3%and 1.6%—2.0%with titanium alloy is from 95.7%—104%,97.8%—100%and 96.6%—103%.The method meets the requirement of rapid detection and hydrogen and greatly reduces the analysis cost.