小角X射线散射法对GH4096高温合金中γ′相的尺寸分布分析  

Size distribution analysis of γ′ precipitate phase in GH4096 superalloy by small angle X-ray scattering

作　　者：卢毓华 王海舟[1,2] 李冬玲 付锐[3] 李福林 冯浩洲[1,2] LU Yuhua;WANG Haizhou;LI Dongling;FU Rui;LI Fulin;FENG Haozhou(Beijing Advanced Innovation Center for Materials Genome Engineering,Central Iron and Steel Research Institute,Beijing 100081,China;Beijing Key Laboratory of Metal Materials Characterization,NCS Testing Technology Co.,Ltd.,Beijing 100081,China;High Temperature Material Research Institute,Center Iron and Steel Research Institute,Beijing 100081,China)

机构地区：[1]钢铁研究总院北京材料基因工程高精尖创新中心,北京100081 [2]钢研纳克检测技术股份有限公司,金属材料表征北京市重点实验室,北京100081 [3]钢铁研究总院高温材料研究所,北京100081

出　　处：《冶金分析》2021年第9期1-10,共10页Metallurgical Analysis

基　　金：国家重点研发计划材料基因工程关键技术与支撑平台(2016YFB0701401)。

摘　　要：通过物理化学相分析的方式,电解提取了5种冷却速率下生产的GH4096高温合金在高温蠕变前、后的γ′析出相,并制样以后进行小角X射线散射(SAXS)分析,得到了γ′析出相的尺寸分布,辅以扫描电子显微镜(SEM)手段,比较了5种冷却速率对γ′相析出的影响以及经高温蠕变后γ′相所发生的变化。研究结果表明:不同的固溶冷却速率对γ′析出相的尺寸分布存在影响。较慢的冷却速率使得γ′析出相在较小过冷度时长大,而在较大过冷度时又大量析出,各个尺寸段的γ′析出相质量分数分布相对平均,没有含量特别高的某一段。较快的冷却速率,析出的γ′相尺寸相对较小,且尺寸较为接近。绝大部分γ′相都分布在10~96nm之间。经过高温蠕变以后,不同冷却速率下制备试样的γ′相平均尺寸和尺寸中位数不同程度地变大。经高温蠕变后,γ′析出相的尺寸分布也发生了一些变化。冷却速率相近的3个试样经过高温蠕变过程后,60~96nm尺寸范围段的γ′析出相质量分数显著大于其他段,而36~60nm尺寸范围段的γ′析出相显著减少。冷却速率最快和冷却速率最慢的试样经过高温蠕变后,200~300nm尺寸范围段的γ′析出相质量分数都较大幅度增加,但发生减少的尺寸范围段不一样。SAXS法得到的数据有统计性意义和趋势性,未来结合图像法的定量结果相互印证可以展现更好的γ′相形貌,助力材料研究。Theγ′precipitate phases in GH4096 superalloy produced at five cooling rates were extracted before and after high-temperature creep by electrolysis with the method of physicochemical phase analysis.After sample preparation,the small angle X-ray scattering(SAXS)analysis was conducted to obtain the size distribution analysis ofγ′precipitate phases.With the aid of scanning electron microscope(SEM),the effect of cooling rate on the precipitation ofγ′phases as well as the change ofγ′phases after high-temperature creep was compared.The results showed that the size distribution ofγ′precipitate phases was affected by the different solution cooling rates.γ′precipitate phases grew up under a lower degree of supercooling while nucleation burst under a higher degree of supercooling.Therfore,the mass fraction distribution ofγ′precipitated phase was relatively average in each size segment,and there was no particularly high content in a certain segment.A faster cooling rate led to a more concentrated size distribution that the size of mostγ′precipitate phases was in range of 10-96 nm.After high temperature creep,the average size and median size ofγ′phases in samples prepared at different cooling rates increased in different degrees.Meanwhile,the size distribution ofγ′precipitate phases also changed.For three samples with similar cooling rate,the mass fraction ofγ′precipitate phases with size of 60-96 nm was obviously higher than that of other segments after high temperature creep,meanwhile,theγ′precipitate phases with size of 36-60 nm decreased significantly.The mass fraction ofγ′precipitate phases with size of 200-300 nm greatly increased after high temperature creep in both samples with the fastest and slowest cooling rates.However,the size segments showing decrease was different.The data obtained in SAXS method had statistical significance and tendency.It could show better morphology ofγ′precipitate phases while combined with the quantitative results of image method in future,which wa

关 键 词：GH4096高温合金 冷却速率 γ′析出相 电解 小角X射线散射(SAXS) 尺寸分布 

分 类 号：O657[理学—分析化学] O434.1[理学—化学]