Size distribution analysis of γ' precipitate phase in GH4096 superalloy by small angle X-ray scattering
LU Yuhua1,2, WANG Haizhou*1,2, LI Dongling1,2, FU Rui3, LI Fulin3, FENG Haozhou1,2
1. Beijing Advanced Innovation Center for Materials Genome Engineering, Central Iron and Steel Research Institute, Beijing 100081, China; 2. Beijing Key Laboratory of Metal Materials Characterization, NCS Testing Technology Co., Ltd., Beijing 100081, China; 3. High Temperature Material Research Institute, Center Iron and Steel Research Institute, Beijing 100081, China
Abstract：The γ' 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 of γ' precipitate phases. With the aid of scanning electron microscope (SEM), the effect of cooling rate on the precipitation of γ' phases as well as the change of γ' phases after high-temperature creep was compared. The results showed that the size distribution of γ' 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 of γ' 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 most γ' precipitate phases was in range of 10-96 nm. After high temperature creep, the average size and median size of γ' phases in samples prepared at different cooling rates increased in different degrees. Meanwhile, the size distribution of γ' precipitate phases also changed. For three samples with similar cooling rate, the mass fraction of γ' precipitate phases with size of 60-96 nm was obviously higher than that of other segments after high temperature creep, meanwhile, the γ' precipitate phases with size of 36-60 nm decreased significantly. The mass fraction of γ' 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 of γ' precipitate phases while combined with the quantitative results of image method in future, which was helpful for material researches.
卢毓华, 王海舟, 李冬玲, 付锐, 李福林, 冯浩洲. 小角X射线散射法对GH4096高温合金中γ'相的尺寸分布分析[J]. 冶金分析, 2021, 41(9): 1-10.
LU Yuhua, WANG Haizhou, LI Dongling, FU Rui, LI Fulin, FENG Haozhou. Size distribution analysis of γ' precipitate phase in GH4096 superalloy by small angle X-ray scattering. , 2021, 41(9): 1-10.
[1] Reed C Reed. The superalloys fundamentals and applications[M].London:Cambridge University Press,2006. [2] 黄乾尧,李汉康.高温合金[M].北京:冶金工业出版社,2000. [3] Aude Laurence,Jonathan Cormier,Patrick Villechaise,et al.Impact of the solution cooling rate and of thermal aging on the creep properties of the new cast&wrought Rene65 Ni-based superalloy[C]//8th International Symposium on Superalloy 718 and Derivatives.Pittsburgh:TMS (The Minerals, Metals & Materials Society), 2014: 297-312. [4] Devaux A,Helstroffer A,Cormier J,et al.Effect of aging heat-treatment on mechanical properties of AD730TM superalloy[C]//8th International Symposium on Superalloy 718 and Derivatives.Pittsburgh:TMS (The Minerals, Metals & Materials Society),2014:485-499. [5] TIAN Sugui,XIE Jun,ZHOU Xiaoming,et al.Microstructure and creep behavior of FGH95 nickel-base superalloy[J].Materials Science and Engineering A,2011(528):2076-2084. [6] Mignanelli P M,Jones N G,Hardy M C,et al.The effect of composition on the gamma prime distribution of Ni-Cr-Al-Nb alloys[C]//8th International Symposium on Superalloy 718 and Derivatives.Pittsburgh:TMS (The Minerals, Metals & Materials Society),2014:527-536. [7] FENG Yefei,ZHOU Xiaoming,ZOU Jinwen,et al.Effect of cooling rate during quenching on the microstructure and creep property of nickel-based superalloy FGH96[J].International Journal of Minerals,Metallurgy and Materials,2019,26(4):493-499. [8] Smith T M,Bonacuse P,Sosa J,et al.A quantifiable and automated volume fraction characterization technique for secondary and tertiary γ' precipitates in Ni-based superalloys[J].Materials Characterization,2018,140: 86-94. [9] 江和甫.对涡轮盘材料的需求及展望[J].燃气涡轮试验与研究, 2002,15(4):1-6. JIANG Hefu.Requirements and forecast of turbine disk materials[J].Gas Turbine Experiment and Research,2002,15(4):1-6. [10] Y Pico,V Andreu.12-Nanosensors and other techniques for detecting nanoparticles in the environment[M].Nanosensors for Chemical and Biological Applications,2014:295-338. [11] Yokoyama T,Masuda H,Suzuki M,et al.Chapter 1.Basic properties and measuring methods of nanoparticles[M].2nd edition.Nanoparticle Technology Handbook,2012:3,5-48. [12] XIANG Yingwei,ZHANG Jinyuan,LIU Chunlan.Verification for particle size distribution of ultrafine powders by the SAXS Method[J].Materials Characterization,2000,44(4-5):435-439. [13] Goertz V,Dingenouts N,Nirschl H.Comparison of nanometric particle size distributions as determined by SAXS, TEM and analytical ultracentrifuge[J].Particle & Particle Systems Characterization,2009,26:17-24. [14] 王辉,曾美琴. X射线小角散射法测量纳米粉末的粒度分布[J].粉末冶金技术,2004(1):7-11. WANG Hui,ZENG Meiqin.Determination of particle size distribution of nanometer-sized powder by small angle X-ray scattering method[J].Powder Metallurgy Technology,2004(1):7-11. [15] 冶金工业部钢铁研究总院.钢和铁,镍基合金的物理化学相分析[M].上海:上海科学技术出版社,1981. [16] 李冬玲,乔雪璎,刘庆斌,等.GH4199镍基高温合金的析出相分析研究[J].冶金分析,2005,25(1):1-6. LI Dongling,QIAO Xueying,LIU Qingbin,et al.The analysis of the precipitate phase in Ni-base wrought superalloy GH4199[J].Metallurgical Analysis,2005,25(1):1-6. [17] 刘庆斌,卢翠芬,燕平.一种定向凝固镍基铸造高温合金的物理化学相分析[J].冶金分析,2006,26(2):9-13. LIU Qingbin,LU Cuifen,YAN Ping.Physicochemical phase analysis of a directionally solidified Ni-based cast superalloy[J].Metallurgical Analysis,2006,26(2):9-13. [18] 李冬玲,刘志勇,李杰,等.建筑用H型耐火钢中析出相的状态分析[J].冶金分析,2009,29(7):1-6. LI Dongling,LIU Zhiyong,LI Jie,et al.State analysis of precipitates in fire-resistant H-beam steels[J].Metallurgical Analysis,2009,29(7):1-6. [19] 李玲霞,赵晓丽,李南,等.一种高铬的铁镍基高温合金物理化学相分析[J].冶金分析,2015,35(2):6-11. LI Lingxia,ZHAO Xiaoli,LI Nan,et al.Physicochemical phase analysis of iron-nickel based high temperature alloy with high chromium[J].Metallurgical Analysis,2015,35(2):6-11. [20] 付锐,冯涤,陈希春,等.电渣重熔连续定向凝固技术研究[J].钢铁研究学报,2011,23(s2):1-4. FU Rui,FENG Di,CHEN Xichun,et al.Research of ESR-CDS technology[J].Journal of Iron and Steel Research,2011,23(s2):1-4. [21] 付锐,陈希春,任昊,等.电渣重熔连续定向凝固Rene88DT合金的组织与热变形行为[J].航空材料学报, 2016,31(3):8-13. FU Rui,CHEN Xichun,REN Hao,et al.Structure and hot deformation behavior of ESR-CDS Rene88DT[J].Journal of Aeronautical Materials,2016,31(3):8-13. [22] 陈希春,付锐,冯涤,等.电渣重熔连续定向凝固René88DT镍基合金锭工艺参数的计算[J].特殊钢,2011,32(5):31-34. CHEN Xichun,FU Rui,FENG Di,et al.Calculation on technological parameters of electroslag remelting continuous-directionally solidified René88DT nickel alloy ingot[J].Special Steel,2011,32(5):31-34. [23] 陈希春,任昊,付锐,等.电渣重熔高温合金凝固组织控制的研究进展[J].特钢技术,2011,17(3):1-4,31. CHEN Xichun,REN Hao,FU Rui,et al.Recent development of solidified structure controlling of superalloy during ESR Process[J].Special Steel Technology,2011,17(3):1-4,31. [24] 李福林,付锐,冯涤,等.镍基变形高温合金CDS&W FGH96 热变形行为研究[J].稀有金属,2015,39(3):201-206. LI Fulin,FU Rui,FENG Di,et al.Hot deformation characteristics of Ni-base wrought superalloy CDS&W FGH96[J].Chinese Journal of Rare Metals,2015,39(3):201-206. [25] 石宇野,焦少阳,董建新,等.镍基高温合金γ'相析出的经典动态模型及应用[J].金属学报,2012,48(6):661-670. SHI Yuye,JIAO Shaoyang,DONG Jianxin,et al.Classical precipitation dynamic model of γ' phase of nickel-based super alloys and applications[J].Acta Metallurgica Sinica,2012,48(6):661-670. [26] Baldan A.Review progress in Ostwald ripening theories and their applications to nickel-base superalloys Part I: Ostwald ripening theories[J].Journal of Materials Science,2002,37:2171-2202. [27] ZHOU Yu,ZHANG Zheng,ZHAO Zihua,et al.Morphological evolution of γ' precipitates in a nickel-based superalloy during various solution treatments[J].Rare Metal,2012(3):221-226.
