小角中子散射原位研究镍基高温合金第二相析出演化行为

doi:10.11900/0412.1961.2024.00068

金属学报

2024, Vol. 60

Issue (8): 1100-1108 DOI: 10.11900/0412.1961.2024.00068

研究论文

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小角中子散射原位研究镍基高温合金第二相析出演化行为

李亚微¹, 谢光¹(

), 柯于斌²^,³, 卢玉章¹, 黄亚奇¹, 张健¹(

)

1 中国科学院金属研究所师昌绪先进材料创新中心沈阳 110016
2 散裂中子源科学中心东莞 523803
3 中国科学院高能物理研究所北京 100049

In Situ Small-Angle Neutron Scattering Study of Precipitation and Evolution Behavior of Secondary Phases in Ni-Based Superalloys

LI Yawei¹, XIE Guang¹(

), KE Yubin²^,³, LU Yuzhang¹, HUANG Yaqi¹, ZHANG Jian¹(

)

1 Shi-changxu Innovation Center for Advanced Materials, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
2 Spallation Neutron Source Science Center, Dongguan 523803, China
3 Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049, China

引用本文:

李亚微, 谢光, 柯于斌, 卢玉章, 黄亚奇, 张健. 小角中子散射原位研究镍基高温合金第二相析出演化行为[J]. 金属学报, 2024, 60(8): 1100-1108.
Yawei LI, Guang XIE, Yubin KE, Yuzhang LU, Yaqi HUANG, Jian ZHANG. In Situ Small-Angle Neutron Scattering Study of Precipitation and Evolution Behavior of Secondary Phases in Ni-Based Superalloys[J]. Acta Metall Sin, 2024, 60(8): 1100-1108.

全文: PDF(2193 KB) HTML

摘要:

γ′和γ′′相是镍基高温合金中的重要强化相，为了阐明其在热处理中的析出演化机制，本工作以广泛使用的GH4169合金为对象，采用小角中子散射原位研究了固溶时效热处理中第二相的析出演化行为，并借助TEM对非原位样品进行验证分析。结果表明：合金中第二相主要在时效过程中析出，包括球状γ′相和γ′与γ′′复合相(以γ′′/γ′/γ′′三明治结构为主)。其中，球状γ′相数量随时效进行不断增多；复合相在一级时效中大量形成，但在二级时效中数量变化不大。此外，2类析出相尺寸均在一级时效时逐渐增大，在二级时效时几乎不变。在整个时效过程中，球状γ′相与基体相界面逐渐尖锐，而复合相越来越扁，其界面成分波动始终显著。由此可知，第二相的析出演化行为受控于界面元素扩散机制。

关键词 ： GH4169, 热处理, 小角中子散射, 第二相, 析出演化行为

Abstract：

The γ′ and γ′′ phases are crucial strengthening components in Ni-based superalloys. Understanding their precipitation and evolution mechanism during heat treatment is essential for tailoring the mechanical properties of the superalloys. Herein, GH4169 superalloy was used to investigate the precipitation and evolution behaviors of secondary phases during in situ standard heat treatment by time-of-flight small-angle neutron scattering. Further, transmission electron microscopy was employed to observe the secondary phases generated in samples after ex situ heat treatment. Results showed that the secondary phases, including the spherical γ′ phase and coprecipitates (mainly the γ′′/γ′/γ′′ sandwich structure), mostly occurred during the aging treatment. After the formation of coprecipitates during the first aging treatment (AT1), their quantity apparently remained stable during the second aging treatment (AT2). Furthermore, the average size of the γ′ phase and coprecipitates gradually increased during the AT1 stage while remaining almost constant during the AT2 stage. Throughout the aging process, the interface between spherical γ′ phase and γ matrix exhibited a decreased composition fluctuation, while the interface fluctuation of coprecipitates was always significant. Thus, it can be inferred that the precipitation and evolution behaviors of secondary phases are controlled by the element diffusion at the interface.

Key words： GH4169 heat treatment small-angle neutron scattering second phase precipitation and evolution behavior

收稿日期: 2024-03-05

ZTFLH:

TG132.3

基金资助:国家重点研发计划项目(2021YFA1600603);国家自然科学基金项目(52271042);国家自然科学基金项目(51911530154);国家自然科学基金项目(91860201);国家自然科学基金项目(U2141206);国家科技重大专项项目(J2019-VI-0010-0124);中国科学院依托重大科技基础设施的建制化科研项目(JZHKYPT-2021-01);航空发动机及燃气轮机基础科学中心项目(P2022-C-IV-001-001)

通讯作者: 谢光，gxie@imr.ac.cn，主要从事高温合金组织性能研究张健，jianzhang@imr.ac.cn，主要从事高温合金研发

Corresponding author: XIE Guang, professor, Tel: (024)23971712, E-mail: gxie@imr.ac.cnZHANG Jian, professor, Tel: (024)23911196, E-mail: jianzhang@imr.ac.cn

作者简介: 李亚微，男，1995年，博士

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图1 GH4169高温合金原位热处理工艺

图2 原位热处理不同阶段下的典型二维小角中子散射(SANS)图谱

图3 原位热处理不同阶段不同时刻下的一维I-Q关系曲线

图4 原位时效热处理中Porod因子的变化

图5 原位时效热处理中盘状第二相半径(R)的变化

图6 原位时效热处理中球状第二相尺寸(r)分布

图7 原位时效热处理中球状第二相中值半径(rmed)的变化

图8 非原位热处理样品中第二相TEM表征

图9 盘状γ′′/γ′/γ′′三明治结构示意图

表1 非原位热处理样品第二相定量统计结果

图10 第二相析出演化过程示意图

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