Study on oxide inclusions of nickel-based P/M superalloy FHG96 by computed tomography technology
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摘要: 利用计算机断层扫描技术（computed tomography，CT）研究了FGH96镍基粉末高温合金内部Al2O3、SiO2及莫来石三种氧化物夹杂对不同工艺（热等静压工艺、热等静压+热挤压+等温锻造工艺及热等静压+等温锻造工艺）的敏感程度。结果表明：热等静压+等温锻造工艺能显著减小Al2O3夹杂物的尺寸和其在合金中的含量，采用热等静压+热挤压+等温锻造工艺最能有效减少SiO2夹杂物在合金中的含量，而莫来石夹杂对热等静压+热挤压+等温锻造工艺和热等静压+等温锻造工艺均较为敏感，且两种工艺对莫来石夹杂的作用效果类似。夹杂物在实际盘件中呈油饼状，极大地恶化了合金低周疲劳性能，且夹杂物越接近试样表面，试样的低周疲劳性能恶化越显著。热等静压+等温锻造工艺对减小三种夹杂的尺寸均有良好效果，这为人们选取合适工艺消除合金中氧化物夹杂提供了重要参考。Abstract: The sensitivity of oxide inclusions (Al2O3, SiO2, and mullite) in nickel-based powder metallurgy (P/M) superalloy (FGH96) to different processing technology was studied by computed tomography (CT) technology. The results show that, the process of hot isostatic pressing + isothermal forging can significantly reduce the Al2O3 inclusion size and decrease the content of Al2O3 inclusion in FGH96 alloy; the process of hot isostatic pressing + hot extrusion + isothermal forging can effectively reduce the content of SiO2 inclusion in the alloy; the mullite inclusions are sensitive to both the process of hot isostatic pressing + hot extrusion + isothermal forging and the process of hot isostatic pressing + isothermal forging, and the effects of the two processes are similar. The inclusions in the actual disc show the oil cake shaped, which greatly deteriorates the low cycle fatigue properties of the alloy. The closer the inclusions are to the sample surface, the more obvious the deterioration of low cycle fatigue properties is. Overall, the process of hot isostatic pressing + isothermal forging shows the good effect on reducing the inclusion size, providing an important reference to eliminate the influence of inclusions in alloys by the appropriate process.
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图 1 氧化物夹杂的显微形貌及能谱分析：（a）Al2O3夹杂物形貌；（b）SiO2夹杂物形貌；（c）Al2O3+SiO2混合夹杂物形貌；（d）Al2O3夹杂物能谱; （e）SiO2夹杂物能谱; （f）Al2O3+SiO2混合夹杂物能谱
Figure 1. Scanning electron microscopy (SEM) and energy dispersion spectrum (EDS) of oxide inclusions: (a) SEM of Al2O3; (b) SEM of SiO2; (c) SEM of Al2O3+SiO2; (d) EDS of Al2O3; (e) EDS of SiO2; (f) EDS of Al2O3+SiO2
图 2 热等静压态样品内Al2O3夹杂的CT扫描结果
Figure 2. CT characterization of Al2O3 inclusions in the as-HIPed samples
图 3 热等静压态样品内部夹杂物显微形貌及粒径分布：（a）Al2O3夹杂物形貌；（b）SiO2夹杂物形貌；（c）Al2O3+SiO2混合夹杂物形貌；（d）Al2O3夹杂物形貌放大图；（e）SiO2夹杂物形貌放大图；（f）Al2O3+SiO2混合夹杂物放大图；（g）Al2O3夹杂物晶粒尺寸分布；（h）SiO2夹杂物晶粒尺寸分布；（i）Al2O3+SiO2混合夹杂物晶粒尺寸分布
Figure 3. Scanning electron microscopy (SEM) and particle size distribution (PSD) of oxide inclusions in the as-HIPed samples: (a) SEM of Al2O3; (b) SEM of SiO2; (c) SEM of Al2O3+SiO2; (d) magnification SEM of Al2O3; (e) magnification SEM of SiO2; (f) magnification SEM of Al2O3+SiO2; (g) PSD of Al2O3; (h) PSD of SiO2; (i) PSD of Al2O3+SiO2
图 4 不同成形工艺下样品内部Al2O3夹杂物显微形貌及粒径分布：（a）HIP夹杂物形貌；（b）HEX夹杂物形貌；（c）HIF夹杂物形貌；（d）HIP夹杂物形貌放大图；（e）HEX夹杂物形貌放大图；（f）HIF混合夹杂物放大图；（g）HIP夹杂物晶粒尺寸分布；（h）HEX夹杂物晶粒尺寸分布；（i）HIF混合夹杂物晶粒尺寸分布
Figure 4. Scanning electron microscopy (SEM) and particle size distribution (PSD) of Al2O3 inclusions in different process conditions: (a) SEM of as-HIPed samples; (b) SEM of as-HEXed samples; (c) SEM of as-HIFed samples; (d) magnification SEM of as-HIPed samples; (e) magnification SEM of as-HEXed samples; (f) magnification SEM of as-HIFed samples; (g) PSD of as-HIPed samples; (h) PSD of as-HEXed samples; (i) PSD of as-HIFed samples
图 5 不同成形工艺下样品内部SiO2夹杂物显微形貌及粒径分布：（a）HIP夹杂物形貌；（b）HEX夹杂物形貌；（c）HIF夹杂物形貌；（d）HIP夹杂物形貌放大图；（e）HEX夹杂物形貌放大图；（f）HIF混合夹杂物放大图；（g）HIP夹杂物晶粒尺寸分布；（h）HEX夹杂物晶粒尺寸分布；（i）HIF混合夹杂物晶粒尺寸分布
Figure 5. Scanning electron microscopy (SEM) and particle size distribution (PSD) of SiO2 inclusions in different process conditions: (a) SEM of as-HIPed samples; (b) SEM of as-HEXed samples; (c) SEM of as-HIFed samples; (d) magnification SEM of as-HIPed samples; (e) magnification SEM of as-HEXed samples; (f) magnification SEM of as-HIFed samples; (g) PSD of as-HIPed samples; (h) PSD of as-HEXed samples; (i) PSD of as-HIFed samples
图 6 不同成形工艺下样品内部莫来石夹杂物显微形貌及粒径分布：（a）HIP夹杂物形貌；（b）HEX夹杂物形貌；（c）HIF夹杂物形貌；（d）HIP夹杂物形貌放大图；（e）HEX夹杂物形貌放大图；（f）HIF混合夹杂物放大图；（g）HIP夹杂物晶粒尺寸分布；（h）HEX夹杂物晶粒尺寸分布；（i）HIF混合夹杂物晶粒尺寸分布
Figure 6. Scanning electron microscopy (SEM) and particle size distribution (PSD) of mullite inclusions in different process conditions: (a) SEM of as-HIPed samples; (b) SEM of as-HEXed samples; (c) SEM of as-HIFed samples; (d) magnification SEM of as-HIPed samples; (e) magnification SEM of as-HEXed samples; (f) magnification SEM of as-HIFed samples; (g) PSD of as-HIPed samples; (h) PSD of as-HEXed samples; (i) PSD of as-HIFed samples
图 7 实际盘件中夹杂物宏观形貌：（a）径向；（b）轴向
Figure 7. Macro morphology of inclusions existed in the real disk: (a) radial direction; (b) axial direction
图 8 超塑性变形盘件中夹杂物形貌的二维切片数据（a）和三维重构结果（b）
Figure 8. 2D slicing data (a) and 3D reconstruction (b) of inclusion morphology existed in the superplastic deformed disk
表 1 FGH96镍基粉末高温合金化学成分
Table 1. Chemical composition of nickel-based powder metallurgy superalloy FGH96
C Cr Co Mo W Al Ti Nb B Zr Ni 0.02~0.05 15.5~16.5 12.5~13.5 3.8~4.2 3.8~4.2 2.0~2.4 3.5~3.9 0.6~1.0 0.006~0.015 0.025~0.050 余量 
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表 2 夹杂物位置对试样低周疲劳性能的影响
Table 2. Effect of inclusion location on the low cycle fatigue properties of the specimen
试样编号 夹杂位置 循环周次 1 试样中心 52179 2 约1/2半径处 44121 3 试样边缘 4550 不含夹杂 — 60000（未断）
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