Effect of high temperature oxidation on the surface state of FGH96 superalloy powders
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摘要: 通过模拟FGH96高温合金粉末在热等静压固结阶段的高温加热过程，利用多种表面分析方法，研究高温氧化对粉末表面状态的影响。结果表明，近热等静压加热温度条件下的高温氧化过程显著改变了FGH96高温合金粉末的表面形貌、表面元素分布和析出相组成。随加热温度的升高和保温时间的延长，胞状晶为主、树枝晶为辅的表面凝固组织被氧化物/碳化物层所覆盖，高温氧化过程促进粉末基体内部的Ni、Ti、Zr、Nb、Al和C原子逐渐扩散到粉末表面，粉末表面预先存在的氧化物（ZrO2）为MC型碳化物（(Ti, Nb)C）的形核提供了结构条件。控制粉末表面氧化物的形成可以有效限制合金中形成原始颗粒边界缺陷。
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关键词:
- FGH96高温合金粉末 /
- 高温氧化 /
- 粉末表面状态 /
- 原始颗粒边界
Abstract: The effect of high temperature oxidation on the surface state of FGH96 superalloy powders was studied by simulating the high temperature heating process during hot isostatic pressing (HIP) consolidation. The results indicate that the surface morphology, surface element distribution, and precipitate composition of the FGH96 superalloy powders are significantly changed by high temperature oxidation at near HIP temperature. With the increase of heating temperature and the extension of holding time, the surface solidification structure of cell crystals and dendritic crystals are covered by oxide/carbide layers. The high temperature oxidation process promotes the diffusion of Ni, Ti, Zr, Nb, Al, and C atoms inside the powder matrix to the powder surface. The pre-existing oxides (ZrO2) on the powder surface provide the structural conditions for the nucleation of MC carbides (Ti, Nb)C. Controlling the formation of oxides on the powder surface can effectively limit the formation of prior particle boundaries (PPBs) defects in the alloys. -
图 1 FGH96高温合金粉末典型特征：（a）粉末显微形貌；（b）粉末最外表面元素分布
Figure 1. Typical characteristics of the FGH96 superalloy powders: (a) SEM images of powders; (b) element distribution on the outmost surface of powders
图 2 不同条件高温氧化后FGH96高温合金粉末的表面形貌：（a）～（d）1020、1070、1120、1170 ℃，保温10 min；（e）～（h）1020、1070、1120、1170 ℃，保温60 min；（i）～（l）1020、1070、1120、1170 ℃，保温240 min
Figure 2. Surface morphology of the FGH96 superalloy powders with the different high temperature oxidation conditions: (a)~(d) 1020, 1070, 1120, 1170 ℃ for 10 min; (e)~(h) 1020, 1070, 1120, 1170 ℃ for 60 min; (i)~(l) 1020, 1070, 1120, 1170 ℃for 240 min
图 3 经1020 ℃保温10 min高温氧化后粉末表面形貌和面扫元素分布
Figure 3. Powder surface morphology and EDS scanning element distribution of powders oxidized at 1020 ℃ for 10 min
图 4 经1170 ℃保温240 min高温氧化后粉末表面形貌和面扫元素分布
Figure 4. Powder surface morphology and EDS scanning element distribution of powders oxidized at 1170 ℃ for 240 min
图 5 经1020 ℃保温10 min高温氧化后粉末截面组织和面扫元素分布
Figure 5. Powder cross-section microstructure and EPMA scanning element distribution of powders oxidized at 1020 ℃ for 10 min
图 6 经1170 ℃保温240 min高温氧化后粉末截面组织和面扫元素分布
Figure 6. Powder cross-section microstructure and EPMA scanning element distribution of powders oxidized at 1170 ℃ for 240 min
图 7 经1020 ℃保温10 min高温氧化后粉末表面随刻蚀深度变化的TOF-SIMS元素分布：（a）～（b）元素分布曲线；（c）～（k）元素3D分布图
Figure 7. TOF-SIMS element distribution of powder surface with the different etching depth after oxidized at 1020 ℃ for 10 min: (a)~(b) the element distribution curves; (c)~(k) the element 3D distribution diagrams
图 9 经1170 ℃保温240 min高温氧化后粉末表面随刻蚀深度变化的TOF-SIMS元素分布：（a）～（b）元素分布曲线；（c）~（k）元素3D分布图
Figure 9. TOF-SIMS element distribution of powder surface with different the etching depth after oxidized at 1170 ℃ for 240 min: (a)~(b) the element distribution curves; (c)~(k) the element 3D distribution diagrams
图 8 经1170 ℃保温10 min高温氧化后粉末表面随刻蚀深度变化的TOF-SIMS元素分布：（a）～（b）元素分布曲线；（c）～（k）元素3D分布图
Figure 8. TOF-SIMS element distribution of powder surface with different the etching depth after oxidized at 1170 ℃ for 10 min: (a)~(b) the element distribution curves; (c)~(k) the element 3D distribution diagrams
图 10 经1020 ℃保温10 min高温氧化后粉末表面析出相分布
Figure 10. Distribution of precipitates on the surface of powders oxidized at 1020 ℃ for 10 min
图 11 经1020 ℃保温240 min高温氧化后粉末表面析出相分布
Figure 11. Distribution of precipitates on the surface of powders oxidized at 1020 ℃ for 240 min
图 12 经1170 ℃保温10 min高温氧化后粉末表面析出相分布
Figure 12. Distribution of precipitates on the surface of powders oxidized at 1170 ℃ for 10 min
图 13 经1170 ℃保温60 min高温氧化后粉末表面析出相分布
Figure 13. Distribution of precipitates on the surface of powders oxidized at 1170 ℃ for 60 min
图 14 经1170 ℃保温240 min高温氧化后粉末表面析出相分布
Figure 14. Distribution of precipitates on the surface of powders oxidized at 1170 ℃ for 240 min
表 1 实验用FGH96高温合金粉末的化学成分（质量分数）
Table 1. Chemical compositions of the investigated FGH96 superalloy powders
% Ni C Cr Mo Nb Fe Co W Ti Al Zr 余量 0.045 16.000 0.510 0.790 0.060 13.200 4.100 4.000 2.200 0.060 
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