High temperature oxidation microstructure analysis of Ni-based P/M superalloy coated with an inorganic aluminum coating
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摘要: 使用TWL12+TWL20无机盐铝涂层喷涂于镍基粉末高温合金表面，采用XRD、SEM、EPMA和TEM研究无机盐铝涂层与粉末高温合金经700、750、800 ℃高温氧化后的组织变化。结果表明：高温氧化后涂层表层结构出现剥落，涂层中的铝与基体合金发生扩散，形成由氧化区、扩散区、互扩散区组成的过渡层，其中氧化区为最外层，该区域主要富集O、Al元素，形成Al2O3层；随之的扩散区主要含有Ni、Al元素，形成NiAl相及在其中弥散分布的α-Cr相；最后是富集Ti、Cr、Co、Ta等元素的互扩散区，存在于扩散区与基体之间，主要由Ni2AlTi相基体及在其中弥散分布的σ相组成；分析表明过渡层厚度随着氧化温度升高而变化，主要表现为互扩散区宽度增加，扩散区中的α-Cr相与互扩散区的σ相尺寸增大，且σ相沿垂直过渡区方向生长的趋势加剧；氧化增重曲线表明，涂层表层结构脱落后，过渡层在750、800 ℃高温氧化过程中表现出良好的抗氧化性能，说明TWL12+TWL20无机盐铝涂层具有为航空发动机用先进粉末高温合金提供高温氧化涂层保护的潜力。
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关键词:
- TWL12+TWL20无机盐铝涂层 /
- 镍基粉末高温合金 /
- 高温氧化 /
- 显微组织
Abstract: In this paper, TWL12 + TWL20 inorganic salt aluminum coating was sprayed on the surface of Ni-based P/M superalloy. The microstructure changes of inorganic salt aluminum coating and P/M superalloy after high temperature oxidation at 700, 750 ℃ and 800 ℃ were studied by XRD, SEM, EPMA and TEM. The results show that after high temperature oxidation, the surface structure of the coating peels off, and the aluminum in the coating diffuses with the substrate to form a transition layer composed of oxidation zone, diffusion layer and interdiffusion zone. The oxidation zone is the outermost layer, where is mainly enriched with O and Al elements to form Al2O3 layer. The diffusion layer mainly contains Ni and Al elements, forming NiAl phase and α-Cr phase dispersed in it. Finally, the interdiffusion zone rich in Ti, Cr, Co, Ta and other elements exists between the diffusion zone and the matrix, which is mainly composed of Ni2AlTi phase matrix and σ phase dispersed in it. The analysis shows that the thickness of transition layer changes with the increase of oxidation temperature, it is mainly manifested by the increase of the width of the interdiffusion zone, the increase of the size of α-Cr phase in the diffusion layer and σ phase in the interdiffusion zone, and the growth trend of σ phase along the vertical transition zone is intensified. The oxidation weight gain curve shows that the transition layer exhibits good oxidation resistance during high temperature oxidation at 750 ℃ and 800 ℃ after the surface structure of the coating falls off, it indicates that the TWL12 + TWL20 inorganic salt aluminum coating has the potential to provide high temperature oxidation coating protection for advanced P/M superalloy used in aeroengines. -
图 2 无机盐铝涂层表面形貌和截面形貌 （a）涂层表面形貌；（b）涂层截面形貌
Figure 2. Surface morphology and cross section morphology of inorganic aluminum coating （a）coating surface morphology；（b）coating cross section morphology
图 4 大气环境中涂层在不同温度下高温氧化100 h后的表面形貌 （a）700 ℃；（b）750 ℃；（c）800 ℃
Figure 4. Surface morphologies of coatings in air environment after 100 h oxidation （a）700 ℃；（b）750 ℃；（c）800 ℃
图 5 涂层高温氧化后表面XRD图
Figure 5. XRD patterns of the coating surface after high temperature oxidation
图 6 大气环境中涂层在700 ℃下高温氧化100 h试样截面分析 （a）截面形貌；（b）EPMA元素分布；（c）图（a）中a1位置高倍形貌；（d）图（a）中a2位置高倍形貌
Figure 6. Cross section analysis of coating samples oxidized at 700 ℃ for 100h in air （a）cross section morphology；（b）EPMA element distribution；（c）high power morphology of a1 position in Fig.（a）；（d）high power morphology of a2 position in Fig.（a）
图 7 扩散区和互扩散区区域的微区TEM分析 （a）扩散区微区的HADDF；（b）扩散区微区的EDS元素点分析；（c）互扩散区微区的HADDF；（d）互扩散区微区的EDS面分布
Figure 7. TEM analysis of diffusion layer and interdiffusion zone （a）HADDF of diffusion layer；（b）EDS element analysis of diffusion layer；（c）HADDF of interdiffusion zone；（d）EDS mapping of interdiffusion zone
图 8 大气环境中涂层在750 ℃下高温氧化100 h试样截面形貌 （a）截面形貌；（b）EPMA元素分布；（c）图（a）中a1位置高倍形貌；（d）图（a）中a2位置高倍形貌
Figure 8. Cross section analysis of coating samples oxidized at 750 ℃ for 100 h in air （a）cross section morphology；（b）EPMA element distribution；（c）high power morphology of a1 position in Fig（a）；（d）high power morphology of a2 position in Fig（a）
图 9 大气环境中涂层在800 ℃下高温氧化100 h试样截面形貌 （a）截面形貌；（b）EPMA元素分布;（c）图（a）中a1位置高倍形貌；（d）图（a）中a2位置高倍形貌
Figure 9. Cross section analysis of coating samples oxidized at 800 ℃ for 100 h in air （a）cross section morphology；（b）EPMA element distribution；（c）high power morphology of a1 position in Fig（a）；（d）high power morphology of a2 position in Fig（a）
图 10 高温氧化过程中涂层与基体的反应机理
Figure 10. Reaction mechanism between coating and substrate during high temperature oxidation
表 1 镍基粉末高温合金主要成分（质量分数/%）
Table 1. Composition of a Ni-based P/M superalloy（mass fraction/%）
Cr Al Ti Co W Mo Nb Ta Other Ni 16-21 3-5 2-3 10-13 2-4 2-4 1-2 2-3 <0.5 Bal 
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