Effect of rare earth Yb and Ce on high temperature oxidation resistance of TiAl alloys
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摘要: 采用放电等离子烧结制备添加微量稀土元素的钛铝合金，研究稀土元素Yb、Ce对钛铝合金高温抗氧化性能的影响。利用金相显微镜、扫描电子显微镜和X射线衍射仪分析钛铝合金的组织结构、微观形貌和物相组成，通过高温氧化实验分析合金的高温抗氧化性能。结果表明：经放电等离子烧结制备的钛铝合金的相对密度最高可达99%。800 ℃高温氧化后的氧化动力学曲线均近似遵循抛物线规律；经过100 h的高温氧化处理后，Ti‒45Al、Ti‒45Al‒0.3Yb2O3和Ti‒45Al‒0.3CeO2三种合金的质量增重分别为14.63 g·m‒2、7.02 g·m‒2、8.19 g·m‒2。添加稀土元素的钛铝合金的高温抗氧化性能明显得到改善，其中添加Yb的钛铝合金的高温抗氧化性能提高约1倍。钛铝合金的氧化产物均具有典型层状结构，最外层为TiO2，第二层为TiO2+Al2O3混合氧化物。Abstract: TiAl alloys added with the trace rare earth elements were prepared by spark plasma sintering (SPS). The effects of rare earth elements Yb and Ce on the high temperature oxidation resistance of TiAl alloys were investigated. The microstructure, morphology, and phase composition of TiAl alloys were analyzed by metallographic microscope, scanning electron microscope, and X-ray diffraction. The high temperature oxidation resistance of the alloys was studied by high temperature oxidation experiment. The results show that the relative density of TiAl alloys prepared by SPS is up to 99%. The oxidation kinetics curves of 800 ℃ high temperature oxidation approximately follow the parabolic rule. After the high temperature oxidation at 800 ℃ for 10 h, the mass gain of Ti‒45Al, Ti‒45Al‒0.3Yb2O3, and Ti‒45Al‒0.3CeO2 are 14.63 g·m‒2, 7.02 g·m‒2, and 8.19 g·m‒2, respectively. The high temperature oxidation resistance of the TiAl alloys with the rare earth elements addition is obviously improved, and the high temperature oxidation resistance of Ti‒45Al‒0.3Yb2O3 is increased by about 1 time compared with that of Ti‒45Al. The oxidation products of TiAl alloys have the typical layered structure, the outermost layer is TiO2, and the second layer is TiO2+Al2O3 mixed oxide.
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图 2 钛铝合金的显微形貌和金相组织：（a）Ti‒45Al；（b）Ti‒45Al‒0.3Yb2O3；（c）Ti‒45Al‒0.3CeO2；（d）Ti‒45Al；（e）Ti‒45Al‒0.3Yb2O3；（f）Ti‒45Al‒0.3CeO2
Figure 2. SEM images and metallographic images of TiAl alloys: (a) Ti−45Al; (b) Ti−45Al−0.3Yb2O3; (c) Ti−45Al−0.3CeO2; (d) Ti−45Al; (e) Ti−45Al−0.3Yb2O3; (f) Ti−45Al−0.3CeO2
图 3 钛铝合金电子背散射衍射形貌和晶粒分布：（a）Ti‒45Al EBSD；（b）Ti‒45Al‒0.3Yb2O3 EBSD；（c）Ti‒45Al‒0.3CeO2 EBSD；（d）Ti‒45Al晶粒分布；（e）Ti‒45Al‒0.3Yb2O3晶粒分布；（f）Ti‒45Al‒0.3CeO2晶粒分布
Figure 3. EBSD and grain size distribution of TiAl alloys: (a) Ti‒45Al EBSD; (b) Ti‒45Al‒0.3Yb2O3 EBSD; (c) Ti‒45Al‒0.3CeO2 EBSD; (d) Ti‒45Al grain size distribution; (e) Ti‒45Al‒0.3Yb2O3 grain size distribution; (f) Ti‒45Al‒0.3CeO2 grain size distribution
图 4 钛铝合金在800 ℃空气中氧化曲线：（a）单位面积质量变化；（b）氧化速率
Figure 4. Oxidation curves of the TiAl alloys at 800 ℃: (a) mass gain in unit area; (b) oxidation rate
图 5 钛铝合金800 ℃在空气中氧化动力学曲线：（a）Ti‒45Al；（b）Ti‒45Al‒0.3Yb2O3；（c）Ti‒45Al‒0.3CeO2
Figure 5. Oxidation kinetics curves of the TiAl alloys oxidized at 800 ℃ in air: (a) Ti‒45Al; (b) Ti‒45Al‒0.3Yb2O3; (c) Ti‒45Al‒0.3CeO2
图 6 800 ℃氧化50 h钛铝合金氧化表面X射线衍射图谱
Figure 6. XRD patterns of the TiAl alloys surface oxidized at 800 ℃ for 50 h
图 7 800 ℃氧化100 h后钛铝合金氧化层表面显微形貌：（a）Ti‒45Al；（b）Ti‒45Al‒0.3Yb2O3；（c）Ti‒45Al‒0.3CeO2
Figure 7. Surface morphology of the TiAl alloys after oxidation at 800 ℃ for 100 h: (a)Ti‒45Al; (b)Ti‒45Al‒0.3Yb2O3; (c)Ti‒45Al‒0.3CeO2
图 8 800 ℃氧化100 h后合金氧化层截面显微形貌和元素面分布能谱分析：（a）Ti‒45Al；（b）Ti‒45Al‒0.3Yb2O3；（c）Ti‒45Al‒0.3CeO2；（d）能谱分析
Figure 8. Microstructure in the cross section and EDS analysis of the alloys after oxidation at 800 ℃ for 100 h: (a) Ti‒45Al; (b) Ti‒45Al‒0.3Yb2O3; (c) Ti‒45Al‒0.3CeO2; (d) EDS analysis
表 1 实验制备试样的化学成分（原子数分数）及相对密度
Table 1. Chemical compositions (atomic fraction) and relative density of the samples
% 试样编号 化学成分 相对密度 1# Ti–45Al 98.2 2# Ti–45Al–0.3Yb2O3 99.5 3# Ti–45Al–0.3CeO2 93.4 
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