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摘要: 以烧结刚玉、α-Al2O3微粉、高纯镁砂、金属铝粉为原料, 酚醛树脂为结合剂, 制备Mg O–Al2O3和Al–MgO–Al2O3系复合材料, 样品成型后经过200℃烘干, 于1500℃氧化气氛烧成。利用X射线衍射仪, 扫描电子显微镜和能谱仪研究了金属铝粉对MgO–Al2O3复合材料抗氧化性的影响。结果表明: 未添加金属铝粉的样品烧后主晶相为α-Al2O3及镁铝尖晶石, 微观结构较为疏松; 引入金属铝粉后, 样品烧后主晶相为α-Al2O3及镁铝尖晶石, 新生相包括Al4O4C、Al4C3、(Al2OC)x(AlN)1-x等, 微观结构较为致密, 样品性能得到改善。添加金属铝粉样品的内外组成呈梯度变化, Al4O4C相主要出现在样品内部, 并有金属铝残留; 金属铝粉引入使样品氧分压从表面到内部依次降低, 金属铝粉氧化后与Mg O原位合成尖晶石, 使结构致密化, 阻隔了氧气的进一步渗入, 样品内部形成的Al2O与C反应得到晶须状Al4O4C。Abstract: MgO–Al2O3 and Al–Mg O–Al2O3 composites were prepared by using the sintered alumina, α-Al2O3 powders, high purity magnesia, and aluminum powders as raw materials, and the phenolic resin as binder. After molding, the samples were dried at 200 ℃ and then sintered at 1500 ℃ in oxidation atmosphere. The effect of aluminum powders on the oxidation resistance of Al2O3–MgO composites were investigated by X-ray diffractometer(XRD), scanning electron microscope(SEM), and energy dispersion spectrometer(EDS). The results show that, the major crystalline phases of the sintered samples without Al addition are α-Al2O3 and MgAl2O4, and the microstructures of the sintered samples are looser. The major crystalline phases of the sintered samples with Al addition are α-Al2O3 and MgAl2O4, and the newly formed phases are Al4O4C, Al4C3, and(Al2OC)x(AlN)1-x; the microstructures of the sintered samples are more densification, and the sintering and properties of samples were improved. The internal and external components of the sintered samples with Al addition show the gradient changes, and the Al4O4C phase mainly appears in the internal region of the sample with residual aluminum. The oxygen partial pressure in the sintered samples decreases gradually from the surface to the interior due to the Al powder addition, the microstructures are densified by spinel, which is in-situ synthesized by oxidizing aluminum powders and MgO, preventing the further infiltration of oxygen. The whisker-like Al4O4C is obtained by the reaction of Al2O formed in the sample and C.
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Keywords:
- composites /
- aluminum powders /
- MgAl2O4 spinel /
- oxidation resistance
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图 1 1500℃烧成后样品X射线衍射仪图谱：（a）整体图；（b）试样内部局部放大图
Figure 1. XRD patterns of samples sintered at 1500℃: (a)whole diagram; (b)local enlargement of internal sample
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图 2 Al–Al2O3体系各气相气压随温度变化图
Figure 2. Gaseous phase pressure with temperature in Al–Al2O3phase system
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图 3 样品宏观切面图：（a)A0;(b)A1
Figure 3. Macroscopic sectional images of samples: (a)A0;(b)A1
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图 4 A0样品断口扫描电子显微形貌：（a）低倍照片；（b）高倍照片
Figure 4. SEM images of fracture surface in A0 sample: (a)low magnification; (b)high magnification
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图 5 A1样品的断口扫描电子显微形貌：（a）外部低倍；（b）外部高倍；（c）内部低倍；（d）内部高倍
Figure 5. SEM images of fracture surfaces in A1 sample: (a)low magnification(outside); (b)high magnification(outside); (c)low magnification(inside); (d)high magnification(inside)
表 1 原料配比（质量分数）
Table 1 Proportion of raw materials
% 样品编号 烧结刚玉 高纯烧结镁砂（≤1mm） 烧结刚玉（≤44μm） 金属铝粉（≤44μm） α-Al2O3微粉（≤5μm） 3~5mm 1~3mm ≤1mm A0 10 40 15 15 15 — 5 A1 10 40 3 15 15 12 5 
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表 2 升温制度
Table 2 Heating condition
温度区间/℃ 运行时间/h 烧结速率/(℃·h-1) 室温~580 1 580 580 1（保温） — 580~1500 3 306 1500 3（保温） — 1300~350 随炉冷却 —
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表 3 烧成后样品物理性能
Table 3 Physical properties of sintered samples
样品编号 显气孔率/% 密度/(g·cm–3) 常温耐压强度/MPa 线变化率（1500 ℃，2 h）/% A0 25.5 2.76 40 0.92 A1 15.4 2.80 61 1.15
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