Superfast preparation of Al-Sc alloys with high Sc content by spark plasma sintering
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摘要: 采用放电等离子烧结技术制备高钪含量Al-Sc合金, 利用扫描电子显微镜、能谱仪和X射线衍射仪等设备对球磨前后Al-Sc合金粉末的形貌、相组成以及不同温度快速烧结样品的显微组织结构进行观察和分析, 研究烧结温度对Al-Sc合金显微组织的影响。结果表明: 球磨后粉末的形状较规则, 其颗粒尺寸为25~45 μm, 并初步实现了机械合金化, 除Al、Sc相以外, 有少量Al3Sc和AlSc2相生成。放电等离子烧结可实现高钪含量铝钪合金的快速致密化, 成功制备出钪含量30%(质量分数)的铝钪合金, 通过调整烧结工艺参数, 烧结样品的相对密度可达92.19%;当烧结温度高于500℃时, 所得样品致密, 无孔洞, 且无明显晶界; 随着烧结温度的提高, Sc相与第二相融合, 形成Al3Sc、AlSc2等第二相, 存在于合金中, 且Al3Sc相呈现逐渐增强的趋势。Abstract: Aluminum-scandium alloys with high scandium content by mass were prepared by spark plasma sintering (SPS). The morphology, the phase composition, and the microstructures after sintering at different temperatures of Al-Sc alloy powders were investigated by scanning electron microscope (SEM), energy dispersive spectrometry (EDS), and X-ray diffractometry (XRD). The effect of sintering temperature on the microstructure of Al-Sc alloys was studied in the paper. The results show that, the Al-Sc alloy powders after ball milling are regular with the particle size of 25~45 μm, and the mechanical alloying of Al-Sc alloy powders is realized initially. In addition to the Al and Sc phases, a small amount of Al3Sc and AlSc2 are generated. The spark plasma sintering can realize the rapid densification of Al-Sc alloy with high scandium content, the Al-Sc alloy with 30% Sc by mass is successfully produced by SPS method. By adjusting the SPS process parameters, the relative density of sintered sample can be improved to 92.19%. The samples with the higher density and non-obvious grain boundary are achieved at the sintered temperature above 500℃. The second phases of Al3Sc and AlSc2 are formed by the combination of Sc with the increase of sintering temperature, and the peak intensity of Al3Sc increases gradually.
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Key words:
- spark plasma sintering /
- Al-Sc alloys /
- rapid densification /
- microstructure /
- sintering properties
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图 1 铝钪混合粉末扫描电镜图谱：（a）球磨前；（b）球磨后
Figure 1. SEM images of Al-Sc powders: (a) before mechanical milling; (b) after mechanical milling
图 2 铝钪合金粉末球磨前后的X射线衍射图谱：（a）球磨前；（b）球磨后
Figure 2. XRD patterns of Al-Sc powders: (a) before mechanical milling; (b) after mechanical milling
图 3 不同烧结温度下Al-30Sc合金样品的X射线衍射图谱：（a）450 ℃；（b）550 ℃；（c）600 ℃
Figure 3. XRD patterns of the Al-30Sc alloy samples sintered at different temperatures: (a) 450 ℃; (b) 550 ℃; (c) 600 ℃
图 4 不同烧结温度所得Al-30Sc合金样品的显微形貌：（a）450 ℃；（b）550 ℃；（c）600 ℃
Figure 4. Microstructures of the Al-30Sc alloy samples sintered at different temperatures: (a) 450 ℃; (b) 550 ℃; (c) 600 ℃
表 1 球磨前后铝钪合金粉末氮氧含量（质量分数）
Table 1. Nitrogen and oxygen contents in Al-Sc powders by mass before and after mechanical milling %
序号 球磨状态 质量分数/ % O N 1 球磨前 0.084~0.240 0.016 2 球磨后 0.053~0.600 0.015 
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表 2 不同烧结温度和压力下Al-30Sc合金样品的密度
Table 2. Density of the Al-30Sc alloy samples sintered at different temperatures and presses
序号 外加压力/ MPa 烧结温度/ ℃ 密度/ (g∙cm-3) 相对密度/ % 1 30 450 2.351 75.84 2 30 550 2.788 89.94 3 30 600 2.829 91.26 4 40 600 2.858 92.19
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表 3 不同温度烧结Al-30Sc合金样品在图 4中不同区域的能谱分析
Table 3. EDS analysis of different zones in Fig. 4 of the Al-30Sc alloy samples sintered at different temperatures
区域组成 450 ℃ 550 ℃ 600 ℃ A B A B A B Al 74.22 0.1 97.38 75.64 73.99 32.74 Sc 25.78 99.9 2.62 24.36 26.01 67.26 相 Al3Sc Sc-rich Sc-rich Al3Sc Al3Sc AlSc
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