Effect of ball milling process on mechanical properties of medical Ti–Mg composites
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摘要: 采用球磨+冷压制坯+微波加热烧结工艺制备Ti–15Mg复合材料，研究球磨工艺对Ti–15Mg混合粉末性能以及烧结后复合材料力学性能的影响。结果表明：以200 r·min−1球磨转速球磨8～10 h，随着球磨时间延长，混合粉末的平均粒径明显变小，粉末粒度分布逐渐集中在10～45 μm区间，粉末的球形度增加。在长时间球磨过程中，软质镁颗粒受到强烈撞击、研磨，引起表面破碎，钛颗粒出现了体积破碎和表面破碎，最终导致软质镁颗粒包裹脆性钛颗粒。球磨8 h后，混合粉末未出现明显的氧化，混合粉末中钛、镁粉末分布较为均匀，复合材料的力学性能较为优良，符合作为医用材料的力学性能要求。在低球磨转速下，球磨转速的提高不会导致粉末性能和烧结后复合材料性能出现明显变化。最佳球磨工艺参数为球磨时间8 h、球磨速度200 r·min−1，过程控制剂为正己烷。Abstract: Ti–15Mg composites were prepared by ball milling, cold pressing, and microwave heating sintering. The effects of ball milling parameters on the properties of the Ti–15Mg mixed powders and the mechanical properties of the sintered composites were studied. The results show that, the average particle size of the mixed powders decreases significantly with the extension of the milling time at the ball milling speed of 200 r·min−1 for 8～10 h, the particle size distribution gradually concentrates in the range of 10～45 μm, and the sphericity of the powders increases. In the process of long-time ball milling, the soft Mg particles are subjected to the strong impact and ground, eventually leading to the soft Mg particles wrapped in the brittle Ti particles. After ball milling for 8 h, there are no obvious oxidations in the mixed powders. The distribution of Ti and Mg powders in the mixed powders are relatively uniform, and the mechanical properties of the composites are relatively excellent, which meets the requirements of medical materials. At low milling speed, the increase of milling speed can not lead to the significant change in the powder’s properties and the sintered composite properties. The optimal ball milling parameters are obtained as the ball milling time of 8 h and the milling speed of 200 r·min−1 with n-hexane as the process control agent.
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Key words:
- mechanical milling /
- medical metal materials /
- Ti–Mg composites /
- mechanical properties
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图 1 原料粉末和球磨不同时间后混合粉末的扫描电子显微形貌：（a）Mg；（b）Ti；（c）6 h；（d）8 h；（e）10 h
Figure 1. SEM images of the raw material powders and the mixed powders after ball milling for the different times: (a) Mg; (b) Ti; (c) 6 h; (d) 8 h; (e) 10 h
图 2 不同球磨时间后混合粉末平均粒径
Figure 2. Average particle size of the mixed powders after different ball milling times
图 3 不同球磨时间球磨后粉末粒径分布
Figure 3. Particle size distribution of the mixed powders after the different milling times
图 4 不同球磨时间粉末压制成形的待烧结Ti–Mg坯体：（a）10 h；（b）8 h
Figure 4. Ti–Mg billets prepared by the mixed powders after ball milling for the different times: (a) 10 h; (b) 8 h
图 5 球磨8 h的Ti–Mg混合粉末微观形貌及能谱分析：（a）微观形貌；（b）Ti；（c）Mg
Figure 5. SEM image and EDS analysis of the Ti–Mg powders after ball milling for 8 h: (a) SEM image; (b) Ti; (c) Mg
图 6 球磨10 h的Ti–Mg粉末微观形貌及能谱分析：（a）微观形貌；（b）位置1能谱分析
Figure 6. Mixed Ti–Mg powders after ball milling for 10 h: (a) SEM image; (b) EDS analysis of location 1
图 7 球磨不同时间后Ti–Mg粉末的X射线衍射图谱（a）及局部放大图（b）
Figure 7. XRD patterns (a) and local magnification (b) of the mixed Ti–Mg powders after ball milling for different times
图 8 球磨过程中Ti–Mg混合粉末结构演变示意图
Figure 8. Structure evolution diagram of the Ti–Mg mixed powders during ball milling
图 10 不同球磨时间后磨罐壁上钛、镁粉体冷焊现象：（a）8 h；（b）10 h
Figure 10. Cold welding phenomenon of the Ti–Mg mixed powders on tank wall after ball milling for different times: (a) 8 h; (b) 10 h
图 11 球磨时间对复合材料性能的影响
Figure 11. Influence of the ball milling time on the properties of the composite materials
图 12 不同球磨转速球磨6 h后粉末粒径分布
Figure 12. Particle size distribution of the mixed powders after ball milling for 6 h with the different ball milling speeds
图 13 不同球磨转速球磨6 h后混合粉末平均粒径
Figure 13. Average particle size of the mixed powders after ball milling for 6 h with the different ball milling speeds
图 14 以100 r·min−1球磨转速球磨6 h后粉末微观形貌
Figure 14. SEM image of the mixed powders after ball milling for 6 h at 100 r·min−1
图 15 不同球磨转速对复合材料性能的影响
Figure 15. Effect of the ball milling speed on the properties of the composite materials
表 1 球磨过程中实验参数
Table 1. Experimental parameters during the ball milling
球料比 过程控制剂 球磨时间 / h 球磨转速 / (r·min−1) 10:1 正己烷 6 200 8 200 10 200 6 100 
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表 2 不同球磨时间下混合粉末的粉末收回率
Table 2. Powder recovery of the mixed powders under the different ball milling parameters
球磨时间 / h 球磨转速 / (r·min−1) 粉末收回率 / % 6 200 94.13 8 200 85.38 10 200 60.48
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表 3 不同球磨转速球磨6 h后混合粉末的粉末收回率
Table 3. Powder recovery rate of the mixed powders after ball milling for 6 h with different ball milling speeds
球磨转速 / (r·min−1) 粉末收回率 / % 200 94.13 100 96.67
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