Study on the preparation process of Ti coatings on ZrO2 balls by mechanical milling coating technology
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摘要: 采用机械球磨涂覆技术在1 mm氧化锆球体上制备钛涂层, 研究了球料比、球磨时间及球磨气氛对钛涂层形成的影响, 利用扫描电子显微镜(scanning electron microscope, SEM)、X射线衍射(X-ray diffraction, XRD)及超声波对钛涂层的显微结构及物理性能进行了表征。结果表明, 钛涂层厚度随球磨时间、球料比的增加先增加后减小, 球磨30 h的涂层平均厚度最大, 约为76 μm, 球料比2.5:1.0的涂层平均厚度最大, 约为73 μm; 钛涂层结合强度随球磨时间的增加先增加后减小; 球磨过程中适当增加球料比, 可缩短涂层的形成时间; 在球磨过程中间歇性引入空气, 球磨罐中的钛粉易被氧化成TiO, 导致涂层形成困难, 故而球磨过程处于密封状态更有利于钛涂层的形成。Abstract: The titanium (Ti) coatings were prepared on the surface of ZrO2 balls in the average diameter of 1 mm by mechanical milling coating technology. The influences of milling time, ball-to-powder weight ratio, and milling atmosphere on the formation of titanium coatings were systemically investigated. The microstructure and physical properties of titanium coatings were characterized by scanning electron microscope (SEM), X-ray diffraction (XRD), and ultrasonic wave. The results show that, the thickness of titanium coatings firstly increases and then decreases with the increasing of milling time and ball-to-powder weight ratio. The average thickness of the coating milled for 30 h reaches the maximum as about 76 μm. Meanwhile, the ball-to-powder weight ratio of 2.5:1.0 can provide the maximum average thickness of Ti coatings (about 73 μm). The binding strength of titanium coating increases first andthen decreases with the increasing of milling time. The forming time of coatings can be shortened by increasing the ball-to-powder weight ratio properly. The titanium powders in the ball-mill can be easilty oxidized to TiO by the intermittent air introduction, which further hinders the formation of coatings. So, the sealing state in ball milling process is more beneficial to the formation of titanium coating.
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图 1 不同球磨时间下氧化锆球表面钛涂层和截面形貌：（a）5 h；（b）10 h；（c）15 h；（d）25 h；（e）35 h
Figure 1. Surface and cross section micrographs of Ti coatings on ZrO2 balls milled for different times: (a) 5 h; (b) 10 h; (c) 15 h; (d) 25 h; (e) 35 h
图 2 球磨时间与氧化锆球增重率及涂层平均厚度的关系
Figure 2. Relationship of the coating thickness, weight gain rate, and milling time
图 3 球磨时间与涂层结合强度（失重率）的关系
Figure 3. Relationship between the bonding strength (weight loss rate) of coating and milling time
图 4 不同球料比球磨15 h后样品的横截面显微照片：（a）1:1；（b）1.5:1.0；（c）2:1；（d）2.5:1.0；（e）3:1；
Figure 4. Cross section micrographs of the coatings milled for 15 h at different ball to powder weight ratio: (a) 1:1; (b) 1.5:1.0; (c) 2:1; (d) 2.5:1.0; (e) 3:1
图 5 球料比与表面涂层平均厚度的关系
Figure 5. Relationship between the ball to powder weight ratio and the average thickness of coatings
图 6 不同球磨气氛下球磨22 h后的样品外观形貌：（a）基体；（b）密封球磨；（c）间歇性引入空气
Figure 6. Sample morphology milled for 22 h in different milling atmosphere: (a) substrate; (b) sealing state; (c) intermittent air introduction
图 7 不同球磨气氛下球磨22 h涂层的横截面照片：（a）密封状态；（b）间歇性引入空气
Figure 7. Cross section micrographs of the coatings milled for 22 h in different milling atmosphere: (a) sealing state; (b) intermittent air introduction
图 8 不同球磨气氛下球磨钛粉的X射线衍射图谱
Figure 8. XRD patterns of Ti powders milled in different milling atmosphere
表 1 球磨工艺参数
Table 1. Process parameters of ball milling
球磨时间/ h 球料比 球磨气氛 球磨转速/ (r·min‒1) 装填量/ g 5 2:1 球磨罐密闭 300 80 10 15 25 35 15 1:1 球磨罐密闭 300 80 1.5:1.0 2:1 2.5:1.0 3:1 22 2.5:1.0 球磨罐密闭
分别在球磨10、14、18 h时引入空气300 80 
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