旋转摩擦挤压加温法制备金刚石表面Ti涂层

李毅; 于爱兵; 洪鑫; 袁建东

doi:10.13801/j.cnki.fhclxb.20210409.001

旋转摩擦挤压加温法制备金刚石表面Ti涂层

doi: 10.13801/j.cnki.fhclxb.20210409.001

宁波大学　机械工程与力学学院，宁波 315211

基金项目: 国家自然科学基金(51875294)；宁波市科技创新2025重大专项(2018B10006)

详细信息

通讯作者:
于爱兵，博士，教授，博士生导师，研究方向为切削加工技术及表面工程　E-mail：yuaibing@nbu.edu.cn

中图分类号: TB333
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出版历程
- 收稿日期: 2021-01-18
- 修回日期: 2021-03-17
- 录用日期: 2021-04-06
- 网络出版日期: 2021-04-12
- 刊出日期: 2022-01-15

Fabrication of Ti layer on diamond surface with rotary friction extrusion heating method

School of Mechanical Engineering and Mechanics, Ningbo University, Ningbo 315211, China

摘要

摘要: 为了实现金刚石表面金属化，提出了一种旋转摩擦挤压加温法在人造单晶金刚石表面制备Ti涂层。利用SEM和XRD，分析了Ti涂层内表面的微观形貌和界面间的物相组成，并采用能谱仪进行了元素分析，研究了扩散退火温度和保温时间对Ti涂层内表面物相组成的影响，并分析了金刚石/Ti涂层的界面形成机制。研究结果表明：经过旋转摩擦挤压涂覆，在金刚石表面形成了均匀、致密的Ti涂层。经过600℃保温0.5 h的扩散退火，Ti涂层内表面生成了点状的TiC晶粒，实现了金刚石与Ti涂层的化学结合。随着扩散退火温度的升高与保温时间的延长，TiC晶粒形貌由点状生长为棒状，界面TiC含量随扩散退火温度提高而增加。旋转摩擦挤压加温法在金刚石表面形成Ti涂层可分为五个阶段，即旋转摩擦挤压初始阶段、初级扩散阶段、二级扩散阶段、TiC成核阶段和TiC生长阶段。
- 旋转摩擦挤压 /
- 扩散退火 /
- 金属化 /
- 金刚石 /
- Ti /
- 涂层
Abstract: In order to realize metallization of the diamond surface, a rotary friction extrusion heating method is proposed to fabricate Ti layer on the surface of artificial single crystal diamond. The micromorphology of the inner surface of Ti layer and the phase composition of the interface between the diamond and Ti layer were analyzed with a scanning electron microscope and an X-ray diffractometer, and element analysis was carried out with an energy disperse spectrometer. The effect of diffusion annealing temperature and holding time on phase composition of the inner surface of Ti layer was studied. The formation mechanism of the diamond/Ti layer interface was analyzed. The research results show that a uniform and dense Ti layer is formed on the diamond surface after rotary friction extrusion. After diffusion annealing at 600°C for 0.5 h, dot-shaped TiC grains were formed on the inner surface of Ti layer, and the chemical combination between diamond and Ti layer was realized. With the increase of diffusion annealing temperature and holding time, the morphology of TiC grains grows from dot-shaped to rod-shaped. The mass fraction of TiC of the interface increases with the increase of diffusion annealing temperature. The formation of Ti layer on the diamond surface with rotary friction extrusion heating method can be divided into five stages: initial stage, primary diffusion stage, secondary diffusion stage, TiC nucleation stage and TiC growth stage.
- rotary friction extrusion /
- diffusion annealing /
- metallizing /
- diamond /
- Ti /
- coating

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图 1 旋转摩擦挤压过程示意图

Figure 1. Schematic diagram of rotary friction extrusion process

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图 2 金刚石Ti 涂层

Figure 2. Ti layer on diamond surface

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图 3 不同转速与挤压力下的Ti涂层厚度

Figure 3. Thickness of Ti layer at different rotational speeds and extrusion pressures

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图 4 不同温度下Ti涂层内表面的XRD图谱

Figure 4. XRD patterns of inner surface of Ti layer at different temperatures

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图 5 保温0.5 h后Ti涂层内表面的XRD图谱

Figure 5. XRD pattern of inner surface of Ti layer after holding for 0.5 h

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图 6 不同保温时间的Ti涂层内表面微观形貌

A—TiC of dot-shaped; B—Size of TiC grains increased; C—TiC of rod-shaped

Figure 6. Micromorphologies of inner surface of Ti layer under different holding time at 600℃

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图 7 金刚石与Ti的扩散过程的分子动力学模拟

Figure 7. Molecular dynamics simulation of diffusion process between diamond and Ti

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图 8 不同温度下保温2 h的Ti涂层内表面微观形貌

Figure 8. Micromorphology of inner surface of Ti layer after 2 h holding at different temperatures

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图 9 不同温度保温2 h的Ti涂层内表面TiC质量分数

Figure 9. TiC mass fraction of inner surface of Ti layer after 2 h holding at different temperatures

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图 10 金刚石Ti涂层形成过程示意图

Figure 10. Schematic diagram of formation process of Ti layer on diamond surface

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表 1 扩散退火前后Ti涂层内表面的EDS能谱分析

Table 1. EDS spectra analysis of inner surface of Ti layer before and after diffusion annealing

	Mass fraction of Ti/wt%	Mass fraction of C/wt%
Before diffusion annealing	99.03	0.97
After diffusion annealing at 500℃	93.83	6.17
After diffusion annealing at 600℃	90.66	9.34
After diffusion annealing at 700℃	88.94	11.06
After diffusion annealing at 800℃	85.20	14.80

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表 2 棒状物质的EDS能谱分析

Table 2. EDS spectra analysis of rod-shaped substance

	Mass fraction/wt%	Atomic fraction/at%
C	18.85	51.9
Ti	81.15	48.1

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表 3 旋转摩擦挤压加温法与一些常见金刚石表面金属化方法对比

Table 3. A comparison between the rotary friction extrusion heating method and some common diamond surface metallization methods

Metallization method	Electroless plating and electroplating method	Physical vapor deposition (PVD)	Chemical vapor deposition (CVD)	Salt bath method and powder coating sintering method	Vacuum micro- evaporation plating method	Rotary friction extrusion heating method
Coating composition	Ni or Ni-W, Ni-Co alloy	Ti, Mo, W, Cr	Ti, Mo, W, Cr and corresponding carbide	Ti, Mo, etc. and corresponding carbides	Ti, Mo, etc. and corresponding carbides	Ti, TiC
Combination forms	Physical	Physical	Chemical	Chemical	Chemical	Chemical
Bond strength	Low	Low	High	High	High	High
Plating temperature	<373 K	<673 K	>1123 K	1123-1373 K	973-1093 K	>873 K
Process cost	High	High	High	High, Medium	High	Low
Environmental pollution	High	Low	Medium	High, Medium	Medium	Low
Technical difficulty	High	High	High	High, Medium	High	Low
Diamond thermal damage	No	No	Severe	Severe	No	No

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