不同气氛热冲击下Al:WS<sub>2</sub>薄膜摩擦学性能的响应机理

刘建; 剡珍; 郝俊英; 刘维民

doi:10.11728/cjss2023.05.2022-0037

不同气氛热冲击下Al:WS₂薄膜摩擦学性能的响应机理

doi: 10.11728/cjss2023.05.2022-0037 cstr: 32142.14.cjss2023.05.2022-0037

刘建^{1, 2, 3,},
剡珍^{1, 3},
郝俊英^{1, 3, ,},
刘维民¹

1.
中国科学院兰州化学物理研究所固体润滑国家重点实验室　兰州　730000
2.
中国科学院大学　北京　100049
3.
青岛市资源化学与新材料研究中心　青岛　266000

基金项目: 国家自然科学基金项目（51835012，51975554），甘肃省自然科学基金项目（21JR7RA093）和青年人才托举工程项目共同资助

详细信息

作者简介:

刘建：E-mail：jliu@licp.cas.cn

通讯作者:

郝俊英，E-mail：jyhao@licp.cas.cn

中图分类号: V519.11
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出版历程
- 收稿日期: 2022-08-07
- 录用日期: 2023-06-25
- 修回日期: 2022-11-30
- 网络出版日期: 2023-06-25

Response Mechanism of Tribological Properties of Al:WS₂ Film under Different Ambient Thermal Shock

LIU Jian^{1, 2, 3
,},
YAN Zhen^{1, 3},
HAO Junying^{1, 3
, ,},
LIU Weimin¹

1.
State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000
2.
University of Chinese Academy of Sciences, Beijing 100049
3.
Qingdao Center of Resource Chemistry and New Materials, Qingdao 266000

摘要

摘要: 采用磁控溅射技术制备了Al:WS₂薄膜。为考查不同气氛热冲击下Al:WS₂薄膜摩擦学性能的响应机理，采用自行研制的温度交变真空摩擦试验机开展了真空、氮气及氧气气氛的–100～+250℃的热冲击试验，并对热冲击后Al:WS₂薄膜结构、成分以及摩擦学性能进行了研究。研究发现，热冲击后，Al:WS₂薄膜柱状晶长大，S含量减少，部分WS₂被氧化为WO₃，薄膜硬度增加。经氮气热冲击后，薄膜的（002）衍射峰强度明显增强，使得摩擦系数降低。经真空热冲击后，在薄膜表面形成的WO₃起到磨粒磨损作用，减少了薄膜寿命；经氧气热冲击后，Al:WS₂薄膜中大量起润滑作用的WS₂被氧化为WO₃，薄膜的寿命显著缩短。
- Al:WS₂薄膜 /
- 热冲击 /
- 气氛 /
- 摩擦
Abstract: Al:WS₂ films were prepared by magnetron sputtering technology. In order to investigate the response mechanism of the tribological properties of Al:WS₂ film under different ambient thermal shock, the thermal shock tests of –100～+250℃ in vacuum, nitrogen and oxygen were carried out using the temperature altering vacuum tribometer developed, and the structure, composition and tribological properties of Al:WS₂ films after thermal shock were mainly studied. It was found that the columnar crystal of Al:WS₂ film grows, S content decreases, part of WS₂ is oxidized to WO₃, and the hardness of film increases after thermal shock. After thermal shock under nitrogen atmosphere, the intensity of (002) diffraction peak of Al:WS₂ film is obviously enhanced, and the friction coefficient decreased. After thermal shock with vacuum, WO₃ appears on the surface of Al:WS₂ film plays the role of abrasive wear, which reduces the life of film. After oxygen thermal shock, a large number of WS₂ is oxidized to WO₃, and the wear life of the film is significantly shortened due to the serious abrasive wear.
- Al:WS₂ film /
- Thermal shock /
- Atmosphere /
- Friction

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图 1 未处理及经热冲击的Al:WS₂薄膜表面与断面形貌

Figure 1. FESEM morphologies of surface and cross-section of untreated and thermal shocked Al:WS₂ films

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图 2 未处理与热冲击Al:WS₂薄膜的GIXRD谱

Figure 2. GIXRD patterns of untreated and thermal shocked Al:WS₂ films

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图 3 未处理及不同气氛热冲击后Al:WS₂薄膜的硬度

Figure 3. Hardness of untreated and thermal shocked Al:WS₂ films

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图 4 未处理及不同气氛热冲击后Al:WS₂薄膜的XPS全谱、W 4f和W 5s高分辨谱

Figure 4. Survey, fitted high-resolution W 4f and W 5s XPS spectra of untreated and thermal shocked Al:WS₂ films

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图 5 未处理及不同气氛热冲击后Al:WS₂薄膜的真空摩擦曲线

Figure 5. Friction curves of untreated and thermal shocked Al:WS₂ films

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图 6 未处理及不同气氛热冲击后Al:WS₂薄膜的 3D形貌

Figure 6. 3D profiles of wear tracks of untreated and thermal shocked Al:WS₂ films

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图 7 计算未处理及不同气氛热冲击后Al:WS₂薄膜的磨损率

Figure 7. Calculated wear rates of untreated and thermal shocked Al:WS₂ films

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图 8 未处理及不同气氛热冲击后Al:WS₂薄膜的磨痕与对偶球磨斑形貌的SEM

Figure 8. SEM micrographs of wear track and wear scar of untreated and thermal shocked Al:WS₂ films

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表 1 磁控溅射沉积Al:WS₂薄膜的工艺参数

Table 1. Deposition parameter of Al:WS₂ film by magnetron sputtering system

Deposition parameters	Values
WS₂ target power/W	600
Al target current/A	0.15
Working pressure/Pa	6.0×10^–3
Bias voltage/V	–20
Ar flow/(mL·min^–1)	70
Substrate rotation speed/(r·min^–1)	1
Deposition time/min	150

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表 2 由XPS计算得到的未处理及不同气氛热冲击后Al:WS₂薄膜的相对元素含量（原子百分数）

Table 2. Calculated element content (atom percent) of untreated and thermal shocked Al:WS₂ films

Specimen	W	S	Al	C	O
Al:WS₂	12.43	19.71	0.92	44.54	22.40
Vacuum	7.73	9.85	1.31	61.86	19.25
N₂	10.42	13.51	0.53	54.54	21.00
O₂	9.43	4.85	0	49.88	35.84

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表 3 未处理及不同气氛热冲击后Al:WS₂薄膜的 W 4f XPS拟合数据

Table 3. Fitted W 4f XPS data of untreated and thermal shocked Al:WS₂ films

Specimen	W 4f
Specimen	WS₂ (atom percent)	WO₃ (atom percent)
Al:WS₂	66.72	33.28
Vacuum	62.91	37.09
N₂	59.56	40.44
O₂	27.14	72.86

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表 4 未处理及不同气氛热冲击后Al:WS₂薄膜的磨斑转移膜EDS元素成分分析（原子百分数）

Table 4. Element content (atom percent) from EDS analysis of transfer films on wear scars of untreated and thermal shocked Al:WS₂ films

Specimen	Al	W	S	C	O	Fe
Al:WS₂	0.2	6.3	5.9	5.5	15.4	66.6
Vacuum	0.1	0.9	0.3	5.0	10.4	83.3
N₂	0.2	21.1	19.0	8.0	24.6	27.0

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