Si<sub>3</sub>N<sub>4</sub>基底表面粗糙度对HFCVD法制备金刚石薄膜摩擦学性能的影响

王贺; 温凯翔; 闫广宇; 王延祥; 靳一帆; SU Peichen

doi:10.13394/j.cnki.jgszz.2022.0184

Si₃N₄基底表面粗糙度对HFCVD法制备金刚石薄膜摩擦学性能的影响

doi: 10.13394/j.cnki.jgszz.2022.0184

王贺^{1, 2, 3,},
温凯翔¹,
闫广宇^{1, 2, 3, ,},
王延祥¹,
靳一帆¹,
SU Peichen⁴

1.
沈阳建筑大学机械工程学院, 沈阳 110000
2.
沈阳建筑大学现代建筑工程装备与技术国际合作联合实验室, 沈阳 110000
3.
沈阳建筑大学高档石材数控加工装备与技术国家地方联合工程实验室, 沈阳 110000
4.
南洋理工大学机械与宇航工程学院, 新加坡 639798

基金项目: 国家自然科学基金（51942507）；学科创新引智项目（D18017）；耐磨及功能薄膜制备与应用研究（G2022006012L）；陶瓷轴承材料基体复合涂层制备及其性能研究（2022JH2/101300234）；中央军委科学技术委员会项目（20-163-00-TS-006-002-11）。

详细信息

作者简介:
王贺，男，1981年生，博士，副教授。主要研究方向：陶瓷零件制备及加工技术。E-mail：wanghe9095@163.com

通讯作者:
闫广宇，男，1991年生，讲师。主要研究方向：功能薄膜制备技术。E-mail：ygy0813@sjzu.edu.cn

中图分类号: TQ164；TQ174.1+2
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出版历程
- 收稿日期: 2022-11-03
- 修回日期: 2022-11-26
- 录用日期: 2022-12-08
- 网络出版日期: 2023-12-07
- 刊出日期: 2023-10-20

Effect of Si₃N₄ substrate surface roughness on the wear resistance of diamond film prepared by HFCVD

WANG He^{1, 2, 3
,},
WEN Kaixiang¹,
YAN Guangyu^{1, 2, 3
, ,},
WANG Yanxiang¹,
JIN Yifan¹,
SU Peichen⁴

1.
Shenyang Jianzhu University, School of Mechanical Engineering, Shenyang 110000, China
2.
Shenyang Jianzhu University, Joint International Research Laboratory of Modern Construction Engineering Equipment and Technology, Shenyang 110000, China
3.
Shenyang Jianzhu University, National Local Joint Engineering Laboratory of High-grade Stone CNC Processing Equipment and Technology, Shenyang 110000, China
4.
Nanyang Technological University, School of Mechanical and Aerospace Engineering, Singapore 639798

摘要

摘要:
采用热丝化学气相沉积法（hot filament chemical vapour deposition，HFCVD）在不同表面粗糙度的Si₃N₄基底表面制备金刚石薄膜，并对薄膜的特性进行检测与分析。利用场发射电子扫描显微镜、原子力显微镜检测植晶后的Si₃N₄基底表面以及制备的金刚石薄膜表面形貌；利用多功能摩擦磨损实验机、探针式轮廓仪，在干摩擦条件下，测试金刚石薄膜的摩擦系数及磨损率。综合基底粗糙度对植晶质量的影响、金刚石薄膜表面形貌与摩擦磨损检测实验结果，确定了Si₃N₄基底表面粗糙度对金刚石薄膜耐磨性的影响。结果表明：基底表面粗糙度会影响植晶的均匀性及致密性，进而影响金刚石颗粒在基底表面的生长，同时基底的表面形貌也会复映在金刚石薄膜表面。表面粗糙度为0.15 μm和0.20 μm的基底所制备的金刚石薄膜拥有较好的耐磨性，可得到最低的磨损率1.75 × 10⁻⁷ mm³/（m·N）和最低的摩擦系数0.078。
- 氮化硅 /
- 表面粗糙度 /
- 热丝化学气相沉积 /
- 金刚石薄膜 /
- 耐磨性
Abstract:
[OBJECTIVES] Silicon nitride engineering ceramic materials are widely used in microelectronics and wear-resistant components due to their excellent physicochemical properties and mechanical stability under severe working conditions. However, silicon nitride ceramics suffer from brittleness, poor plastic deformation, and a tendency for brittle fracture, which limits their reliability in components for reducing wear and enhancing resistance. With the development of CVD technology, diamond-coated silicon nitride materials show great potential for wide application. Research indicates that the substrate surface roughness affects the properties of diamond films. In this study, diamond films were prepared by HFCVD with silicon nitride ceramic substrates of varying roughness to investigate the effect of substrate surface roughness on the tribological properties of diamond films.
[METHODS] The silicon nitride ceramic substrates were ground to various surface roughness levels using diamond grinding pastes of different grain sizes. After pretreatment by ultrasonic cleaning, a diamond suspension was used for crystal seeding on the surface to increase the nucleation density of diamonds. Thin film deposition was then carried out on the surface of the processed silicon nitride ceramic substrate using parameters of 1% methane concentration, 1KPa chamber pressure, and a substrate temperature of 2500±10 ℃. This process yielded micrometer-scale diamond thin films (MCD) on the surface of the silicon nitride ceramic substrate with different surface roughness. The surface morphology was characterized using a scanning electron microscope and an atomic force microscope. The quality and rate of grain growth in the diamond films on substrates of different roughness were analyzed to assess the influence of surface roughness on film growth. The physical phase composition of diamond films on substrates with varying roughness was characterized by Raman spectrometer. The bond strength between the diamond films and the silicon nitride ceramic substrates with different roughness was characterized by using an Anton Paar scratch meter microscopic combination viewer (MCT3) and an ultra-deep field microscope. The critical loads Lc1 and Lc2—corresponding to the onset of semicircular cracks within the film scratches and the appearance of adhesion failure-type debris at the scratch edges, respectively—were determined through acoustic emission, load-friction curves, and examination of the scratch surface morphology. This analysis also explored the fracture mechanisms of the films and the effect of substrate surface roughness on the film-substrate bonding strength. Tribological properties of the diamond films were investigated using a "ball-on-disk" reciprocating friction and wear tester, with silicon nitride ceramic balls as the counter-body. Scanning electron microscope (SEM), probe-type surface profiler (PSP) and super depth-of-field microscope (DFM) were used to examine the diamond films after abrasion.
[RESULTS] The results showed that: (1) diamond films exhibited the highest growth rate of 0.647 μm/h on substrates with surface roughness of 0.15 μm and 0.20 μm. The density and dimensional homogeneity of diamond grains decreased with the increase of substrate surface roughness due to the influence of the quality of crystallization, and the surface roughness of the diamond films increased with the grain sizes and the substrate roughness. The content of diamond phases in the films gradually increased and the content of trans-polyacetylene and graphite gradually decreased with the increase of substrate surface roughness, particularly notable on substrates with 0.30 μm roughness, where diamond films showed the highest diamond phase content and the least graphite phase, impurities, and grain defects. (2) Diamond films on the substrate with surface roughness of 0.20 μm could withstand the highest load, with critical loads Lc1 and Lc2 being 9.4 N and 11.9 N, respectively.(3) The friction coefficient of diamond film correlated with the roughness of the substrate, the size of the grains and the content of the impurities, with the lowest coefficient of 0.078 observed on substrates with 0.20 μm roughness. The wear rate of diamond films aligned with that of the counter-abrasive, with insufficient film-substrate bonding leading to film detachment and increased wear. High-quality grains and strong film-substrate bonding yielded low wear rates for both diamond films and counter-abrasives, with the lowest wear rate on substrates with 0.20 μm roughness being 1.75x10-7mm3/(m N).
[CONCLUSION] This study shows that the tribological properties of diamond films initially improve and then decline with increasing substrate surface roughness. Notably, micrometer-scale diamond films grown on substrates with a surface roughness of 0.10 to 0.20 μm exhibit superior growth quality and tribological performance.
- Si₃N₄ /
- surface roughness /
- hot filament chemical vapour deposition （HFCVD） /
- diamond films /
- wear resistance

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图 1 基底植晶后表面形貌

Figure 1. Surface morphology of the substrate after crystal implantation

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图 2 金刚石薄膜截面

Figure 2. Diamond film cross-sectional view

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图 3 金刚石薄膜表面形貌

Figure 3. Diamond film surface morphology

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图 4 金刚石薄膜三维形貌

Figure 4. 3D morphology of the diamond film

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图 5 金刚石薄膜摩擦系数

Figure 5. Friction coefficients of diamond films

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图 6 金刚石薄膜磨损后形貌

Figure 6. Diamond film morphology after wear

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图 7 金刚石薄膜磨痕曲线

Figure 7. Diamond film abrasion curves

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