目的 改善类金刚石碳（Diamond-like Carbon,DLC）薄膜的摩擦性能。方法 采用中频磁控溅射技术,通过调控溅射电流（1~3 A）在W18Cr4V钢基体和硅片上沉积了不同硅含量的Si-DLC薄膜。利用场发射扫描电子显微镜（SEM）、原子力显微镜（AFM）、拉曼光谱（Raman）和X射线光电子能谱（XPS）等表征手段,详细分析了薄膜的表面形貌、元素组成和化学键合状态。随后分别使用球盘式摩擦试验机和HT-1000型高温摩擦试验机,对Si-DLC薄膜在大气环境下和高温条件（100~300 ℃）下的摩擦系数和磨损率进行测试,利用光学显微镜观察Si-DLC薄膜的磨痕及对偶球磨斑形貌,评价薄膜的磨损横截面积和磨痕轮廓,并对磨痕（中间、边缘）和磨斑（对偶球中间、边缘）进行拉曼光谱和能谱分析（Energy Dispersive Spectrometer,EDS）。结果 不同溅射电流制备Si-DLC薄膜的表面均匀致密,无孔洞裂纹产生。随着溅射电流的增加,薄膜中sp³—C杂化键的比例（原子数分数）从10.12%（1 A）增至21.00%（3 A）,相应地,薄膜硬度和弹性模量分别从10.98 GPa和87.90 GPa增至13.10 GPa和104.00 GPa。适度掺Si可有效缓解薄膜内应力,降低残余应力。1.5 A制备的Si-DLC薄膜具有优异的室温摩擦性能（平均摩擦系数小于0.04）和磨损率（2.78× 10-7 mm3/(N·m)）。300 ℃下,低电流（1 A）制备的薄膜表现出优异的摩擦稳定性,平均摩擦系数仅为0.1,磨损率为4.16×10-7 mm3/(N·m);而高电流（2 A）制备的薄膜摩擦系数急剧升高,薄膜发生磨穿现象。结论 合理设置中频磁控溅射电流,可有效提升Si-DLC薄膜的室温和高温摩擦性能,较高Si含量DLC薄膜则呈现加剧磨损失效现象。
Abstract
Diamond-like carbon (DLC) films are widely recognized for their exceptional hardness, low friction and wear resistance, but their performance at elevated temperatures and under high stress remains limited due to graphitization and internal stress accumulation. To address these challenges, the work aims to systematically investigate the role of silicon (Si) doping and sputtering current modulation in enhancing the tribological properties of Si-DLC films under both ambient and high-temperature conditions. The originality of this work lies in the precise control of mid-frequency magnetron sputtering parameters to tailor the sp3—C hybridization content, Si distribution, and stress-relief mechanisms, thereby optimizing the mechanical and tribological properties of the films.
Si-DLC films were deposited on W18Cr4V steel substrates and silicon wafers through mid-frequency magnetron sputtering with varying currents (1-3 A). A Cr layer was first deposited by DC magnetron sputtering (20 min) to enhance the adhesion between the film and the substrate. Subsequently, Si-DLC films were deposited through mid-frequency pulsed magnetron sputtering (MFMS) of a silicon target in an Ar/CH4 mixed atmosphere. The microstructure and composition of the films were characterized through field-emission scanning electron microscopy (SEM), atomic force microscopy (AFM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). Surface roughness and cross-sectional morphology were analyzed to evaluate film uniformity and defect density. Mechanical properties, including hardness and elastic modulus, were measured via nanoindentation. Tribological properties were assessed with a ball-on-disc tribometer test (GCr15 steel ball counterpart, 5 N load, 0.1 m/s sliding speed) and an HT-1000 high-temperature friction tester (100-300 ℃). Wear tracks and counterpart ball scars were examined via optical microscopy to determine cross-sectional wear profiles. Raman spectroscopy and energy-dispersive spectroscopy (EDS) were conducted on the wear tracks (center/edge) and ball scars (center/edge) to analyze phase transformations and tribochemical reactions.
The Si-DLC films exhibited dense, uniform surfaces without cracks or voids. As the sputtering current increased, the sp3—C hybridization content rose from 10.12at.% (1 A) to 21.00at.% (3 A), accompanied by enhanced hardness (10.98 GPa to 13.10 GPa) and elastic modulus (87.90 GPa to 104.00 GPa). Moderate Si doping effectively relieved internal stress. The film deposited at 1.5 A demonstrated superior room-temperature tribological properties, with an average friction coefficient below 0.04 and a wear rate of 2.78×10-7 mm3/(N·m). At 300 ℃, the low-current (1 A) film maintained excellent friction stability (average coefficient: 0.1, wear rate: 4.16×10-7 mm3/(N·m)), whereas the high-current (2 A) film suffered severe wear and a sharp rise in friction. Optimizing the mid-frequency sputtering current significantly enhances the tribological properties of Si-DLC films at both room and elevated temperatures. Higher Si content promotes an abrasive wear mechanism. This study elucidates the mechanism by which sputtering current modulates the Si content and sp3—C ratio, thereby affecting the mechanical properties and tribological behavior of Si-DLC films. This work not only clarifies the interplay between Si doping and sp3—C content but also establishes a novel strategy for enhancing DLC durability in extreme environments, marking a advanced step forward in tribological coating technology. The findings provide critical theoretical insights and technical guidance for developing high-performance Si-DLC films tailored for elevated-temperature applications. The results hold significant implications for expanding the use of DLC films in high-temperature friction systems, such as aerospace components and automotive engines.
关键词
Si-DLC薄膜 /
磁控溅射 /
电流 /
机械性能 /
摩擦性能 /
磨损机制
Key words
Si-doped DLC films /
magnetron sputtering /
current /
mechanical properties /
tribological properties /
wear mechanism
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基金
国家重点研发计划（2022YFB3809000）; 甘肃省重点研发计划（22YF7GA156）; 甘肃省高校教师创新（2025A-232）; 甘肃省科技重大专项（23ZDGA01,22ZD6GA008）; 兰州理工大学红柳一流学科计划（CGZH001）
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