基体偏压对TiN涂层微观结构、化学成分以及机械性能的影响
doi: 10.11728/cjss2025.02.2024-0142 cstr: 32142.14.cjss.2024-0142
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牟存礼 男, 1999年出生于山东省青岛市, 青岛农业大学在读硕士生, 现于中国科学院兰州物理化学研究所进行课题学习, 主要研究方向为氮化物基涂层的制备及其性能的研究. E-mail: mcl1621873878@163.com -
郝俊英 女, 现为中国科学院兰州物理化学研究所研究员, 博士生导师, 主要研究方向为固体润滑涂层及固–液复合润滑材料的研究与技术开发. E-mail: jyhao@licp.cas.cn
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Influence of Substrate Bias on the Microstructure, Chemical Composition and Mechanical Properties of TiN Coatings
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摘要: 采用高功率脉冲磁控溅射(HiPIMS)技术在9Cr18钢等基材上沉积了TiN涂层, 系统研究了不同偏压对涂层微观结构、化学成分以及机械性能的影响. 结果表明, 随着偏压的增加, TiN涂层的组织结构逐渐致密, 晶粒细化为不规则的三棱锥状, 涂层表面的致密度先增加后减少, 而截面形貌始终保持致密结构. TiN涂层的择优取向为(200)面. 涂层中Ti元素的含量在51 at%～56 at% (原子百分比)之间变化, 外观颜色稳定为紫色. 当偏压为–150 V时, 涂层的硬度最高, 约为21.2 GPa, 弹性模量约为221 GPa. 同时, 涂层还具有最大压缩残余应力, 约为2.79 GPa. 在不同偏压下, 涂层与基体之间存在较高的结合强度, 范围为49～74 N. 施加适当的负偏压可以增加基体表面受到的离子轰击能量, 促进涂层的致密化, 减少孔隙和缺陷, 提高涂层的机械性能以及涂层与基材之间的结合强度.Abstract: TiN coatings were used to deposite on 9Cr18 steel substrate by High-Power Impulsed Magnetron Sputtering (HiPIMS) technology. The influence of different substrate bias voltage on microstructure, chemical composition and mechanical properties of TiN coatings were systematically investigated. The crystal phase structure of the coatings were analyzed by X-ray diffractometer, the surface and cross-section structure and the elemental composition of the coatings were analyzed by field emission scanning electron microscopy and energy dispersive spectrometer. In addition, the hardness and elastic modulus of the coatings were measured by nanoindenter, the adhesion strength of coatings were analyzed by scratch tester and optical microscope, and the compressive residual stress of the coatings were analyzed by stress tester. The results indicate that: with the increase of substrate bias voltage, the microstructure of TiN coating gradually becomes denser, and the grains are refined into triangular pyramid shape. The density of the TiN coating surface was first increased and then decreased, while the cross-sectional morphology always maintain the dense structure. In addition, the preferred orientation of coatings were TiN (200) plane. The content of Ti element in the coatings vary between 51 at% and 56 at% and the appearance color of the coatings were stable in purple. The coating was the highest hardness, about 21.2 GPa, and the highest elastic modulus was about 221 GPa when the substrate bias voltage was -150 V. At the same time, the coating also showed the maximum compressive residual stress, approximately 2.79 GPa. Under the different structure bias voltages, the adhesion strength between the TiN coatings and the substrate were excellent, ranging from 49 N to 74 N. Applying an appropriate substrate bias can increase the energy of ion bombardment on substrate surface, promoting the densification of the coatings, reducing pores, defects and improve the mechanical properties of coatings. Besides, the appropriate substrate bias also can enhance the adhesion strength between the coatings and the substrate.
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图 2 不同基体偏压下TiN涂层GIXRD图谱
Figure 2. GIXRD patterns of TiN coatings under different substrate bias voltage
图 3 TiN涂层的表面和截面FESEM形貌
Figure 3. Surface and cross-sectional FESEM morphology of TiN coatings
图 5 不同基体偏压下TiN涂层的外观颜色
Figure 5. Appearance color of TiN coatings under different substrate bias voltage
图 7 TiN涂层的硬度和弹性模量及 H/E和H 3/E 2比值
Figure 7. Hardness and elastic modulus, H/E and H 3/E 2 ratios of TiN coatings
图 9 TiN涂层的摩擦系数、摩擦力曲线、声信号、加载力关系
Figure 9. Relationship of friction coefficient curve, friction curve, acoustic signal, and loading force of TiN coatings
图 10 本研究制备的TiN涂层与其他研究制备的氮化物涂层的硬度和结合强度对比
Figure 10. Comparison of the hardness, adhesion strength of TiN coatings with nitride coatings prepared by other research
表 1 采用HiPIMS技术在不同基体偏压下沉积TiN涂层的工艺参数
Table 1. Process parameters for depositing TiN coatings by using HiPIMS technology under different substrate bias voltage
Parameters Values Base pressure / Pa 1.0 × 10–3 Working pressure/ Pa 1.3 Bias voltage/ V –90/–120/–150/–180 Average output power/ kW 5 Peak current/A 180 Frequency/ Hz 100 Ar flow rate/ sccm 60 N2 flow rate/ sccm 60 Deposition time / h 3 
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