许浩杰,陈仁德,周广学,叶羽敏,汪爱英.工作气压对管内壁沉积Si/O-DLC薄膜结构与性能的影响[J].表面技术,2023,52(6):439-499.
XU Hao-jie,CHEN Ren-de,ZHOU Guang-xue,YE Yu-min,WANG Ai-ying.#$NP Effect of Working Pressure on Structure and Properties of Si/O-DLC Films Deposited on Inner Wall of the Tube[J].Surface Technology,2023,52(6):439-499 |
| 工作气压对管内壁沉积Si/O-DLC薄膜结构与性能的影响 |
| #$NP Effect of Working Pressure on Structure and Properties of Si/O-DLC Films Deposited on Inner Wall of the Tube |
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| DOI：10.16490/j.cnki.issn.1001-3660.2023.06.041 |
| 中文关键词: 工作气压 空心阴极等离子体增强化学气相沉积 管内壁 Si/O-DLC 等离子体放电光学现象 均匀性 |
| 英文关键词:working pressure HC-PECVD inner wall of tube Si/O-DLC plasma discharge optical phenomena uniformity |
| 基金项目:中国科学院-韩国国家科技理事会协议项目(174433KYSB20200021);王宽城率先人才计划卢嘉锡国际团队(GJTD-2019-13);中科院创新团队(292020000008) |
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| Author | Institution |
| XU Hao-jie | Faculty of Materials Science and Chemical Engineering, Ningbo University, Zhejiang Ningbo 315211, China;Key Laboratory of Marine Materials and Related Technologies,Zhejiang Key Laboratory of Marine Materials and Protective Technologies, Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Zhejiang Ningbo 315201, China |
| CHEN Ren-de | Key Laboratory of Marine Materials and Related Technologies,Zhejiang Key Laboratory of Marine Materials and Protective Technologies, Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Zhejiang Ningbo 315201, China |
| ZHOU Guang-xue | Key Laboratory of Marine Materials and Related Technologies,Zhejiang Key Laboratory of Marine Materials and Protective Technologies, Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Zhejiang Ningbo 315201, China |
| YE Yu-min | Faculty of Materials Science and Chemical Engineering, Ningbo University, Zhejiang Ningbo 315211, China |
| WANG Ai-ying | Key Laboratory of Marine Materials and Related Technologies,Zhejiang Key Laboratory of Marine Materials and Protective Technologies, Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Zhejiang Ningbo 315201, China |
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| 中文摘要: |
| 目的 探讨工作气压对管内等离子体放电光学现象以及Si/O-DLC(Si and O Incorporated DLC，Si/O-DLC)薄膜结构与性能的影响，为获得管内高质量、均匀的Si/O-DLC薄膜制备工艺技术提供指导。方法 利用空心阴极等离子体增强化学气相沉积(Hollow Cathode Plasma Enhanced Chemical Vapor Deposition，HC-PECVD)技术，通过改变工作气压在管内沉积Si/O-DLC薄膜。利用高速摄像机记录并对比不同工作气压下管内等离子体放电光学现象。通过SPM、XPS和Raman光谱仪表征不同工作气压下薄膜的三维立体表面形貌和微观结构，并利用SEM、纳米压痕仪以及划痕测试系统，对比研究管内Si/O-DLC薄膜的硬度、弹性模量、膜基结合力以及沿管轴向的薄膜厚度分布。结果 随着工作气压的上升，管径向中心处亮斑面积和光强先增大增强后趋于缩小暗淡。在不同工作气压下，均能够在管内获得表面光滑的Si/O-DLC薄膜，粗糙度为3~10 nm。随着工作气压的上升，管内Si/O-DLC薄膜的平均厚度从1.42 μm增大到2.06 μm，且沿管轴向的薄膜厚度分布均匀度从24%显著提高到65%;不同工作气压下管内Si/O-DLC薄膜沿管轴向平均硬度呈先增大后减小的趋势，总体平均硬度可达(14±1) GPa。管内Si/O-DLC薄膜在工作气压上升到25 mTorr时获得较高的平均膜基结合力。结论 改变工作气压能够显著影响管内壁Si/O-DLC薄膜的结构与性能，当工作气压为25 mTorr时，在管内获得均匀性最优、结合力较高的Si/O-DLC薄膜。 |
| 英文摘要: |
| Metal tubes are widely used in important fields such as national defense and military, aerospace, petrochemical, and marine engineering equipment including rocket engine propellant refueling systems, oil and gas transportation pipelines, and plunger sets of deep-sea sea pumps, which play an important role in guaranteeing national security and industrial development. However, in harsh environments, the inner walls of tube fittings often face serious damage such as corrosion, scratching and abrasion, which not only leads to shortened service life, but also brings huge economic losses. The design and preparation of multifunctional protective coatings with smooth and dense surface, high hardness, and strong film-based bonding inside the tube has become an urgent need. A stainless steel tube with a length of 300 mm, an outer diameter of 105 mm, and an inner diameter of 100 mm was used as the substrate, and polished and cleaned in turn. Seven locations 5, ‒5, 10, ‒10, 15 and ‒15 cm from the middle of the tube were selected to characterize the structural and mechanical properties of the 304 stainless steel tube coated with Si/O-DLC film inside the tube. Different working pressures (15 mTorr, 20 mTorr and 25 mTorr) were changed to explore the effects on the plasma glow discharge in the tube and the structure and properties of the thin film. Firstly, a high-speed camera (Photron fastcam MiNi 100, Photron Co, Japan) was used to observe Plasma discharge optical phenomena. Secondly, scanning electron microscope and atomic force microscope were used to observe the surface morphology and roughness of the thin film and measure the thickness of the thin film. Then, the microstructure and mechanical properties of the film in the tube were analyzed by Raman spectroscopy, nanoindenter, and scratch testing system. With the increase of the working pressure, the bright spot area and light intensity at the center of the tube diameter firstly increased and then tended to shrink and fade. The average thickness of Si/O-DLC films in the tube increased from 1.42 μm to 2.06 μm with the increase of working pressure, and the uniformity of film thickness along the axial direction of the tube increased significantly from 24% to 65%; and the average hardness of Si/O-DLC films in the tube at different working pressure increased firstly and then decreased. The average hardness of inside Si/O-DLC films of the tube tended to increase and then decrease along the axial direction of the tube at different working pressure, with an overall average hardness of (14±1) GPa. The inside Si/O-DLC films of the tube obtained a high average film-base bonding at working pressure up to 25 mTorr. The distribution of the thickness and roughness of the Si/O-DLC film along the axial direction of the tube has the best uniformity at 25 mTorr. As the working pressure rises, the average thickness of the film on the inner wall of the tube along the tube axis increases, and the uniformity is improved. The overall roughness value of the surface morphology of the film in the tube is small and varies in a small range. In general, the roughness distribution of the film in the tube under different working pressure is relatively uniform, and the film and the substrate are closely bonded without microscopic defects. |
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