贾倩,张斌,赖振国,张俊彦.非晶含氢碳薄膜本征结构对退火行为的影响[J].表面技术,2022,51(7):98-106.
JIA Qian,ZHANG Bin,LAI Zhen-guo,ZHANG Jun-yan.Annealing Treatment of Hydrogenated Amorphous Carbon Film is Affected by Its Intrinsic Structure[J].Surface Technology,2022,51(7):98-106
非晶含氢碳薄膜本征结构对退火行为的影响
Annealing Treatment of Hydrogenated Amorphous Carbon Film is Affected by Its Intrinsic Structure
  
DOI:10.16490/j.cnki.issn.1001-3660.2022.07.009
中文关键词:  非晶含氢碳薄膜  退火  双极脉冲  直流脉冲  等离子体增强化学气相沉积
英文关键词:hydrogenated amorphous carbon film  annealing  bipolar pulse  DC pulse  plasma-enhanced chemical vapor deposition
基金项目:国家自然科学基金(U1737213)
作者单位
贾倩 中国科学院兰州化学物理研究所 中国科学院材料磨损与防护重点实验室,兰州 730000;中国科学院大学 材料与光电技术学院,北京 100049 
张斌 中国科学院兰州化学物理研究所 中国科学院材料磨损与防护重点实验室,兰州 730000;中国科学院大学 材料与光电技术学院,北京 100049 
赖振国 中国科学院兰州化学物理研究所 中国科学院材料磨损与防护重点实验室,兰州 730000;中国科学院大学 材料与光电技术学院,北京 100049 
张俊彦 中国科学院兰州化学物理研究所 中国科学院材料磨损与防护重点实验室,兰州 730000;中国科学院大学 材料与光电技术学院,北京 100049 
AuthorInstitution
JIA Qian Key Laboratory of Science and Technology on Wear and Protection of Materials, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China;Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China 
ZHANG Bin Key Laboratory of Science and Technology on Wear and Protection of Materials, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China;Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China 
LAI Zhen-guo Key Laboratory of Science and Technology on Wear and Protection of Materials, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China;Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China 
ZHANG Jun-yan Key Laboratory of Science and Technology on Wear and Protection of Materials, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China;Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China 
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中文摘要:
      目的 为在高温工况下服役的含氢碳(a–C:H)薄膜的制备提供新思路。方法 首先利用DP–PECVD和BiP–PECVD两种方法分别在Si基底上制备了两种本征结构不同的a–C:H薄膜,分别在350、450、550、650 ℃下进行退火处理。通过纳米硬度、X射线光电子能谱、傅里叶转变红外光谱、激光共聚焦拉曼光谱、场发射扫描电镜及CSM摩擦试验机等,分别评价了未退火和不同退火温度下两种不同结构a–C:H薄膜的结构、表面形貌、力学及摩擦学等性能。研究了不同本征结构a–C:H薄膜对退火行为的影响。结果 DP–PECVD方法在制备a–C:H薄膜(A薄膜)的过程中具有更高的沉积速率,是BiP–PECVD法(B薄膜)的1.52倍。随着退火温度的增加,两种方法制备的a–C:H薄膜均发生H脱附,但是A薄膜的脱H转变点为450 ℃,B薄膜的脱H转变点为350 ℃。DP–PECVD法制备的a–C:H薄膜在H脱附过程中更容易形成sp3–C,而BiP–PECVD法制备的a–C:H薄膜在此过程中形成sp3–C和sp2–C杂化键的概率基本相同。BiP–PECVD法制备的a–C:H薄膜在退火过程中更容易失去H,且在450 ℃以上出现大面积剥离,摩擦失效。而DP–PECVD法制备的碳薄膜则表现出更好的热和摩擦学稳定性,在350~650 ℃均可保持薄膜的完整性,并且在350~ 550 ℃退火后保持低至约0.06的摩擦因数。结论 DP–PECVD方法制备的a–C:H薄膜具有更好的热稳定性、力学稳定性及摩擦学稳定性。
英文摘要:
      Hydrogenated amorphous carbon (a-C:H) film was used in different field due to its excellent electrical, optical and tribological properties. With the evolution of the mechanic systems, the a-C:H film is required not only to have the performance of low friction coefficient, but also to meet the high temperature (≥350 ℃) service conditions. Thus, the thermal stability of the a-C:H film is the key point. The stability of a-C:H films is closely related to their inner structure, which depends on the preparation methods. So it is important to study the effects of different preparation methods on the nano structure of a-C:H films with variation of temperatures. The previous work mainly focused on the structural changes of specific a-C:H films at different annealing temperatures. However, there still lack of attention to the effect of film’s intrinsic structure on the annealing results. Thus, in this work, DC Pulsed Plasma Enhanced Chemical Vapor Deposition (PD-PECVD) and Bipolar Pulsed Plasma Enhanced Chemical Vapor Deposition (BiP-PECVD) were used to deposit two kinds of a-C:H films with different structures, then of which were annealed at 350 ℃, 450 ℃, 550 ℃ and 650 ℃, respectively. The variation of structural, mechanical properties, surface morphology and tribological properties of two kinds of a-C:H films were evaluated by appropriate testing methods. The results show that the deposition rate of a-C:H films, deposited via PD-PECVD method is 1.52 times higher than that of the BiP-PECVD method. With the increase of the annealing temperature, the a-C:H films prepared by the two methods all desorbed H but the transitional temperature point of desorption of H at 450 ℃ and 350 ℃, respectively. One can be also confirmed that the a-C:H film prepared by the PD-PECVD method is easier to form sp3-C during the H desorption process, while the a-C:H film prepared by the BiP-PECVD method has the same probability of forming sp3-C and sp2-C hybrid bonds. In addition, the a-C:H film, prepared by the BiP-PECVD method, is easier to lose H during the annealing process and peeled off in a large area beyond the annealing temperature of 450 ℃, resulting in friction failure. The a-C:H film prepared by the PD-PECVD method is unpeeled off and keep the friction coefficient as low as 0.06 when annealing at 350-550 ℃. To sum up, the film prepared by PD-PECVD method has better thermal, mechanical and tribological stability, which can work under high-temperature conditions.
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