退火处理对DLC薄膜结构及摩擦学性能的影响
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摘要
目的研究退火处理对DLC薄膜结构及摩擦学性能的影响,并讨论它们之间的相互关系。方法采用平板空心阴极等离子体增强化学气相沉积系统,以C2H2和Ar作为反应气源制备DLC薄膜,将DLC薄膜在大气环境中进行不同温度的退火处理。采用扫描电子显微镜、Raman光谱仪及金相显微镜、薄膜应力测试仪及球-盘摩擦实验仪等,对退火处理前后的DLC薄膜结构、应力及摩擦学性能等进行测试分析。结果在较低温度(?≤300℃)下退火,随退火温度的增加,薄膜中sp3-C的相对含量缓慢减少,结构没有发生明显的变化,内应力降低,薄膜的摩擦系数变化趋势相同,且随退火温度的增加,摩擦系数达到平稳的趋势发生得更早。在400℃退火温度下,DLC薄膜的结构发生了明显的改变,且表面发生了一定的氧化,初始摩擦系数较高,随摩擦时间的延长,薄膜的摩擦系数降低,同时稳定后的摩擦系数(～0.16)较低温退火的DLC薄膜高。在450℃退火温度下,DLC薄膜结构发生了明显的改变,并出现了严重的氧化,摩擦学性能严重恶化并迅速失效。结论退火温度的选择对DLC薄膜的结构及摩擦学性能具有重要影响。
The work aims to study the effects of annealing treatment on the structure and tribological properties of dia-mond-like carbon thin films and discuss the inter relation. Diamond like carbon(DLC) films were deposited by plate hollowcathode plasma enhanced chemical vapor deposition method with C2 H2 and Ar as the reaction gas source. Then, the DLC thinfilms were annealed in the atmospheric environment with different temperature. The structure, stress and tribological propertiesof the DLC thin films before and after annealing were investigated and tested by scanning electron spectroscopy(SEM), Ramanspectroscopy, metalloscopy, stress analyzer and ball-on-disk tribotester. After annealing at lower temperature(?≤300 ℃), thecontent of sp3-C in the thin films slowly decreased as the annealing temperature increased and the structure of DLC films had nosignificant changes. However, the internal stress decreased and the friction coefficient firstly decreased and came to the stablestate earlier. At 400 ℃ annealing temperature, the structure of DLC thin films changed obviously and oxidation was observedon the surface. The initial friction coefficient was high and the friction coefficient of thin films decreased as the friction time ex-tended. Meanwhile, the stable friction coefficient(～0.16) was high for the DCL thin film annealed at lower temperature. At450 ℃ annealing temperature, the structure of thin films changed significantly and serious oxidation was observed. The tri-bological properties was seriously deteriorated and came to failure quickly. The annealing temperature significantly affects thestructure and tribological properties of DLC thin films.
The work aims to study the effects of annealing treatment on the structure and tribological properties of dia-mond-like carbon thin films and discuss the inter relation. Diamond like carbon(DLC) films were deposited by plate hollowcathode plasma enhanced chemical vapor deposition method with C2 H2 and Ar as the reaction gas source. Then, the DLC thinfilms were annealed in the atmospheric environment with different temperature. The structure, stress and tribological propertiesof the DLC thin films before and after annealing were investigated and tested by scanning electron spectroscopy(SEM), Ramanspectroscopy, metalloscopy, stress analyzer and ball-on-disk tribotester. After annealing at lower temperature(?≤300 ℃), thecontent of sp3-C in the thin films slowly decreased as the annealing temperature increased and the structure of DLC films had nosignificant changes. However, the internal stress decreased and the friction coefficient firstly decreased and came to the stablestate earlier. At 400 ℃ annealing temperature, the structure of DLC thin films changed obviously and oxidation was observedon the surface. The initial friction coefficient was high and the friction coefficient of thin films decreased as the friction time ex-tended. Meanwhile, the stable friction coefficient(～0.16) was high for the DCL thin film annealed at lower temperature. At450 ℃ annealing temperature, the structure of thin films changed significantly and serious oxidation was observed. The tri-bological properties was seriously deteriorated and came to failure quickly. The annealing temperature significantly affects thestructure and tribological properties of DLC thin films.
引文
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[20]DENG X,KOUSAKA H,TOKOROYAMA T,et al.Thermal stability and high-temperature tribological properties of a-C:H and Si-DLC deposited by microwave sheath voltage combination plasma[J].Tribology online,2013,8(4):257-264.
[2]TZENG S S,FANG Y L,CHIH Y K,et al.Surface characterization and nanomechanical properties of diamondlike carbon films synthesized by RF plasma enhanced chemical vapor deposition[J].Thin solid films,2011,519(15):4870-4873.
[3]YANG W J,CHOA Y H,SEKINO T,et al.Thermal stability evaluation of diamond-like nanocomposite coatings[J].Thin solid films,2003,434(1-2):49-54.
[4]CHIU M C,HSIEH W P,HO W Y,et al.Thermal stability of Cr-doped diamond-like carbon films synthesized by cathodic arc evaporation[J].Thin solid films,2005,476(2):258-263.
[5]FERRARI A C,KLEINSORGE B,MORRISON N A,et al.Stress reduction and bond stability during thermal annealing of tetrahedral amorphous carbon[J].Journal of applied physics,1999,85(10):7191-7197.
[6]HATADA R,BABA K,FLEGE S,et al.Long-term thermal stability of Si-containing diamond-like carbon films prepared by plasma source ion implantation[J].Surface&coatings technology,2016,305:93-98.
[7]HUANG L,YUAN J,LI C,et al.Influence of annealing temperature on thermal stabilities of hydrogenated amorphous carbon on silicon nitride balls[J].Vacuum,2016,127:96-102.
[8]刘正兵,周升国,吴杨敏,等.退火处理对WC-DLC薄膜结构及性能的影响[J].中国表面工程,2017,30(3):16-24.LIU Zheng-bing,ZHOU Sheng-guo,WU Yang-min,et al.Effects of annealed treatment on structure and performance of WC-DLC films[J].China surface engineering,2017,30(3):16-24.
[9]WANG J,PU J,ZHANG G,et al.Interface architecture for superthick carbon-based films toward low internal stress and ultrahigh load-bearing capacity[J].Applied materials&interfaces,2013,5(11):5015-5024.
[10]WANG J,PU J,ZHANG G,et al.Tailoring the structure and property of silicon-doped diamond-like carbon films by controlling the silicon content[J].Surface&coatings technology,2013,235(12):326-332.
[11]王永霞,冶银平,李红轩,等.退火温度对a-C:H膜结构及摩擦学性能的影响[J].无机材料学报,2011,26(2):209-213.WANG Yong-xia,YE Yin-ping,LI Hong-xuan,et al.Effect of annealing temperature on the structure and tribological property of a-C:H film[J].Journal of inorganic materials,2011,26(2):209-213.
[12]LI H,XU T,WANG C,et al.Annealing effect on the structure,mechanical and tribological properties of hydrogenated diamond-like carbon films[J].Thin solid films,2006,515:2153-2160.
[13]HE D,PU J,WANG L,et al.Investigation of post-deposition annealing effects on microstructure,mechanical and tribological properties of WC/a-C nanocomposite coatings[J].Tribology letters,2016,63(2):14.
[14]PETER S G,NTHER M,GORDAN O,et al.Experimental analysis of the thermal annealing of hard a-C:H films[J].Diamond&related materials,2014,45(5753):43-57.
[15]NAKAZAWA H,KAWABATA T,KUDO M,et al.Structural changes of diamond-like carbon films due to atomic hydrogen exposure during annealing[J].Applied surface science,2007,253(9):4188-4196.
[16]代明江,韦春贝,周克崧,等.退火温度对W-DLC薄膜结构与摩擦学性能的影响[J].真空科学与技术学报,2016,36(10):1112-1118.DAI Ming-jiang,WEI Chun-bei,ZHOU Ke-song,et al.Influence of annealing temperature on microstructures and tribological behavior of W-Doped diamond-like-carbon coatings[J].Chinese journal of vacuum science and technology,2016,36(10):1112-1118.
[17]ZHAI Z,SHEN H,CHEN J,et al.Investigation of substrate temperature and cooling method on the properties of amorphous carbon films by hot-filament CVD with acetylene[J].Carbon,2017,117(3):322-330.
[18]龚耀庭,彭先.MPCVD类金刚石膜抗氧化和摩擦性能的研究[J].表面技术,2018,47(2):136-143.GONG Yao-ting,PENG Xian.Anti-oxidation and tribology properties of MPCVD DLC films[J].Surface technology,2018,47(2):136-143.
[19]夏立芳,李光,马南.类金刚石碳膜的热稳定性[J].材料科学与工艺,2000,8(4):80-85.XIA Li-fang,LI Guang,MA Nan.Thermal stability of diamond-like carbon films[J].Material science&techology,2000,8(4):80-85.
[20]DENG X,KOUSAKA H,TOKOROYAMA T,et al.Thermal stability and high-temperature tribological properties of a-C:H and Si-DLC deposited by microwave sheath voltage combination plasma[J].Tribology online,2013,8(4):257-264.
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