Ti/Ti-类金刚石多层膜的制备与表征

黄江涛; 谷坤明; 毛斐; 虞烈; 汤皎宁

doi:10.7498/aps.61.088102

摘要

采用电子回旋共振-化学气相沉积结合中频磁控溅射的真空镀膜技术, 以99.99%Ti为靶材, 乙炔为碳源制备了Ti/Ti-类金刚石(DLC)多层膜. 利用X射线衍射仪、扫描电子显微镜、X射线光电子能谱仪对Ti/Ti-DLC多层膜进行了相结构、组织、成分及形态分析. 采用显微硬度仪、摩擦磨损仪、表面粗糙度仪对Ti/Ti-DLC多层膜进行了力学性能考察. 结果表明: Ti/Ti-DLC多层膜中主要含有TiC晶相; Ti层和Ti-DLC层中未出现柱状晶体生长模式, 分层中均以岛状模式生长; 当调制周期 50 nm时, 分层结构变模糊; 调制周期对Ti/Ti-DLC多层膜的复合硬度、摩擦系数、表面形貌、表面粗糙度都有影响, 当调制周期较小时表现出纳米增硬效应, 表面出现大颗粒, 表面粗糙度和摩擦系数均变大.

关键词:

Abstract

The titanium/titanium diamond-like carbon (Ti/Ti-DLC) multi-layered films are deposited by combined electron cyclotron resonance microwave plasma enhanced chemical vapor deposition method and mid-frequency magnetron sputtering method using acetylene as the reactive gas and Ti target with a purity of 99.99%. The structures, compositions and surface morphologies of the samples are characterized by X-ray diffraction, scanning electron microscope, and X-ray photoelectron spectrometer. The mechanical properties of Ti/Ti-DLC multilayer films are investigated by microhardness tester, friction wear test instrument and surface roughmeter. The results show that TiC phase appears in multilayered film. The main growth mode of the film is island mode and there exists columnar crystal structure neither in Ti layer nor Ti-DLC layer. The properties of the multi-layered film, including composite hardness, friction coefficient, surface morphology and surface roughness are affected by the modulation period . It is shown that nano-hardening effect takes place when is small while large particles appear on the surface of the film, leading to a large surface roughness and friction coefficient. The layered structure of the film is not clear when 50 nm.

Keywords:

Ti/Ti-diamond-like carbon multilayered films /
electron cyclotron resonance-chemical vapor deposition /
modulation cycle

作者及机构信息

1.
深圳大学材料学院, 深圳市特种功能材料重点实验室, 深圳 518060;

2.
西安交通大学机械工程学院, 西安 710049

基金项目: 国家高技术研究发展计划(批准号: 2007AA050501)、广东省科技计划(批准号: 2009B010900035)和深圳市科技计划(批准号: JC200903130309A)资助的课题.

Authors and contacts

1.
Key Laboratory of Special Functional Materials of Shenzhen, School of Materials, Shenzhen University, Shenzhen 518060, China;

2.
College of Mechanical Engineering, Xi'an Jiaotong University, Xi'an 710049, China

Funds: Project supported by the National High Technology Research and Development Program of China (Grant No. 2007AA050501), the Science and Technology Program of Guangdong Province, China (Grant No. 2009B010900035), and the Science and Technology Program of Shenzhen, China (Grant No. JC200903130309A).

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[25]	Li G, Xia L F 2001 Thin Solid Films 396 16
[26]	Schroeder A, Francz G, Bruinink A, Hauert R, Mayer J, Wintermantel E 2000 Biomaterials 21 449
[27]	Chen X C, Peng Z J, Fu Z Q, Wang C B 2010 China Surf. Eng. 23 36 (in Chinese) [陈新春, 彭志坚, 付志强, 王成彪 2010 中国表面工程 23 36]
[28]	Wang J G, Ma G J, Deng X L, Li X, Tang Z A 2003 Vac. Sci. Technol. 23 429 (in Chinese) [王金刚, 马国佳, 邓新绿, 李新, 唐祯安 2003 真空科学与技术 23 429]
[29]	Li F J, Zhang S, Kong J H, Zhang Y J, Zhang W L 2011 Thin Solid Films 519 4910
[30]	Jao J Y, Han S, Yen C C, Liu Y C, Chang L S, Chang C L, Shih H C 2011 Diam. Relat. Mater. 20 123
[31]	Kong M, Yue J L, Li G Y 2010 J. Inorg. Mater. 25 113 (in Chinese) [孔明, 岳建岭, 李戈扬 2010 无机材料学报 25 113]
[32]	Zhao D C, Xiao G J, Ren N, Ma Z J, Wu S H 2008 Vac. Cryog. 14 27 (in Chinese) [赵栋才, 肖更竭, 任妮, 马占吉, 武生虎 2008 真空与低温 14 27]
[33]	Xie H M 2011 Surf. Technol. 40 90 (in Chinese) [谢红梅 2011 表面技术 40 90]
[34]	Wang P J, Jiang M F, Du J L, Dai Y F 2010 Acta Phys. Sin. 59 8920 (in Chinese) [王培君, 江美福, 杜记龙, 戴永丰 2010 物理学报 59 8920]

施引文献

[1]	Xie Z W 2007 M. S. Dissertation (Harbin: Harbin Institute of Technology) (in Chinese) [解志文 2007 硕士学位论文 (哈尔滨: 哈尔滨工业大学)]
[2]	Xiao X L, Zhang X, Li F Q, Hou H J, Lin S S 2010 Chin. J. Vac. Sci. Technol. 30 690 (in Chinese) [肖晓玲, 张馨, 李福球, 侯惠君, 林松盛 2010 真空科学与技术学报 30 690]
[3]	Li G Y, Xu J H, Gu M Y 2001 J. Shanghai Jiaotong Univ. 35 457 (in Chinese) [李戈扬, 许俊华, 顾明元 2001 上海交通大学学报 35 457]
[4]	Tao S W, Lei N, Qu X H 2005 Dev. Nano-hard Thin Film 33 37 (in Chinese) [陶斯武, 雷诺, 曲选辉 2005 稀有金属与硬质合金 33 37]
[5]	Warcholinski B, Gilewicz A 2011 Wear 271 2812
[6]	Yang W B, Fan S H, Zhang G L, Ma P N, Zhang S Z, Du J 2005 Acta Phys. Sin. 54 4944 (in Chinese) [杨武保, 范松华, 张谷令, 马培宁, 张守忠, 杜健 2005 物理学报 54 4944]
[7]	Yoshihiko U, Toshifumi K, Takema T, Yoshio H, Keiro T 2011 Surf. Coat. Technol. 205 2778
[8]	Robertson J 2002 Mater. Sci. Eng. R37 129
[9]	Ji L, Li H X, Zhao F, Quan W L, Chen J M, Zhou H D 2009 Appl. Surf. Sci. 255 4180
[10]	Tobi Mohd A L, Shipway P H, Leen S B 2011 Wear 271 1572
[11]	Lin Y H, Lin H D, Liu C K, Huang M W, Chen J R, Shih H C 2010 Diam. Relat. Mater. 19 1034
[12]	Bolelli G, Bonferroni B, Coletta G, Lusvarghi L, Pitacco F 2011 Surf. Coat. Technol. 205 4211
[13]	Bertran E, Corbella C, Pinyol A, Vives M, Andujar J L 2003 Diam. Relat. Mater. 12 1008
[14]	Ziegele H, Scheibe H J, Schultrich B 1997 Surf. Coat. Technol. 97 385
[15]	Qi Z Q, Meletis E I 2005 Thin Solid Films 479 174
[16]	Delplancke-Ogletree M P, Monteiro O R 1998 Surf. Coat. Technol. 108---109 484
[17]	Lin S S, Dai M J, Li H W, Zhu X G, Hou H J, Lin K S 2007 Chinese Patent 200710028834 (in Chinese) [林松盛, 代明江, 李洪武, 朱霞高, 侯惠君, 林凯生 2007 中国专利 200710028834]
[18]	Rao J, Cruz R, Lawson K J, Nicholls J R 2005 Diam. Relat. Mater. 14 1805
[19]	Ma G J, Liu X L, Zhang H F, Wu H C, Peng L P, Jiang Y L 2007 Acta Phys. Sin. 56 2377 (in Chinese) [马国佳, 刘喜亮, 张华芳, 武洪臣, 彭丽平, 蒋艳莉 2007 物理学报 56 2377]
[20]	Wu P, Jiang E Y, Liu Y G, Wang C D 1996 Acta Metall. Sin. 32 1209 (in Chinese) [吴萍, 姜恩永, 刘裕光, 王存达 1996 金属学报 32 1209]
[21]	Lin S S, Dai M J, Hou H J, Li H W, Zhu X G, Lin K S 2007 Chin. J. Vac. Sci. Technol. 27 418 (in Chinese) [林松盛, 代明江, 侯惠君, 李洪武, 朱霞高, 林凯生 2007 真空科学与技术学报 27 418]
[22]	Lü S G 2010 M. S. Dissertation (Dalian: Dalian University of Technology) (in Chinese) [吕世功 2010 硕士学位论文 (大连: 大连理工大学)]
[23]	Li L H, Zhang H Q, Cui X M, Zhang Y H 2001 Acta Phys. Sin. 50 1549 (in Chinese) [李刘合, 张海泉, 崔旭明, 张彦华 2001 物理学报 50 1549]
[24]	Ma G J, Zhang X N, Wu H C, Zhang H F, Peng L P 2008 Rare Met. Mater. Eng. 37 1614 (in Chinese) [马国佳, 张晓囡, 武洪臣, 张华芳, 彭丽平 2008 稀有金属材料与工程 37 1614]
[25]	Li G, Xia L F 2001 Thin Solid Films 396 16
[26]	Schroeder A, Francz G, Bruinink A, Hauert R, Mayer J, Wintermantel E 2000 Biomaterials 21 449
[27]	Chen X C, Peng Z J, Fu Z Q, Wang C B 2010 China Surf. Eng. 23 36 (in Chinese) [陈新春, 彭志坚, 付志强, 王成彪 2010 中国表面工程 23 36]
[28]	Wang J G, Ma G J, Deng X L, Li X, Tang Z A 2003 Vac. Sci. Technol. 23 429 (in Chinese) [王金刚, 马国佳, 邓新绿, 李新, 唐祯安 2003 真空科学与技术 23 429]
[29]	Li F J, Zhang S, Kong J H, Zhang Y J, Zhang W L 2011 Thin Solid Films 519 4910
[30]	Jao J Y, Han S, Yen C C, Liu Y C, Chang L S, Chang C L, Shih H C 2011 Diam. Relat. Mater. 20 123
[31]	Kong M, Yue J L, Li G Y 2010 J. Inorg. Mater. 25 113 (in Chinese) [孔明, 岳建岭, 李戈扬 2010 无机材料学报 25 113]
[32]	Zhao D C, Xiao G J, Ren N, Ma Z J, Wu S H 2008 Vac. Cryog. 14 27 (in Chinese) [赵栋才, 肖更竭, 任妮, 马占吉, 武生虎 2008 真空与低温 14 27]
[33]	Xie H M 2011 Surf. Technol. 40 90 (in Chinese) [谢红梅 2011 表面技术 40 90]
[34]	Wang P J, Jiang M F, Du J L, Dai Y F 2010 Acta Phys. Sin. 59 8920 (in Chinese) [王培君, 江美福, 杜记龙, 戴永丰 2010 物理学报 59 8920]

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