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退火对B掺杂纳米金刚石薄膜微结构和电化学性能的影响

潘金平 胡晓君 陆利平 印迟

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退火对B掺杂纳米金刚石薄膜微结构和电化学性能的影响

潘金平, 胡晓君, 陆利平, 印迟

Influence of annealing on the microstructure and electrochemical properties of B-doped nanocrystalline diamond films

Pan Jin-Ping, Hu Xiao-Jun, Lu Li-Ping, Yin Chi
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  • 采用热丝化学气相沉积法制备B掺杂纳米金刚石薄膜,并对薄膜进行真空退火处理,系统研究了不同退火温度对B掺杂纳米金刚石薄膜的微结构和电化学性能的影响.结果表明,当退火温度升高到800 ℃后,薄膜的Raman谱图中由未退火时在1157,1346,1470,1555 cm-1处的4个峰转变为只有D峰和G峰,说明晶界上的氢大量解吸附量减少,并且D峰和G峰的积分强度比ID/IG值变为最小,即sp2相团簇
    The annealing under different temperatures was performed on boron-doped nanocrystalline diamond films synthesized by hot filament chemical vapor deposition (HFCVD). The effects of annealing on the microstructure and electrochemical properties of films were systematically investigated. The results show that there are four peaks at 1157,1346,1470 and 1555 cm-1 in Raman spectra of the unannealed sample. When the films were annealed at temperatures above 800 ℃, there are only two peaks of D and G band, indicating that the hydrogen in grain boundaries significantly decreased. The area-integrated intensity ratio of D band to G band (ID/IG) reaches minimum value, revealing that the cluster number or cluster size of sp2 phase was reduced. The G peak position shifts to lower wave number, indicating an decrease in the ordering of graphitic component. The electrode exhibits the widest potential window and the highest oxygen evolution potential, and the quasi-reversible reaction occurs on the surface of the samples. The D peak is quite sharp and its intensity increases when the sample was annealed at 1000 ℃. The ID/IG value attains to the maximum value and the G peak position clearly shifts to higher value. The electrode exhibits the narrowest potential window and the lowest oxygen evolution potential, and the reversible electrochemical reaction occurs in the surface of the sample. The above results reveal that the cluster number or cluster size of sp2 phase, the amounts of trans-polyacetylene related to hydrogen in the grain boundaries, the disordering of graphitic components and the boron diffusion in the nanocrystalline diamond films give contributions to the complex change in electrochemical properties of the films with the annealing temperature increasing.
    • 基金项目: 国家自然科学基金(批准号:50602039, 50972129)和浙江省"钱江人才"计划(批准号:2010R10026)资助的课题.
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    Zhou Y L, Zhi J F, Zou Y S 2008 Anal. Chem. 80 4141

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    Ayten A Y, Swope V M, Swain G M 2008 Electrochemical Society 155 B1013

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    Wang S H, Swope V M, Butler J E 2009 Diam. Rel. Mater. 18 669

    [17]

    Ferrari A C, Robertson J 2001 Nanostruct. Carbon 1 77

    [18]

    Ferrari A C, Robertson J 2001 Phys. Rev. B 63 121405

    [19]

    Hao L, Sheldon B W, Kothari A 2006 Appl. Phys. Lett. 100 094309

    [20]

    Teii K, Ikeda T 2007 Diam. Rel. Mater. 16 753

    [21]

    Neto M A, Fernandes A J S, Silva R F 2007 Vacuum 81 1416

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    Arenal R, Montagnac G, Bruno P 2007 Phys. Rev. B 76 245316

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    Shi J R, Shi X, Sun Z 2000 Thin Solid Films 366 169

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    Rodil S E, Muhl S, Maca S 2003 Thin Solid Films 433 119

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    Ferrari A C, Kleinsorge B, Morrison N A 1999 Appl. Phys. Lett. 85 7191

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    Chhowalla M, Ferrari A C, Robertson J 2000 Appl. Phys. Lett. 76 1419

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  • [1]

    Fujishima A, Rao T N, Popa E, Sarada B V, Yagi I, Tryk D A 1999 Electroanal. Chem. 473 179

    [2]

    Sarada B V, Rao T N, Tryk D A, Fujishima A 1999 Electrochem. Soc. 146 1469

    [3]

    Xu J S, Chen Q Y, Swain G M 1998 Anal. Chem. 70 3146

    [4]

    Swain G M 1994 Electrochem. Soc. 141 3382

    [5]

    Declements R, Swain G M 1997 Electrochem. Soc. 144 856

    [6]

    Fischer A E, Swain G M 2005 Electrochem. Soc. 152 B369

    [7]

    Wei J J, He Q, Gao X H, Guo H B, Shi S Y, Lü F X, Tang W Z, Chen G C 2007 J. Syn. Crystals 36 569 (in Chinese) [魏俊 俊、贺 琦、高旭辉、郭会斌、石绍渊、吕反修、唐伟忠、陈广超 2007 人工晶体学报 36 569] 〖8] Qiu D J, Shi C R, Wu H Z 2002 Acta Phys. Sin. 51 1870 (in Chinese) [邱东江、石成儒、吴惠桢 2002 物理学报 51 1870]

    [8]

    Gruen D M 1999 Ann. Rev. Mater. Sci. 29 211

    [9]

    May P W, Ludlow W J, Hannaway M 2008 Diam. Rel. Mater. 17 105

    [10]

    Show Y, Witek M A, Sonthalia P 2003 Chem. Mater. 15 879

    [11]

    Liu C Y, Liu C 2003 Acta Phys. Sin. 52 1479 (in Chinese) [刘存业、刘 畅 2003 物理学报 52 1479]

    [12]

    Sun Z, Shi J R, Tay B K 2000 Diam. Rel. Mater. 9 1979

    [13]

    Birrell J, Gerbi J E, Auciello O, Gibson J M, Johnson J, Carlisle J A 2005 Diam. Rel. Mater. 14 86

    [14]

    Zhou Y L, Zhi J F, Zou Y S 2008 Anal. Chem. 80 4141

    [15]

    Ayten A Y, Swope V M, Swain G M 2008 Electrochemical Society 155 B1013

    [16]

    Wang S H, Swope V M, Butler J E 2009 Diam. Rel. Mater. 18 669

    [17]

    Ferrari A C, Robertson J 2001 Nanostruct. Carbon 1 77

    [18]

    Ferrari A C, Robertson J 2001 Phys. Rev. B 63 121405

    [19]

    Hao L, Sheldon B W, Kothari A 2006 Appl. Phys. Lett. 100 094309

    [20]

    Teii K, Ikeda T 2007 Diam. Rel. Mater. 16 753

    [21]

    Neto M A, Fernandes A J S, Silva R F 2007 Vacuum 81 1416

    [22]

    Arenal R, Montagnac G, Bruno P 2007 Phys. Rev. B 76 245316

    [23]

    Shi J R, Shi X, Sun Z 2000 Thin Solid Films 366 169

    [24]

    Rodil S E, Muhl S, Maca S 2003 Thin Solid Films 433 119

    [25]

    Ferrari A C, Kleinsorge B, Morrison N A 1999 Appl. Phys. Lett. 85 7191

    [26]

    Chhowalla M, Ferrari A C, Robertson J 2000 Appl. Phys. Lett. 76 1419

    [27]

    Hu X J, Cao H Z, Zheng G Q, Cao S 2006 J. Chem. Engng. Chin. Univ. 20 932 (in Chinese) [胡晓君、曹华珍、郑国渠、曹 帅 2006 高校化学工程学报 20 932]

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  • 收稿日期:  2009-11-03
  • 修回日期:  2010-01-11
  • 刊出日期:  2010-05-05

退火对B掺杂纳米金刚石薄膜微结构和电化学性能的影响

  • 1. 浙江工业大学化学工程与材料学院,杭州 310014
    基金项目: 国家自然科学基金(批准号:50602039, 50972129)和浙江省"钱江人才"计划(批准号:2010R10026)资助的课题.

摘要: 采用热丝化学气相沉积法制备B掺杂纳米金刚石薄膜,并对薄膜进行真空退火处理,系统研究了不同退火温度对B掺杂纳米金刚石薄膜的微结构和电化学性能的影响.结果表明,当退火温度升高到800 ℃后,薄膜的Raman谱图中由未退火时在1157,1346,1470,1555 cm-1处的4个峰转变为只有D峰和G峰,说明晶界上的氢大量解吸附量减少,并且D峰和G峰的积分强度比ID/IG值变为最小,即sp2相团簇

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