仪器科学与技术

纳米多孔氧化硅薄膜的表征及其基于UAFM弹性性能的检测

  • 张改梅 ,
  • 王灿 ,
  • 宋晓利 ,
  • 何存富 ,
  • 陈强
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  • 1. 北京印刷学院印刷与包装工程学院 北京 102600;
    2. 北京工业大学机械工程与应用电子技术学院 北京 100124
张改梅,女,1975年出生,博士,教授,硕士研究生导师。主要研究方向为纳米无损检测技术、包装防护理论与方法。E-mail:zhanggaimei@bigc.edu.cn

收稿日期: 2017-05-20

  修回日期: 2017-10-30

  网络出版日期: 2018-06-20

基金资助

国家自然科学基金(51305038)和北京印刷学院校级资助项目(Ed201804)资助项目。

Characterization and Measurement of Elastic Modulus Based on Ultrasonic Atomic Force Microscopy for Nano-porous Silicon Oxide Film

  • ZHANG Gaimei ,
  • WANG Can ,
  • SONG Xiaoli ,
  • HE Cunfu ,
  • CHEN Qiang
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  • 1. School of Printing and Packagine Engineering Beijing Institute of Graphic Communication, Beijing 102600;
    2. College of Mechanical Engineering & Applied Electronics Technology, Beijing University of Technology, Beijing 100124

Received date: 2017-05-20

  Revised date: 2017-10-30

  Online published: 2018-06-20

摘要

纳米级多孔氧化硅薄膜介电常数低,和铝复合后可以大大降低电阻损耗,是最有希望的新一代低介电材料。在纳电子器中低介电薄膜孔隙率及孔尺寸可以控制其机械性能。薄膜的弹性模量是器件设计的必需参数,然而传统方法很难在纳米尺度表征弹性模量。采用等离子体增强化学气相沉积法,以六甲基二硅氧烷为单体,氧气作为反应气体,再加入少量的有机物质在玻璃基材上沉积纳米厚度的氧化硅薄膜,再进行热处理使氧化硅薄膜中的有机成分挥发形成孔隙(以下称纳米多孔氧化硅薄膜),从而降低薄膜介电常数。结果表明氧化硅薄膜的折射率热处理后得到减小,当放电功率为100 W时,氧气与单体的比例为1∶4时,放电时间10 min沉积的薄膜热处理后的纳米多孔氧化硅薄膜的折射率最小,介电常数1.885。首次采用超声原子力显微镜技术对纳米多孔氧化硅薄膜的弹性性能进行无损检测,分别检测纳米氧化硅薄膜和纳米多孔氧化硅薄膜的前两阶接触谐振频率。以纳米氧化硅薄膜为参考试样,利用参考法计算得到纳米多孔氧化硅薄膜的压痕模量为35.24 GPa。相比纳米氧化硅薄膜的压痕模量78.18 GPa,纳米多孔氧化硅薄膜的压痕模量降低了42.94 GPa。

本文引用格式

张改梅 , 王灿 , 宋晓利 , 何存富 , 陈强 . 纳米多孔氧化硅薄膜的表征及其基于UAFM弹性性能的检测[J]. 机械工程学报, 2018 , 54(12) : 109 -114 . DOI: 10.3901/JME.2018.12.109

Abstract

Nano-porous silicon oxide film with low dielectric constant, compositing with aluminum can greatly reduce the resistance loss, it is the most promising of the new generation of low dielectric material. In nano-electronics, the mechanical properties of the low dielectric film can be controlled by its porosity and pore size. The elastic modulus is a required parameter in device designs. However, the traditional methods can not characterize the elastic modulus at the nano-scale. Herein, using plasma enhanced chemical vapor deposition (PECVD) method, hexamethyldisiloxane (HMDSO) is as monomer and oxygen as a reaction gas, meanwhile a small amount of organic material is added, the silicon oxide film is deposited on the glass substrate surface with glow discharge plasma, then the film is heat-treated at a high temperature, so organic components such hydrogen bonds are removed and the pores are formed (hereafter refer to nano-porous silicon oxide film) to reduce the dielectric constant. The results show that the refractive index of the silicon oxide film is reduced with heat treatment, wherein when the discharge power is 100 W, ratio of oxygen to monomer is 1:4, the discharge time is 10min, the refractive index of the film is minimized after the heat treatment, the dielectric constant is 1.885. At the same time, using ultrasonic atomic force microscopy system (UAFM) the elastic modulus of the nano-porous silicon oxide film is tested with non-destructive. Silicon oxide nano-film as a reference sample, elastic properties silicon oxide films with heat-treated is detected experimentally. Indentation modulus of silicon oxide nano-film after heat treatment is 35.24 GPa. Comparing to the silicon oxide nano-film with 78.8 GPa indentation modulus, it reduces 42.94 GPa for nano-porous silicon oxide film.

参考文献

[1] MILLER, R. D. In search of Low-k dielectrics[J]. Science, 1999, 286(5439):421.
[2] 姬亚宁,唐小青,刘业强, 等. 低介电常数无氟聚酰亚胺薄膜制备方法的研究进展[J]. 绝缘材料, 2016,49(9):28-32 JI Yaning, TANG Xiaoqing, LIU Yeqiang, et al. Development of preparation methods for low dielectric constant non-fluorinated polyimide film[J]. Insulating Materials, 2016, 49(9):28-32.
[3] MAEX K, BAKLANOV M R, SHAMIRYAN D, et al, Low dielectric constant materials for microelectronics[J]. Journal of Applied Physics. 2003, 93(11):8793-8841.
[4] BALUCANI M, BONDARENKO V, VOROZOV N., et al. Technological aspects of oxidated porous silicon waveguides[J]. Physica E, 2003, 16(3-4):586-590.
[5] QIAN Xin,HUANG Tao, NARA H. Electrodeposited three-dimensional porous Si-O-C/Ni thick film as high performance anode for lithium-ion batteries[J]. Journal of Power Sources, 2014, 272:794-799.
[6] DANKO V A,ZLOBIN S O,INDUTNYI I Z, et al. Influence of the HF vapor treatment on the structure and luminescence properties of porous si/siox nanocomposites[J]. Ukrainian Journal of Physics, 2010, 55(9):1042-1048.
[7] GUENDOUZ M,PEDRONO N,ETESSE R,et al. Oxidised and non oxidised porous silicon/disperse red 1composite:Physical and optical properties[J]. Physica Status Solid, 2003, 197(2):414-418.
[8] JAIN A, ROGOJEVIC S, PONOTH S, et al. Porous silica materials as low k dielectrics for electronic and optical interconnects[J]. Thin Solid Films, 2001, 398-399:513-522.
[9] 吴兆丰,吴广明, 姚兰芳,等. 低介电常数多孔氧化硅薄膜的制备与研究[J]. 材料科学与工程学报, 2005, 23(3):408-411. WU Zhaofeng, WU Guangming, YAO Lanfang, et al. Preparation and study of low dielectric constant mesoporous silica films[J]. Journal of Materials Science and Engineering, 2005, 23(3):408-411.
[10] 马建华, 孟祥建, 孙璟兰,等. 常压制备SiO2气凝胶薄膜[J]. 红外与毫米波学报, 2004(6):465-468. MA Jianhua, MENG Xiangjian, SUN Jinlan, et al. Silica aerogel thin films prepared at amient pressure[J]. Journal of Infrared and Millimeter Waves, 2004(6):465-468.
[11] GRILL A, PATEL V. Ultralow-k dielectrics prepared by plasma-enhanced chemical vapor deposition[J]. Applied Physics Letters, 2001, 79(6):803-805.
[12] FAVENNEC L, JOUSSEAUME V, GERBAUD G, et al. Ultralow k using a plasma enhanced chemical vapor deposition porogen approach:Matrix structure and porogen loading influences[J]. Journal of Applied Physics, 2007, 102(6):064107-064107-9.
[13] 陶珺,穆磊,杜平.多点光纤光栅测温系统在渗流监测中的应用研究[J].量子电子学报,2010, 27(1):105-109. TAO Jun, MU Lei, DU Ping. Application of multi-point optical fiber grating temperature measurement system on seepage monitoring[J]. Chinese Journal of Quantum Electronics, 2010, 27(1):105-109.
[14] ZHANG Gaimei, HE Cunfu, WU Bin, et al. Evaluating local elasticity of the metal nano-films quantitatively based on referencing approach of atomic force acoustic microscopy[J]. Chinese Journal of Mechanical Engineering, 2012, 25(6):1281-1286.
[15] RABE U, JANSER K, ARNOLD W. Vibrations of free and surface-coupled atomic force microscope cantilevers:Theory and experiment[J]. Review of Scientific Instruments,1996, 67(9):3281-3293.
[16] KOPYCINSKA-MULLER M, CLAUSNER A, YEAP K B, et al. Mechanical characterization of porous nano-thin films by use of atomic force acoustic microscopy[J]. Ultramicroscopy, 2016, 162:82-90.
[17] 孙运金, 陈强, 张跃飞,等. 新型高阻隔有机氧化硅薄膜制备[J]. 真空, 2008, 45(2):46-49. SUN Yinjin, CHEN Qiang, ZHANG Yuefei, et al. Preparation of a new high-barrier organic SiOx thin film[J]. Vacuum, 2008, 45(2):46-49.
[18] 吴兆丰, 吴广明, 姚兰芳. 疏水型介孔氧化硅薄膜的制备与研究[J]. 材料导报, 2005(3):106-108. WU Zhaofeng, WU Guangming, YAO Lanfang, et al. Preparation an investigation of hydrophobic mesoporous silica films[J]. Materials Review, 2005(3):106-108.
[19] CHEN Hongji, FU Meng. Core-shell-shaped organic-inorganic hybrid as pore generator for imprinting nanopores in organosilicate dielectric films[J]. Macromolecules, 2007, 40(6):2079-2085.
[20] 姚启钧. 光学教程[M]. 北京:高等教育出版社, 1989 YAO Qijun. Optical tutorial[M]. Beijing:Higher Education Press, 1989.
[21] 李靓, 姚熹, 张良莹. 低介电常数多孔二氧化硅薄膜的制备与性能研究[J]. 固体电子学研究与进展, 2005(4):549-553. LI Liang, Yao Xi, ZHANG Liangying. Preparation and characterization of low dielectric constant porous silica films[J]. Research and Progress of SSE, 2005(4):549-553.
[22] JOHNSON K. Contact mechanics[M]. Cambridge:Cambridge University Press, 1995.
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