应用化学 ›› 2019, Vol. 36 ›› Issue (10): 1179-1185.DOI: 10.11944/j.issn.1000-0518.2019.10.190050

• 研究论文 • 上一篇    下一篇

胍基硅前驱体的合成及应用

马潇a,许从应a*(),许东升b,丁玉强a,金成刚c,季佩宇c   

  1. a江南大学化学与材料工程学院 江苏 无锡 214122
    b江苏南大光电材料股份有限公司 江苏 苏州 215001
    c苏州大学物理科学与技术学院 江苏 苏州 215006
  • 收稿日期:2019-02-26 接受日期:2019-05-05 出版日期:2019-10-01 发布日期:2019-09-29
  • 通讯作者: 许从应
  • 基金资助:
    国家科技重大专项“极大规模集成电路制造装备及成套工艺”(2016ZX02301003-004-004)资助

Synthesis and Application of Guanidinato Silicon Precursors

MA Xiaoa,XU Chongyinga*(),XU Dongshengb,DING Yuqianga,JIN Chenggangc,JI Peiyuc   

  1. aSchool of Chemical and Material Engineering,Jiangnan University,Wuxi,Jiangsu 214122,China
    bJiangsu Nata Opto-Electronic Material Co. Ltd.,Suzhou,Jiangsu 215001,China
    c School of Physical Science and Technology,Soochow University,Suzhou,Jiangsu 215006,China
  • Received:2019-02-26 Accepted:2019-05-05 Published:2019-10-01 Online:2019-09-29
  • Contact: XU Chongying
  • Supported by:
    Supported by National Science and Technology Major Project Ultra Large-Scale Integrated Circuit Manufacture Complete Set of Equipment and Technology(No.2016ZX02301003-004-004)

摘要:

以胍基取代的二甲基二氯硅烷与胺基锂反应合成了3种硅基化合物,使用核磁共振、高分辨质谱、元素分析对化合物结构进行了表征,通过热重分析(TGA)研究了化合物的热稳定性、挥发性、蒸汽压等性能。 3种化合物均具有良好的热稳定性及挥发性,无明显热分解过程,固体残留小于1%,接近纯挥发过程,最高蒸汽压在3600~5300 Pa,满足前驱体使用要求。 以二甲基-胍基-甲乙胺基-硅烷为前驱体,采用螺旋波等离子体气相沉积(HWPCVD)工艺制备了硅基薄膜,使用X射线光电子能谱(XPS)和扫描电子显微镜(SEM)分析了薄膜的化学组成和膜表面结构,XPS分析结果证实该薄膜为Si、N、C组成,实验结果表明,该类胍基硅化合物可作为硅基化学气相沉积(CVD)前驱体材料应用于集成电路制造。

关键词: 胍基, 前驱体, 化学气相沉积, 应用

Abstract:

Three silicon compounds were synthesized by reaction of dimethyldichlorosilane with 1,1,3,3-tetramethylguanidine substituent and lithium amide. The structures of the compounds were verified by 1H nuclear magnetic resonance (NMR), 13C NMR, electron ionization-mass spectrometry (EI-MS), and elemental analysis. The thermal stability and vapor pressures of these compounds were evaluated by thermo gravimetric analysis(TGA). The results show a nearly pure volatilization with low decomposition process and residual(<1%). The highest vapor pressure ranges from 3600 Pa to 5300 Pa, which is suitable for chemical vapor deposition (CVD) precursors. Silicon films were prepared by using dimethyl-guanidinato-ethylmethylamide silane as the precursor in Helicon wave plasma CVD (HWP-CVD). The properties of the films were studied by scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The films are composed of Si, N, and C. Guanidinate-based silicon compounds as CVD precursors have potential applications in fabrication of semiconductor devices.

Key words: guanidinate, precursor, chemical vapor deposition, application