Citation: MA Xiao, XU Chongying, XU Dongsheng, DING Yuqiang, JIN Chenggang, JI Peiyu. Synthesis and Application of Guanidinato Silicon Precursors[J]. Chinese Journal of Applied Chemistry, ;2019, 36(10): 1179-1185. doi: 10.11944/j.issn.1000-0518.2019.10.190050 shu

Synthesis and Application of Guanidinato Silicon Precursors

a.
School of Chemical and Material Engineering, Jiangnan University, Wuxi, Jiangsu 214122, China
b.
Jiangsu Nata Opto-Electronic Material Co. Ltd., Suzhou, Jiangsu 215001, China
c.
School of Physical Science and Technology, Soochow University, Suzhou, Jiangsu 215006, China

Corresponding author: XU Chongying, chongying_xu@yahoo.com
Received Date: 26 February 2019
Revised Date: 15 April 2019
Accepted Date: 5 May 2019

Fund Project: National Science and Technology Major Project Ultra Large-Scale Integrated Circuit Manufacture Complete Set of Equipment and Technology 2016ZX02301003-004-004Supported by National Science and Technology Major Project Ultra Large-Scale Integrated Circuit Manufacture Complete Set of Equipment and Technology(No.2016ZX02301003-004-004)

Figures(7)

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.
- guanidinate,
- precursor,
- chemical vapor deposition,
- application
1. [1]
  Kern W, Schuegraf K K. Deposition Technologies and Applications: Introduction and Overview[M]. In Handbook of Thin Film Deposition Processes and Techniques.2nd ed, 2001: 11-43.
2. [2]
  Jang W, Jeon H, Song H. The Effect of Plasma Power on the Properties of Low-Temperature Silicon Nitride Deposited by RPALD for a Gate Spacer[J]. Phys Status Solid, 2015,212(12):2785-2790. doi: 10.1002/pssa.201532274
3. [3]
  Wrobel A M, Walkiewicz P A. Mechanism of the Initiation Step in Atomic Hydrogen-Induced CVD of Amorphous Hydrogenated Siliconcarbon Films from Single-Source Precursors[J]. Chem Vap Deposition, 1998,4(4):133-141. doi: 10.1002/(SICI)1521-3862(199807)04:04<133::AID-CVDE133>3.3.CO;2-U
4. [4]
  Saloum S, Alkhaled B. Structural, Optical and Electrical Properties of Plasma Deposited Thin Films from Hexamethyldisilazane Compound[J]. Acta Phys Pol A, 2011,119(3):369-373. doi: 10.12693/APhysPolA.119.369
5. [5]
  Liu X M, Yu Z J, Ryo I. Single-Source-Precursor Synthesis and Electromagnetic Properties of Novel RGO SiCN Ceramic Nanocomposites[J]. J Mater Chem C, 2017,5:7950-7960. doi: 10.1039/C7TC00395A
6. [6]
  Faisal A M, Francesco M, Muhammad I A, et al. Synthesisi, Characterization and Optical Constants of Silicon Oxycarbide[R]. EP J Web Conferences, 2017, 139: 00002-00009.
7. [7]
  Namrata B P, Yogesh S M, Anil S G. Synthesis and Characterization of Porogen Based Porous Low-k Thin Films[J]. Silicon, 2017,9(3):439-446. doi: 10.1007/s12633-016-9475-z
8. [8]
  Klaus J W, Ott A W, Dillon A C. Atomic Layer Controlled Growth of Si₃N₄ Films Using Sequential Surface Reactions[J]. Surf Sci, 1998,418:14-19. doi: 10.1016/S0039-6028(98)00705-5
9. [9]
  Yokoyama S, Ikeda N, Kajikawa K. Atomic-Layer Selective Deposition of Silicon Nitride on Hydrogen-Terminated Si Surfaces[J]. Appl Surf Sci, 1998,130:352-356.
10. [10]
  Fang Q, Hodson C. Silicon Nitride and Silicon Oxide Thin Films by Plasma ALD[R]. In Proceedings of the 8^th International Conference on Atomic Layer Deposition, Bruges, Belgium, 2008.
11. [11]
  Fainer I N, Golubenko N A, Rumyantsev M Y. Synthesis of Silicon Carbonitride Dielectric Films with Improved Optical and Mechanical Properties from Tetramethyldisilazane[J]. Glass Phys Chem, 2013,39(1):77-88.
12. [12]
  Du L Y, Chu W X, Ding Y Q. Synthesis, Characterization, and Properties of Silicon (Ⅳ) Compounds Containing N, N'-Symmetrically Alkyl Substituted 1, 3-Diketimine Ligands and Their Potential as CVD Precursor Material[J]. Phosphorus, Sulfur Silicon Relat Elem, 2017,192(11):1212-1218. doi: 10.1080/10426507.2017.1358718
13. [13]
  Yuan J N, Li M H, Ji N. Recent Progress in Chiral Guanidine-Catalyzed Michael Reactions[J]. Curr Org Chem, 2017,21(13):1205-1226. doi: 10.2174/1385272821666170127153759
14. [14]
  Travis L C, Scott D B. Synthesis and Characterization of a Series of Zinc Complexes Stabilized by 1, 1, 3, 3-Tetraalkylguanidinate (TAG) Ligands:[Zn(μ-TAG){N(SiMe₃)₂}]₂[J]. Polyhedron, 2007,26(18):5506-5512. doi: 10.1016/j.poly.2007.08.013
15. [15]
  Chen T N, William H, Philip S C. Synthesis, Structural Characterization, and Thermal Properties of the First Germanium N, N, N', N'-Tetraalkylguanidinates[J]. Organometallics, 2010,29(2):501-504. doi: 10.1021/om900801w
16. [16]
  Chen C W, Liu P T, Chang T C. Cu-Penetration Induced Breakdown Mechanism for a-SiCN[J]. Thin Solid Films, 2004,469:388-392.
17. [17]
  Wu C, Lu Y, Baklanov M R. Electrical Reliability Challenges of Advanced Low-k Dielectrics[J]. ECS J Solid State Sci Technol, 2015,4(1):N3065-N3070. doi: 10.1149/2.0091501jss
18. [18]
  Chang W Y, Chang C Y, Jihperng L. Optical Properties of Plasma-enhanced Chemical Vapor Deposited SiC_xN_y Films by Using Silazane Precursors[J]. Thin Solid Films, 2017,636:671-679. doi: 10.1016/j.tsf.2017.07.016
19. [19]
  Todd J W, Jason P C, Ahsan M. Group 11 Amidinates and Guanidinates:Potential Precursors for Vapour Deposition[J]. Eur J Inorg Chem, 2011,2011(21):3240-3247. doi: 10.1002/ejic.201100262
20. [20]
  Wright S F, Dunn J G, Alexander K. Determination of the Vapor Pressure Curves of Adipic Acid and Triethanolamine Using Thermogravimetric Analysis[J]. Thermochim Acta, 2004,421(1):25-30.
21. [21]
  Edward G G, Andrew R B. Chemical Vapor Deposition of Hexagonal Gallium Selenide and Telluride Films from Cubane Precursors:Understanding the Envelope of Molecular Control[J]. Mater Chem, 1997,9(12):3037-3048. doi: 10.1021/cm9703886
22. [22]
  Momtazur, Kamrul, Ellipsometric. XPS and FTIR Study on SiCN Films Deposited by Hot-Wire Chemical Vapor Deposition Method[J]. Mat Sci Semicon Proc, 2016,42:373-377. doi: 10.1016/j.mssp.2015.11.006
23. [23]
  Du L Y, Chu W X, Miao H Y. Synthesis, Characterization, Thermal Properties of Silicon (Ⅳ) Compounds Containing Guanidinato Ligands and Their Potential as CVD Precursors[J]. RSC Adv, 2015,5:71637-71643. doi: 10.1039/C5RA09755J
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