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Fabrication of silicon oxycarbide fibers from alkoxide solutions along the sol–gel process

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Abstract

Spinnable solutions are obtained in the sol–gel system of tetraethoxide (TEOS, Si(OC2H5)4) and vinyltrimethoxysilane (VTMS, CH2=CHSi(OCH3)3) under aqueous condition (water) with acid catalysts (HNO3 and HCl). Polysiloxane (PSO) fibers are drawn from the solution and characterized by spectroscopic and structural analyses. 29Si-nuclear magnetic resonance NMR) spectral analysis of the PSO fiber indicates the incorporation of atomic carbon in the silica network. 13C-NMR analysis shows the existence of considerable amount of hydroxyl groups in the PSO fiber. The spinnablity of the solution is studied by varying the mole ratios of the alkoxides, solvents and catalysts as well as precursor chemistries. The amount of water and catalysts are found to be important for the attaining of a spinnable state in the solution. SiOC fibers are obtained after pyrolysis of the PSO fibers with a high ceramic yield (88 wt%). The high ceramic yield attributes to the incorporation of vinyl-groups in the gel fiber that enhances crosslinking during pyrolysis. The SiOC fiber has a tensile strength of 776 MPa and electrical conductivity of 3.6 × 10−4 S/m.

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References

  1. Miele P, Bernard S, Cornu D, Toury B (2006) Recent developments in polymer-derived ceramic fibers (PDCFs): preparation, properties and applications–a review. Soft Mater 4(2–4):249–286

    Article  CAS  Google Scholar 

  2. Baldus P, Jansen M, Sporn D (1999) Ceramic fiber for matrix composites in high-temperature engine applications. Science 285:699–703

    Article  CAS  PubMed  Google Scholar 

  3. Varshavskii VV (2004) Ceramic fibers, a review. Fibre Chem 25:1573–8493

    Google Scholar 

  4. Sakka S, Kamiya K (1982) The sol–gel transition in the hydrolysis of metal-alkoxides in relation to the formation of glass fibers and films. J Non-Cryst Solids 48:31–46

    Article  CAS  ADS  Google Scholar 

  5. Kamiya K, Yoko T (1986) Synthesis of SiO2 glass fibers from Si(OC2H5)4–H2O-C2H5OH-HCl solutions through sol–gel method. J Mater Sci 21:842–848

    Article  CAS  ADS  Google Scholar 

  6. Kamiya K, Iwamoto Y, Yoko T, Sakka S (1988) Hydrolysis and condensation reactions of Si(OC2H5)4 related to silica fiber drawing. J Non-Cryst Solids 100:195–200

    Article  CAS  ADS  Google Scholar 

  7. Sakka S, Kozuka H (1988) Rheology of sols and fiber drawing. J Non-Cryst Solids 100:142–153

    Article  CAS  ADS  Google Scholar 

  8. Kamiya K, Katayama A, Suzuki H, Nishida K, Hashimoto T, Matsuoka J, Nasu H (1999) Preparation of silicon oxycarbide glass fibers by Sol–Gel method effect of starting sol composition on tensile strength of fibers. J Sol Gel Sci Technol 14:95–102

    Article  CAS  Google Scholar 

  9. Kolar F, Machovic V, Svitilova J, Borecka L (2004) Structural characterization and thermal oxidation resistance of silicon oxycarbides produced by polysiloxane pyrolysis. Mater Chem Phys 86:88–98

    Article  CAS  Google Scholar 

  10. Cordelair J, Greil P (2000) Electrical conductivity measurements as a microprobe for structure transitions in polysiloxane derived Si-O-C ceramics. J Eur Ceram Soc 20:1947–1957

    Article  CAS  Google Scholar 

  11. Colombo P, Gambaryan-Roisman T, Scheffler M, Buhler P, Greil P (2001) Conductive ceramic foams from preceramic polymers. J Am Ceram Soc 84:2265–2268

    Article  CAS  Google Scholar 

  12. Colombo P, Hellmann JR (2002) Ceramic foams from preceramic polymers. Mater Res Innov 6:260–272

    Article  CAS  Google Scholar 

  13. Riedel R, Gabriel M, Ralf H, Alexander K (1996) Silicon-based polymer-derived ceramics: Synthesis properties and applications—A review. Jpn J Ceram Soc 114:425–444

    Article  Google Scholar 

  14. Hu Y (2000) Preparation of silicon oxycarbide glass fibers from organically modified silicates. J Mater Sci 35:3155–3159

    Article  CAS  Google Scholar 

  15. Chen LF, Cai ZH, Zhou W, Lan X, Chen XJ (2005) Preparation and properties of silicon oxycarbide fibers. J Mater Sci 40:3497–3501

    Article  CAS  ADS  Google Scholar 

  16. Chen LF, Cai ZH, Zhang L, Lan L, Chen XJ, Zeng J (2007) Preparation and properties of silicon oxycarbide fibers. J Mater Sci 42:1004–1009

    Article  CAS  ADS  Google Scholar 

  17. Su D, Li YL, An HJ (2010) Pyrolytic transformation of liquid precursors to shaped bulk ceramics. J Eur Ceram Soc 30:1503–1511

    Article  CAS  Google Scholar 

  18. Soraru GD, Liu Q, Interrante LV, Apple T (1998) Role of precursor molecular strucrure on the microstructure and high temperature stability of silicon oxycarbide glass derived from methylene-bridged polycarbosilanes. Chem Mater 10:4047–4054

    Article  CAS  Google Scholar 

  19. Takamura N, Taguchi K, Gunji T, Abe Y (1999) Preparation of silicon oxycarbide ceramic films by pyrolysis of polymethy-and polyvinysilsesquioxanes. J Sol–Gel Sci Techno 16:227–234

    Article  CAS  Google Scholar 

  20. Soraru GD (2000) Hybrid RSiO1.5/B2O3 gels from Modified Silicon alkoxides and boric acid. J Sol Gel Sci Technol 18:11–19

    Article  CAS  Google Scholar 

  21. Alonso RP, Soraru GD (2007) Synthesis and characterization of hybrid borosiloxane gels as precursors for Si-B-O-C fibers. J Sol Gel Sci Technol 43:313–319

    Article  Google Scholar 

  22. Mah SK, Chung IJ (1995) Effects of dimethyldiethoxysilane addition on tetraethylorthosilicate sol–gel process. J Non-Cryst Solids 183:252–259

    Article  CAS  ADS  Google Scholar 

  23. Zhang ZP, Gorman BP, Dong HJ, Orozco-Teran RA, Mueller DW, Reidy RF (2003) Investigation of polymerization and crystallization of dimethyldiethoxysilane by 29Si NMR and FTIR. J Sol Gel Sci Technol 28:159–165

    Article  CAS  Google Scholar 

  24. Kroke E, Li YL, Konetschny C, Lecomte E, Fasel C, Riedel R (2000) Silazane derived ceramics and related materials. Mater Sci Eng R 26:97–199

    Article  Google Scholar 

  25. Lipowitz J (1991) Structure and properties of ceramic fibers prepared from organosilcon polymers. J Inorg Organomet Polym 3:277–297

    Article  Google Scholar 

  26. Pantano CG, Singh AK, Zhang HX (1999) Silicon oxycarbide glass. J Sol Gel Sci Technol 14:7–25

    Article  CAS  Google Scholar 

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Acknowledgments

This work is supported by the National Basic Research Program of China (Grant No. 2010CB934700), National Science Foundation for Distinguished Young Scholars (50625207), the Applied Fundamental and Frontier Research Foundation of Tianjin Municipal, and State Key Laboratory of Precise Measurement and Equipment, Tianjin University, China.

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Correspondence to Ya-Li Li.

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Ruan, DS., Li, YL., Wang, L. et al. Fabrication of silicon oxycarbide fibers from alkoxide solutions along the sol–gel process. J Sol-Gel Sci Technol 56, 184–190 (2010). https://doi.org/10.1007/s10971-010-2292-8

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  • DOI: https://doi.org/10.1007/s10971-010-2292-8

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