Skip to main content
Log in

Study of a silicon-based preceramic for the processing of polymer-derived ceramics

  • Original Paper: Characterization methods of sol-gel and hybrid materials
  • Published:
Journal of Sol-Gel Science and Technology Aims and scope Submit manuscript

Abstract

Silicon-based preceramic polymers are an important type of precursor used in the processing of novel polymer-derived ceramics (PDCs), which includes the cross-linking and pyrolysis of the precursor. An integral study of physicochemical and rheological properties of a silicon-based preceramic regarding the variables that control the crosslinking and the characterization pyrolyzed material were accomplished. The precursor synthetized by the sol–gel method was characterized by density measurement, SEC, ATR-FTIR, NMR, and DSC. Flow properties in function of temperature and time, and viscoelastic properties as a function of deformation, frequency, temperature and time were studied by rotational and oscillatory testing, respectively. Also, the crosslinking process in the presence of a catalyst was studied by ATR-FTIR and dynamic tests. The phases generated at high temperature were characterized by XRD, Raman spectroscopy, and EDS. The results indicate that the studied precursor could be considered as a preceramic polymer for developing SiOC-based PDCs.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8
Fig. 9

Similar content being viewed by others

References

  1. Riedel R, Mera G, Hauser R, Klonczynski A (2006) Silicon-based polymer-derived ceramics: synthesis properties and applications—a review. J Ceram Soc Japan 114:425–444

    Article  Google Scholar 

  2. Colombo P, Mera G, Riedel R, Sorarù GD (2010) Polymer-derived ceramics: 40 years of research and innovation in advanced ceramics. J Am Ceram Soc 93:1805–1837

    Google Scholar 

  3. Colombo P, Riedel R, Sorarù GD, Kleebe H-J (2010) Polymer derived ceramics: from nano-structures to applications. DEStech Publications Inc., Lancaster

    Book  Google Scholar 

  4. Vakifahmetoglu C, Zeydanli D, Colombo P (2016) Porous polymer derived ceramics. Mater Sci Eng: R Rep 106:1–30

    Article  Google Scholar 

  5. Mera G, Navrotsky A, Sen S et al. (2013) Polymer-derived SiCN and SiOC ceramics—structure and energetics at the nanoscale. J Mater Chem A 1:3826–3836

    Article  Google Scholar 

  6. Ionescu E (2012) Polymer-derived ceramics. In: Riedel R, Chen I-W (eds) Ceramics Science and Technology. Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim, Germany, pp 457–500

  7. Li J, Lu K, Lin T, Shen F (2015) Preparation of micro-/mesoporous SiOC bulk ceramics. J Am Ceram Soc 98:1753–1761

    Article  Google Scholar 

  8. Sorarù GD, D’Andrea G, Campostrini R et al. (1995) Structural characterization and high-temperature behavior of silicon oxycarbide glasses prepared from sol–gel precursors containing Si–H bonds. J Am Ceram Soc 78:379–387

    Article  Google Scholar 

  9. Bernardo E, Fiocco L, Parcianello G et al. (2014) Advanced ceramics from preceramic polymers modified at the nano-scale: a review. Materials 7:1927–1956

    Article  Google Scholar 

  10. Colombo P, Bernardo E, Parcianello G (2013) Multifunctional advanced ceramics from preceramic polymers and nano-sized active fillers. J Eur Ceram Soc 33:453–469

    Article  Google Scholar 

  11. Kaur S, Riedel R, Ionescu E (2014) Pressureless fabrication of dense monolithic SiC ceramics from a polycarbosilane. J Eur Ceram Soc 34:3571–3578

    Article  Google Scholar 

  12. Hossain SS, Sarkar S, Oraon NK, Ranjan A (2016) Pre-ceramic polymer-derived open/closed cell silicon carbide foam: microstructure, phase evaluation, and thermal properties. J Mater Sci 51:9865–9878

    Article  Google Scholar 

  13. Mantzel N, Schröckert F, Bucharsky EC et al. (2018) Reduction of the sintering temperature for the manufacturing of carbon-rich dense SiOC bulk ceramics. Adv Eng Mater 20:1800369

    Article  Google Scholar 

  14. Zhao Z, Niu M, Wang H et al. (2019) Preparation and the effects of ion irradiation on bulk SiOC ceramics. J Eur Ceram Soc 39:832–837

    Article  Google Scholar 

  15. Su D, Li Y-L, An H-J et al. (2010) Pyrolytic transformation of liquid precursors to shaped bulk ceramics. J Eur Ceram Soc 30:1503–1511

    Article  Google Scholar 

  16. Li X, Pei X, Zhong X et al. (2019) Highly effective free-radical-catalyzed curing of hyperbranched polycarbosilane for near stoichiometric SiC ceramics. J Am Ceram Soc 102:1041–1048

    Article  Google Scholar 

  17. Konegger T, Williams LF, Bordia RK (2015) Planar, polysilazane-derived porous ceramic supports for membrane and catalysis applications. J Am Ceram Soc 98:3047–3053

    Article  Google Scholar 

  18. Janakiraman N, Aldinger F (2009) Fabrication and characterization of fully dense Si–C–N ceramics from a poly(ureamethylvinyl)silazane precursor. J Eur Ceram Soc 29:163–173

    Article  Google Scholar 

  19. Jiang T, Hill A, Fei W et al. (2010) Making bulk ceramics from polymeric precursors. J Am Ceram Soc 93:3017–3019

    Article  Google Scholar 

  20. Balan C, Riedel R (2006) Rheological investigations of a polymeric precursor for ceramic materials: experiments and theoretical modeling. J Optoelectron Adv Mater 8:561–567

    Google Scholar 

  21. Balan C, Völger KW, Kroke E, Riedel R (2000) Viscoelastic properties of novel silicon carbodiimide gels. Macromolecules 33:3404–3408

    Article  Google Scholar 

  22. Harshe R, Balan C, Riedel R (2004) Amorphous Si(Al)OC ceramic from polysiloxanes: bulk ceramic processing, crystallization behavior and applications. J Eur Ceram Soc 24:3471–3482

    Article  Google Scholar 

  23. Reschke V, Bordia RK, Scheffler F, Scheffler M (2015) Rheology and crosslinking of a low-viscosity SiOC preceramic polymer. Ceram Int 42:7620–7625

    Article  Google Scholar 

  24. Winter HH, Chambon F (1986) Analysis of linear viscoelasticity of a crosslinking polymer at the gel point. J Rheol 30:367–382

    Article  Google Scholar 

  25. Kickelbick G (2007) Introduction to hybrid materials. In: Hybrid materials. Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim, Germany, pp. 1–48

  26. Wallace WE, Guttman CM, Antonucci JM (2000) Polymeric silsesquioxanes: degree-of-intramolecular-condensation measured by mass spectrometry. Polymer 41:2219–2226

    Article  Google Scholar 

  27. Eisenberg P, Erra-Balsells R, Ishikawa Y et al. (2002) Silsesquioxanes derived from the bulk polycondensation of [3-(Methacryloxy)propyl]trimethoxysilane with concentrated formic acid: evolution of molar mass distributions and fraction of intramolecular cycles. Macromolecules 35:1160–1174

    Article  Google Scholar 

  28. Bautista Y, Gozalbo A, Mestre S et al. (2017) Improvement in char strength with an open cage silsesquioxane flame retardant. Materials (Basel) 10:1–14

    Google Scholar 

  29. Innocenzi P, Brusatin G, Licoccia S et al. (2003) Controlling the thermal polymerization process of hybrid organic−inorganic films synthesized from 3-Methacryloxypropyltrimethoxysilane and 3-Aminopropyltriethoxysilane. Chem Mater 15:4790–4797

    Article  Google Scholar 

  30. El hadad A, Carbonell D, Barranco V et al. (2011) Preparation of sol–gel hybrid materials from γ-methacryloxypropyltrimethoxysilane and tetramethyl orthosilicate: study of the hydrolysis and condensation reactions. Colloid Polym Sci 289:1875–1883

    Article  Google Scholar 

  31. Nishiyama N, Horie K, Asakura T (1987) Hydrolysis and condensation mechanisms of a silane coupling agent studied by 13C and 29Si NMR. J Appl Polym Sci 34:1619–1630

    Article  Google Scholar 

  32. Peng J, Xu K, Cai H et al. (2014) Can an intact and crystalline octakis(methacryloxypropyl) silsesquioxane be prepared by hydrolysis-condensation of a trimethoxysilane precursor? RSC Adv 4:7124–7131

    Article  Google Scholar 

  33. Gualandris V, Hourlier-Bahloul D, Babonneau F (1999) Structural investigation of the first stages of pyrolysis of Si-C-O preceramic polymers containing Si-H bonds. J Sol–Gel Sci Technol 14:39–48

    Article  Google Scholar 

  34. Fanovich MA, Pellice SA, Galliano PG, Williams RJJ (2002) Organic/inorganic hybrid materials based on silsesquioxanes derived from (3-Methacryloxypropyl) trimethoxysilane and their blends with vinylester resins. J Sol–Gel Sci Technol 23:45–52

    Article  Google Scholar 

  35. Mezger T (2006) The rheology handbook: for users of rotational and oscillatory rheometers, 2nd ed. Vincentz Network, Hannover

    Google Scholar 

  36. Ferry JD (1980) Viscoelastic properties of polymers, 3rd ed. John Wiley & Sons, Inc, New York, NY

    Google Scholar 

  37. Macosko CW (1994) Rheology: principles easurements, and applications. Wiley-VCH, New York, NY

    Google Scholar 

  38. Kobayashi K, Huang C, Lodge TP (1999) Thermoreversible gelation of aqueous methylcellulose solutions. Macromolecules 32:7070–7077

    Article  Google Scholar 

  39. Young RJ, Lovell PA (2011) Introduction to polymers, Third Edition. CRC Press, Boca Raton

    Book  Google Scholar 

  40. Vakifahmetoglu C, Pippel E, Woltersdorf J, Colombo P (2010) Growth of one-dimensional nanostructures in porous polymer-derived ceramics by catalyst-assisted pyrolysis. Part I: Iron catalyst. J Am Ceram Soc 93:959–968

    Article  Google Scholar 

  41. Vakifahmetoglu C, Colombo P, Carturan SM et al. (2010) Growth of one-dimensional nanostructures in porous polymer-derived ceramics by catalyst-assisted pyrolysis. Part II: cobalt catalyst. J Am Ceram Soc 93:3709–3719

    Article  Google Scholar 

  42. Siddiqi SA, Hendry A (1985) The influence of iron on the preparation of silicon nitride from silica. J Mater Sci 20:3230–3238

    Article  Google Scholar 

  43. Weimer AW, Eisman GA, Susnitzky DW et al. (1997) Mechanism and kinetics of the carbothermal nitridation synthesis of α-silicon nitride. J Am Ceram Soc 80:2853–2863

    Article  Google Scholar 

  44. Bois L, Maquet J, Babonneau F, Bahloul D (1995) Structural characterization of sol-gel derived oxycarbide glasses. 2. Study of the thermal stability of the silicon oxycarbide phase. Chem Mater 7:975–981

    Article  Google Scholar 

  45. Seo WS, Koumoto K (1996) Stacking faults in β-SiC formed during carbothermal reduction of SiO2. J. Am. Ceram. Soc. 79:1777–1782

    Article  Google Scholar 

  46. Pujar VV, Cawley JD (2001) Computer simulations of diffraction effects due to stacking faults in β-SiC: II, experimental verification. J Am Ceram Soc 84:2645–2651

    Article  Google Scholar 

  47. Martin H-P, Müller E, Irmer G, Babonneau F (1997) Crystallisation behaviour and polytype transformation of polymer-derived silicon carbide. J Eur Ceram Soc 17:659–666

    Article  Google Scholar 

  48. Ferrari AC, Robertson J (2004) Raman spectroscopy of amorphous, nanostructured, diamond-like carbon, and nanodiamond. Philos Trans A Math Phys Eng Sci 362:2477–2512

    Article  Google Scholar 

Download references

Acknowledgements

The authors gratefully acknowledge Dr. M. Valiente Malmagro (Research Group of Separation Techniques in Chemistry, UAB, Barcelona, Spain) for accomplishing the 1H, 13C, 29Si NMR tests used in this work. This study was funded by the National Scientific and Technical Research Council, CONICET, Argentina (PIP 0128), and the National Agency of Scientific and Technological Promotion, ANPCyT, Argentina (PICT 2790).

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Mariano H. Talou.

Ethics declarations

Conflict of interest

The authors declare that they have no conflict of interest.

Additional information

Publisher’s note: Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Supplementary Information

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Rivera, J.O.B., Talou, M.H., Hung Hung, Y.M.X. et al. Study of a silicon-based preceramic for the processing of polymer-derived ceramics. J Sol-Gel Sci Technol 91, 446–460 (2019). https://doi.org/10.1007/s10971-019-05051-x

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10971-019-05051-x

Keywords

Navigation