Abstract
Room-temperature cross-linking of a hyperbranched polycarbosilane (HBPCS) with divinylbenzene (DVB) in the presence of the cyclohexanone peroxide–cobaltous naphthenate (CHP–CN) initiator system was studied. According to the Fourier transform infrared spectroscopy (FT-IR) and 1H nuclear magnetic resonance (1H NMR) results, the cross-linking reaction occurred via the vinyl polymerization. The GPC analysis confirmed the molecular weight of the cross-linked HBPCS significantly increased. Thermal behaviors of cross-linked HBPCS and original HBPCS were investigated by thermal gravimetric analysis-differential thermal analysis (TGA–DTA). The TGA results indicated that the ceramic yield of HBPCS remarkably increased by the cross-linking treatment. For the HBPCS/10 wt% DVB system, the maximum of reaction degree of HBPCS was obtained, which might be responsible for the highest ceramic yield of 70.1 wt% at 1000 °C. However, the ceramic yield of the non-crosslinked HBPCS was only 45 wt% at 1000 °C. The evolution of crystal structure of SiC as a function of pyrolysis temperature was traced by means of X-ray diffraction (XRD) and FT-IR. With the pyrolysis temperature increasing, the β-SiC peaks became sharper and the grain size also grew larger. As the DVB content increased, the intensity of β-SiC peaks significantly reduced, indicating smaller β-SiC grain size.
Similar content being viewed by others
References
Kita K, Narisawa M, Nakahira A et al (2010) J Mater Sci 45(1):139. doi:10.1007/s10853-009-3905-x
Interrante LV, Shen QH (2009) In: Dvornic PR, Owen MJ (eds) Silicon-containing dendritic polymers, chap 12. Springer, Dordrecht
Whitmarsh CK, Interrante LV (1991) Organometallics 10:1336
Rushkin IL, Shen Q, Lehman SE et al (1997) Macromolecules 30:3141
Interrante LV, Moraes K, MacDonald L et al (2002) Ceram Trans 144:125
Kotani M, Kato Y, Kohyama A et al (2003) J Ceram Soc Jpn 111:300
Zheng J, Akinc M (2001) J Am Ceram Soc 84:2479
Huang TH, Yu ZJ, He XM et al (2007) Chin Chem Lett 18:754
Huang MH, Fang YH, Li R et al (2009) J Appl Polym Sci 113:1611
Li HB, Zhang LT, Cheng LF et al (2008) J Mater Sci 43:2806. doi:10.1007/s10853-008-2539-8
Li HB, Zhang LT, Cheng LF et al (2008) J Eur Ceram Soc 28:887
Li HB, Zhang LT, Cheng LF et al (2009) J Mater Sci 44:721. doi:10.1007/s10853-008-3176-y
Bouillon E, Pailler R, Naslain R et al (1991) Chem Mater 3:356
Froehling PE (1993) J Inorg Organomet Polym 3:251
Interrante LV, Shen QH (2000) In: Jones RG et al (eds) Silicon-containing polymers. Kluwer Academic Publishers, Dordrecht
Liu Q, Wu HJ, Lewis R et al (1999) Chem Mater 11:2038
Yu ZJ, Huang MH, Li R et al (2009) J Chin Ceram Soc 37:105
George SL, Geoffrey P (1969) I&EC Prod Res Dev 8:124
Maddocks AR, Hook JM, Stender H et al (2008) J Mater Sci 43:2666. doi:10.1007/s10853-008-2488-2
Jian K, Chen ZH, Ma QS et al (2007) Ceram Int 33:905
Jian K, Chen ZH, Ma QS et al (2007) Ceram Int 33:73
Jian K, Chen ZH, Ma QS et al (2005) Mater Sci Eng A 408:330
Shriver DF, Drezdzon MA (eds) (1986) The manipulation of air-sensitive compounds. Wiley, New York
Kumagawa K, Yamaoka H, Shibuya M et al (1998) Ceram Eng Sci Proc 19:65
Zhou MH, Kim SH, Park JG (2000) Polym Bull 44:17
Ma R, Song ZY, Hou YB et al (2009) J Macromol Sci A 46:193
Dean JA (ed) (1991) Lange’s chemistry handbook, 13th edn. Science Press, Beijing
Meng GR, Zhao L, Liang GZ et al (2001) Thermoset Resin 16: 34 (in Chinese)
Michael B, Anton LG (eds) (2001) In: Macromolecular symposia. Wiley-VCH, Berlin
Yu ZJ, Huang MH, Fang YH et al (2010) React Funct Polym 70:334
Fang YH, Huang MH, Yu ZJ et al (2008) J Am Ceram Soc 91:3298
Moraes K, Vosburg J, Wark D et al (2004) Chem Mater 16:125
Tang M, Yu ZJ, Yu YX et al (2009) J Mater Sci 44:1633. doi:10.1007/s10853-009-3246-9
Ogawa I (1997) Carbon 35:1846
Acknowledgements
The project was supported by the National Natural Science Foundation of China (Nos. 50802079, 20925208, and 50532010) and Natural Science Foundation of Fujian Province of China (2008J0165).
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Yu, Z., Zhan, J., Huang, M. et al. Preparation of a hyperbranched polycarbosilane precursor to SiC ceramics following an efficient room-temperature cross-linking process. J Mater Sci 45, 6151–6158 (2010). https://doi.org/10.1007/s10853-010-4701-3
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10853-010-4701-3