Synthesis and characterization of novel preceramic polymer for SiC
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Polyphenylcarbosilane as a novel preceramic polymer for SiC was synthesized by thermal rearrangement of polymethylphenylsilane at around 350–430 °C. Characterization of the synthesized polyphenylcarbosilane was performed using 29Si NMR, 13C NMR and 1H NMR spectroscopy, FT-IR spectroscopy and TG, XRD, and GPC analysis. From the FT-IR data, the band at 1035 cm−1 was very strong and was assigned to the CH2 bending vibration in the Si–CH2–Si group, indicating the formation of polyphenylcarbosilane. The average molecular weight (Mw) of the polyphenylcarbosilane synthesized was 2,500, and it was found to easily dissolve in an organic solvent. TGA data indicate that polyphenylcarbosilane is thermally stable up to 200 °C. However, rapid weight loss occurs above 200 °C because of the decomposition of polyphenylcarbosilane, and the diffraction peak of the pyrolysis residue at 1200 °C corresponds to β-SiC ceramic. The ceramic yield calculated from TGA is approximately 60%.
KeywordsThermal Gravimetric Analysis Thermal Gravimetric Analysis Curve Ceramic Yield Thermal Rearrangement Pyrolysis Residue
This work was supported by the Korea Science and Engineering Foundation (KOSEF) grant funded by the Korea government (MOST) (No. R01-2007-000-20320-0). The authors would like to thank Dr. Duk-Young Han in Korea Basic Science Institute, Seoul Branch for his assistance in data collection of the samples using Solid NMR, 200B instrument. J.-H.-P.K.’s work for methyltriphenylsilane structural studies was supported under the auspices of the US DOE by LLNL under Contract DE-AC52-07NA27344. Single crystal X-ray diffraction data collection of methyltriphenylsilane was carried out at the Advanced Light Source (ALS). ALS is supported by the Director, Office of Science, Office of Basic Energy Sciences, of the U.S. Department of Energy under Contract No. DE-AC02-05CH11231.
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