Polymer(Korea), Vol.23, No.2, 197-203, March, 1999
백금촉매에 의한 PCS-co-MPS 세라믹 전구체의 합성과 열분해 특성
Synthesis of PCS-co-MPS Ceramic Precursor with Platinum Catalyst and Its Pyrolysis
초록
백금촉매를 이요한 hydrosilylation 반응에 의해 높은 수율의 세라믹 전구체를 얻기 위해서 polycarbosilane-co-methacryloxypropyltrimethoxy silane (PCS-CO-MPS)을 합성하였다. 합성한 시료의 FT-IR 스펙트럼에서 2100, 1720, 1640, 1170, ⅰ130 cm-1 부근에서의 흡수 피크 변화와 ¹H-NMR의 4.1, 3.5, 1.8 ppm 부근에서 특성 피크를 확인해 시료의 합성을 확인하였다. 또한 1500 ℃까지 열분해시킨 후 29Si-NMR 분석결과 δ=-60, -109 ppm 부근에서 특성 피크와 X-ray회절 분석결과 2θ=34, 61, 78°에서 결정성 피크로 β-SiC의 전환을 확인하였고, PCS-co-MPS의 열분해 전환율은 87,5%로 PCS에 비해 18.2%가 증가함을 보였다.
In order to increase the yield of the ceramic precursors, copolymers of polycarbosilane(PCS) and γ-methacryloxypropyltrimethoxy silane (γ-MPS) were synthesized by hydrosilylation with platinum catalyst. The structures of PCS-co-MPS ceramic precursors were investigated by using FT-IR and 1H-NMR spectrometers. The syntheses of ceramic precursors were confirmed by monitoring the change of the absorption bands appearing at 2100, 1720, 1640, 1170, 1130 cm-1 on the FT-IR spectra. The syntheses of eramic precursors were also confirmed by the presence of peaks at 4.1, 3.5, 1.8 ppm on the 1 H-NMR spectra. The conversion of PCS-co-MPS copolymers was around 87.5% and 18.2% higher than that of the pure PCS. After the heat-treatment at 1500 ℃, the crystalline peaks for β-Sic were observed at-60, -109, ppm on the29 Si-NMR spectra, and at 2θ=35°, 59° and 71° on the X-ray spectra, respectively. It showed the conversion of ceramic precursors to crystalline β-SiC.
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