| Summary: | Silicone resin is a high-temperature resistant material with excellent performance. The improvement of its thermal stability has always been the pursuit of researchers. In this paper, a sequence of silicone resins containing trifluorovinyl ether groups were prepared by the co-hydrolysis-polycondensation of methyl alkoxysilane monomers and {4-[trifluorovinyl(oxygen)]phenyl}methyldiethoxysilane. The structures of the silicone resins were characterized by FT-IR and <sup>1</sup>H NMR. The curing process of them was studied by DSC and FT-IR spectra, and results showed that the curing of the resins included the condensation of the Si-OH groups and the [2 + 2] cyclodimerization reaction of the TFVE groups, which converted to perfluorocyclobutane structure after curing. The thermal stability and thermal degradation behavior of them was studied by TGA and FT-IR spectra. Compared with the pure methyl silicone resin, silicone resins containing TFVE groups showed better thermal stability under both N<sub>2</sub> and air atmosphere. Their hydrophobic properties were characterized by contact angle test. Results showed that PFCB structure also improved the hydrophobicity of the silicone resin.
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