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Nanocomposites (PMSEPE/Q8M8H) were prepared via solution blending of octakis(dimethylsiloxy)octasilsesquoixane (Q8M8H) into poly(dimethylsilyleneethynylenephenyleneethynyle ne) (PMSEPE). PMSEPE/Q8M8H nanocomposites were characterized by Fourier transform infrared (FT-IR) spectroscopy, rheological measurement, differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and thermal gravimetric analysis (TGA). The experimental results show that the hydrosilylation reaction in PMSEPE/Q8M8H nanocomposites occurs slowly exceeding 180℃. PMSEPE/Q8M8H nanocomposites can be cured at temperatures less than 260℃and the cube structure of Q8M8H keeps stable during the curing process. POSS domains are evenly dispersed in the cured nanocomposite. However, serious aggregation of POSS occurs at 15%Q8M8H content. The thermal and thermooxidative stabilities of PMSEPE/Q8M8H nanocomposites obviously depend on the content of Q8M8H. The incorporation of Q8M8H can effectively enhance the thermal and thermooxidative stabilities of cured PMSEPE. PMSEPE/Q8M8H nanocomposites can be the candidates for applications in high temperature environment.

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