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A novel polyhedral oligomeric octadiphenylsulfonylsilsesquioxane (ODPSS) was synthesized from octaphenylsilsesquioxane and benzenesulfonyl chloride via a Friedel-Crafts reaction with a high yield. ODPSS was identified by Fourier transform infrared spectroscopy, 1 H-NMR, 13 C-NMR, 29 Si-NMR, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS), wide-angle X-ray diffraction, and elemental analysis to be a kind of polyhedral oligomeric silsesquioxane of a T 8 R 8 structure. ODPSS exhibited superior thermal stability according to thermogravimetric analysis. Its initial thermal decomposition temperature (T onset ) was at 491 C in air and 515 C in nitrogen. Thermal and mechanical properties of epoxy resin (EP) composites with ODPSS added were studied by differential scanning calorimetry and tensile testing. The results show that the incorporation of ODPSS at a low loading content not only improved the glass-transition temperature of the EP composites but also enhanced their tensile strength.