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A series of novel hybrid poly(acetoxylstyrene-co-isobutylstyryl-POSS)s (PAS−POSS) and poly(vinylpyrrolidone-co-isobutylstyryl-POSS)s (PVP−POSS) are synthesized and characterized. The POSS content in these hybrids can be controlled by varying the monomer feed ratio. The polyhedral oligosilsesquoixane (POSS) moiety can effectively increase the T g of the resultant organic/inorganic hybrid polymer at a relatively high POSS content and produce the hybrid copolymer with narrower molecular weight distribution. The FTIR spectra are used to investigate the structure−property relationship of these hybrid polymers, and the T g enhancement mechanism is discussed in detail.

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