AbstractSinglet oxygen was used to synthesize hydroperoxide functional groups onto a polybutadiene. These hydroperoxides served as grafting sites for the preparation of polybutadiene‐modified polystyrene by a bulk polymerization process. As anticipated, the dispersed polybutadiene droplet size decreased as the level of hydroperoxidation increased. Various types of morphology, similar to those of butadiene–styrene diblock and styrene–butadiene–styrene triblock copolymer systems, were obtained. Furthermore, at an extremely high level of hydroperoxidation, a unique reticular structure of polybutadiene was de
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