We present a new phase separation phenomenon “nanophase separation”, which occurred in comb-shaped polymers. We have found that comb-shaped polymers such as poly(alkyl acrylamides) and poly(alkyl acrylates) formed a highly oriented lamellar structure by annealing the film under humid condition. The effect of temperature and humidity to the lamellar formation suggested that the nanophase separation, which is the phase separation between alkyl side chains and main chain is the driving force for the lamellar formation. We combined the nanophase separation to the microphase separation in block copolymer to prepare a vertically aligned nanocylinder film.
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