Morphology Control of Highly Sulfonated Block Copolymers by a Simple Thermal Process

Well‐defined sulfonated block copolymers were prepared by direct thermolysis with block copolymers of n‐butyl acrylate (nBA) and neopentyl styrene sulfonated (NSS), which were synthesized by Cu‐based living radical polymerization ( <1.20). A simple thermal process for 10 min at 150 °C completely deprotected the neopentyl groups in the poly(NSS) block segment to give fully sulfonated polystyrene backbone. SAXS profile of the block copolymer with 47 wt.‐% of poly(NSS) showed lamella structure, which appeared more clearly with long ranged order after sulfonation of the block copolymer.