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Polystyrene (PS)/poly(ethylene oxide) (PEO) prototype brushes were prepared by alternating free-radical copolymerization of methacryloyl-terminated PS and ␣-vinylbenzyl--hydroxy or ␣-vinylbenzyl--perfluoroalkyl (R f ) PEO macromonomers with the addition of Lewis acid (SnCl 4 ). It was found from their dilute-solution properties that PS/PEO end-capped with R f (PBR f ), and PS/PEO having OH groups at terminal ends (PBOH) prototype brushes formed a single molecule in benzene and aggregates in chloroform, respectively. However, the brush PBOH formed a single molecule in N,Ndimethylformamide. Such aggregation behaviors seemed to be caused by the interaction between hydroxy groups of PEO chain ends. The brush PBOH was also converted into PBR ftype brush by chemical modification, using corresponding acid chloride. The substitution of R f groups was ϳ70% due to slipping of terminal hydroxy groups into PEO internal domains.

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