Summary: A series of helix‐coil diblock copolymers based on poly(ethylene oxide) and optically active helical poly{(+)‐2,5‐bis4′‐((S)‐2‐methylbutoxy)phenyl]styrene} (PMBPS) were synthesized via atom transfer radical polymerization (ATRP). The synthetic methodology permitted straightforward preparation of the diblock copolymers with relatively low polydispersities and a broad range of compositions and molecular weights. Depending on the composing block length and the initial concentration, the copolymers self‐assembled into different supramolecular structures in aqueous solution, including spherical micelles, vesicles, multilamellar vesicles, large compound vesicles, and tubules.
Schematic representation of the synthesis of PEO‐b‐PMBPS block copolymers and their aggregation in aqueous solution.