The first successful synthesis of conjugated rod–coil star block copolymer, (PF‐b‐P2VP)n, containing conjugated poly[2,7‐(9,9‐dihexylfluorene)] (PF), and coil‐like poly(2‐vinylpyridine) (P2VP) by combining a Suzuki coupling reaction and living anionic polymerization is reported. With increasing methanol content in THF/methanol mixtures (PF‐b‐P2VP)n symmetric star‐block copolymers maintain spherical micelles, but PF‐b‐P2VP asymmetric diblock copolymers vary from spherical micelles to vesicles. Both the absorption and emission spectra of PF‐b‐P2VP blue shift with increasing methanol content, suggesting an “H‐type” aggregation. However, (PF‐b‐P2VP)n star‐block exhibits no shift in absorption but a red shift in the emission spectra, indicating a different type of aggregation. These results suggest the significance of polymer architectures on microphase‐separated morphologies and photophysical properties. magnified image
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