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In this research, the authors develope a novel organic/inorganic hybrid system by using a highly crystalline π‐conjugated polymer poly(3‐butylthiophene) (P3BT) as a structure‐regulating template. The efficient coordination between thiophene segments in P3BT and zinc ions as well as the formation of cooperative assembly of P3BT/Zn2+ complex system enable the facile synthesis of ZnO nanocrystals on one‐dimensional P3BT nanofibrils after a thermal oxidation treatment. The nanowire structured P3BT/ZnO system with optimized nanoscopic phase separation possess large donor/acceptor interfacial area for exciton dissociation and offers continuous channels for charge transport through the hybrid, leading to a significant photoluminescence quenching effect. Accelerated aging tests further demonstrate the superior thermal stability of the hybrid system. These results demonstrate that the in situ synthesized P3BT/ZnO nanohybrid could serve as a high quality optoelectronic material and show potential for advanced applications.

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