In recent decades, there has been a great deal of interest in conducting polymers due to their broad applications. At the same time, various synthetic techniques have been developed to produce various nanostructures of the conducting polymers with their fascinating properties. However, the techniques for the manufacture of 2D nanosheets are either complex or expensive. No comprehensive approach for constructing 2D and 3D materials or their composites has been documented. Herein, a simple and scalable synthetic protocol is reported for the design of 2D, 3D, and related conducting polymer nanocomposites by interface manipulation in a bicontinuous microemulsion system. In this method, diverse bicontinuous thin layers of oil and water are employed to produce 2D nanosheets of conducting polymers. For the fabrication of 3D polypyrrole (PPY) and their composites, specially designed linkers of the monomers are applied to lock the 3D networks of the conducting polymers and their composites. The technique can be extended to the fabrication of most conducting polymer composites, being cost‐effective and easily scalable. The optimum electrical conductivity obtained for 2D PPY nanosheets is 219 S cm−1, the highest literature value reported to date to the best of knowledge.
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