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In order to improve the performance and fundamental understanding of conducting polymers, development of new nanotechnologies for engineering aggregated states and morphologies is one of the central focuses for conducting polymers. In this work, we demonstrated an interfacial engineering method for the rational synthesis of a two-dimensional (2D) polyaniline (PANI) nano-array and its corresponding nitrogen-doped porous carbon nanosheets. Not only was it easy to produce a sandwich-like 2D morphology, but also the thickness, anchored ions and produced various metal phosphides were easily and rationally engineered by controlling the composition of the aqueous layer. The novel structural features of these hybrids enabled outstanding electrochemical capacitor performance. The specific capacitance of the as-produced diiron phosphide embedded nitrogen-doped porous carbon nanosheets was calculated to be as high as 1098 F g−1 at 1 A g−1 and an extremely high specific capacitance of 611 F g−1 at 10 A g−1, outperforming state-of-the-art performance among porous carbon and metal-phosphide-based supercapacitors. We believe that this interfacial approach can be extended to the controllable synthesis of various 2D material coupled sandwich-like hybrid materials with potential applications in a wide range of areas.