Herein, we develop a cascade growth strategy to fabricate laminated heterostructures based on graphdiyne (GDY), which can not only retain the intrinsic structure of GDY to the maximum extent, but also realize the effective regulation of its basic properties. The chlorine heteroatom doped GDY film (Cl-GDY/GDY) is prepared through coupling the hexaalkynylbenzene on the copper substrates which are pre-decorated with chlorine substitute GDY (Cl-GDY). An interweaved aggregating morphology consisting of nanofiber and nanosheets is observed, which can be assigned to Cl-GDY and GDY components, respectively. Moreover, the interaction between Cl-GDY and GDY induces the tunable energy level structure. As a result, the conductive properties of Cl-GDY/GDY films are tuned in an order of magnitude rather than the simple superposition of the two components, which can be clearly observed in both the carbon/electrolyte electrochemical cell and the carbon-based heterojunction device.

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