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[Display omitted] • The porous few-layer bimetallic co-doped g-C 3 N 4 is prepared via a facile bottom-up method. • The bimetallic synergetic regulating effect on the electronic structure can be produced in Co/Ni-g-C 3 N 4. • The superior performance results from the improved charge separation efficiency and visible light harvestability. • This work provides meritorious guidance for new bimetallic co-doped g-C 3 N 4 photocatalysts. The low specific surface area and low charge transfer efficiency of conventional graphite carbon nitride (g-C 3 N 4) are the main obstacles to its application in photocatalytic CO 2 reduction. In this paper, graphite carbon nitride was protonated by phosphoric acid (H 3 PO 4), and a new few-layer porous carbon nitride was prepared by intercalation polymerization with doping bimetal in the cavity of g-C 3 N 4. Under visible light irradiation, the CO formation rate of Co/Ni co-doped g-C 3 N 4 can reach 13.55 μmol g−1 h−1, which was 3.9 times higher than that of g-C 3 N 4 (3.49 μmol g−1 h−1). The density functional theory (DFT) calculations showed that the addition of Co and Ni in the cavity of g-C 3 N 4 can induce bimetallic synergistic regulation of the electronic structure, thus improving the separation efficiency of charges and visible light capture ability of g-C 3 N 4. Our work has great reference value for designing and synthesizing novel bimetallic co-doped g-C 3 N 4 photocatalytic materials. [ABSTRACT FROM AUTHOR]