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An indium and phosphorus co-doped g-C3N4 photocatalyst (In,P-g-C3N4) was prepared by K2HPO4 post-treatment of an indium-doped g-C3N4 photocatalyst (In-g-C3N4) derived from in situ copolymerization of dicyandiamide and indium chloride. The experimental results and theoretical simulations revealed that the doped indium ions were located between the planes of g-C3N4 and phosphorus atoms were introduced into the g-C3N4 plane by replacing the carbon atoms, which existed in the form of P＝N bonds. The co-doping of indium and phosphorus with g-C3N4 not only extended its response to the visible light region but also synergistically promoted the separation and migration of photogenerated charge carriers. As a result, the In,P-g-C3N4 photocatalyst exhibited a hydrogen evolution rate as high as 4.03 mmol h−1 g−1, ca. 50 times that of pristine g-C3N4 (0.08 mmol h−1 g−1). [ABSTRACT FROM AUTHOR]