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In this report, g-C 3 N 4 -based photocatalysts with dual co-catalysts of amorphous NiS and carbon black were firstly synthesized through a facile two-step process. The g-C 3 N 4 /carbon black/NiS composite photocatalyst were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), ultraviolet–visible spectroscopy (UV–vis), N 2 adsorption, photoluminescence (PL) spectra and transient photocurrent responses. The photocatalytic activities for photocatalytic hydrogen evolution under visible light irradiation ( λ ≥ 420 nm) were measured using an aqueous solution containing triethanolamine as an electron donor. Moreover, the results showed that the ternary g-C 3 N 4 photocatalyst loaded by 0.5 wt% carbon black and 1.5 wt% NiS could achieve the highest H 2 -production rate of 992 μmol g −1 h −1 under visible-light irradiation (>420 nm), which is about 2.51 times higher than that of the corresponding binary g-C 3 N 4 /1.5% NiS photocatalyst. It is believed that the enhanced photocatalytic H 2 -evolution activities could be attributed to the excellent synergetic effect between the carbon black and NiS as co-catalysts on the surface of g-C 3 N 4 , leading to the improved visible light absorption, promoted charge separation and enhanced the following H 2 -evolution kinetics. This work would not only demonstrate the promising potentials of carbon black as co-catalyst for applications in visible-light H 2 generation, but also offer a new insight into the construction of highly efficient and stable g-C 3 N 4 -based hybrid semiconductor nanocomposites with dual co-catalysts for diverse photocatalytic applications. [ABSTRACT FROM AUTHOR]