A new quaternary Ni-Fe-P-C composite coating was deposited on copper substrates by an electrodeposition process. The morphology, structure and composition of the prepared electrode were characterized using scanning electron microscopy (SEM), Xray diffraction (XRD) pattern, and energy dispersive X-ray spectroscopy (EDX). The activity of the composite coating toward hydrogen evolution reaction (HER) was evaluated on the basis of the steady-state polarization Tafel curves and electrochemical impedance spectroscopy (EIS) in 1 M NaOH at temperature of 298 K. The experimental results revealed that the HER activity of the Ni-Fe-P-C coatings was enhanced compared with both ternary coatings of NiP -C and Ni-Fe-C. The source of its activity was found from its high surface area and its intrinsic properties. It was sufficient to assume the Volmer-Heyrovský mechanism with the Heyrovský reaction as the ratedetermining step to explain the experimental data. Besides the high electrocatalytic activity, excellent chemical and electrochemical stability were observed for Ni-Fe-P-C composite coating toward the HER in 1 M NaOH at 298 K.