Ni-S-Fe alloy has been successfully fabricated on a copper foil substrate through direct current electrodeposition as an electrocatalyst for hydrogen evolution reaction (HER) in alkaline solution. The Ni-S-Fe alloy is characterized with X-ray diffraction (XRD), scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS). The electrocatalytic performance of Ni-S-Fe alloy for HER is studied in 30 wt% KOH solution. The results show that the Ni-S-Fe alloy exhibits much higher catalytic activity for HER relative to Ni-S alloy, as manifested by smaller overpotential of 222 mV at 10 mA cm(-2) and higher exchange current density of 1.60 x 10(-2) mA cm(-2). The Tafel slope of 84.5 mV.dec(-1) implies an underlying Volmer-Heyrovsky mechanism. The outstanding catalytic performance of the Ni-S-Fe alloy may originate from the synergistic effects of Ni and Fe, refined grain, and enlarged surface area of Ni-S-Fe alloy upon Fe doping. In addition, the Ni-S-Fe alloy has better anti-corrosion property than Ni-S alloy as a result of the poorer crystallinity of Ni-S-Fe alloy. (C) 2017 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.