Abstract: The effects of different electrodeposition conditions in the pulse plating process to prepare Ni-Mo coating on its composition, apparent morphology and HER (hydrogen evolution reaction) activity were investigated. If the quantitative ratio of nickel to molybdenum is lower than 1 (mol%), the Mo content in the coating decreases gradually with the molybdenum salt adding to the coating, while the corresponding HER overpotential increases. The Ni-Mo coating thus prepared presents amorphous structure (w(Mo)=30%) in combination with homogeneous, smooth and characteristics, especially it provides a higher catalytic activity (80°C, η200=62 mV) with high corrosion resistance. After the galvanostatic electrolysis in 33% NaOH solution for 100 hr, the amorphous structure is destroyed due to Mo dissolution, then the bubbling comes to pass with increasing porosity.