Electrodeposition of Ni-Mo-P alloy coatings from ammoniacal citrate baths was studied, as well as characterization of low overpotential electrocatalysis for hydrogen evolution in alkaline solution. It was observed that the use of cathodes electrodeposited with Ni-Mo-P alloy containing 25 to 29 atomic percent molybdenum, and 0.1 to 0.8 atomic percent phospho rus, relative to Mo for water electrolysis, resulted in decreased overpotential for hydrogen evolution, Some scanning electron microscope (SEM) observations were also made.