Objective of this work is to study the electrodeposition conditions of Ni and Ni-W alloy owing to its catalytic capabilities in electrolysis of water in alkaline medium for hydrogen production at low temperatures [1] which is of increasingly considered a clean and promising source of energy, Electrochemical measurements by cyclic voltammetry and chronoamperometry, morphological and structural analysis by SEM and EDX were exploited. The synthesis of Nickel-Tungsten alloys has been made possible by the modification of the watt bath. The electrodeposited alloys are characterized by a remarkable stability in corrosive medium (NaCl 3.5%), the W element is an improving corrosion resistance factor, tungsten preferentially migrates on the surface to form tungsten oxides [2] the Ni-W alloy is an excellent catalytic cathode to produce hydrogen by electrolysis in an alkaline medium KOH (25%). It has been found that these properties are closely related to the synthesis conditions: applied potential, temperature, pH and electrolyte composition.