Composite Ni+Mo coatings were obtained by electrodeposition of Ni with Mo particles on a steel substrate from the nickel bath in which metallic powder was suspended by stirring. Deposition was conducted under galvanostatic conditions. Deposits were characterized by the presence of Mo microsize particles embedded into the nanocrystalline nickel matrix. The influence of metal powder amount in the bath, as well as deposition current density on the chemical composition of coatings was investigated. It was stated that the content of incorporated Mo increases with the increase in the amount of metal powder in the bath, and diminishes with the increase in deposition current density. The mechanism of metallic particles embedding was explained on the base of Ni²⁺ ions adsorption process. Incorporation of Mo powder into electrolytic nickel matrix causes an increase in the real surface area of deposits.
Thermal treatment of deposited coatings leads to chemical reactions in the solid state and in a consequence exerts significant influence on their phase composition and surface morphology. As a result of interaction between the nickel matrix and incorporated Mo particles Ni₃Mo intermetallic phase and Ni-Mo solid solution are arising.
The obtained composite coatings were tested as electrode materials for hydrogen evolution in alkaline environment. Electrochemical characterization of the composites was carried out by steady-state polarization method. It was ascertained, that as-deposited Ni+Mo coatings are characterized by enhanced electrochemical activity for this process, which was confirmed by considerable decrease in the hydrogen evolution overpotential, by a nearly 170-260 mV compared to nickel electrode. Thermal treatment decreases electrochemical activity of investigated materials, as the values of hydrogen evolution overpotential on heated coatings are much higher.

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