Composite Ni+Al layers were prepared by co-deposition of nickel and aluminium particles on a steel substrate from a nickel plating bath in which Al powders were held in suspension. The electrodeposition was carried out under galvanostatic conditions at a temperature of 323 K. These layers are characterized by the presence of Al micro-particles embedded into the nanocrystalline nickel matrix. The embedding mechanism of solid particles into the layers structure was explained basing on Ni²⁺ adsorption/desorption processes on the metal powder. Obtained layers could be applied as semi-finished products to obtain Ni-based layers containing the intermetallic phases as well as novel electrode materials in electrochemistry. The influence of Al content in the electroplating bath on the chemical composition of obtained layers was investigated. It was found that Al content in the layers was an increasing function of metal powders amount in the bath. The maximum Al content was 44 wt% for the Ni+Al layers, respectively. The size of the nickel crystallites has been determined from the diffraction peaks half-widh (27 nm). Basing on phase diagrams for Ni+Al systems. The heat-treatment in argon atmosphere of deposited layers under proposed conditions leads to obtain different intermetallic phases of Ni with Al.

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