The electrochemical behaviour of nickel(II)-rhenium(VII) and the electrodeposition of nickel-rhenium alloy using choline chloride: 2 Urea deep eutectic solvent (Reline DES) is reported. Speciation of nickel(II)-rhenium(VII) in Reline DES was studied using UV -Visible spectroscopy. Cyclic voltammetry of Ni2+-ReO4 − in Reline indicates the simultaneous reduction of two metal ions at glassy carbon electrode controlled by non-reversible diffusion process. Chronoamperograms obtained for the reduction of Ni2+-ReO4 − suggests nucleation and three-dimensional growth of bimetallic phase on electrode surface followed progressive nucleation. Electrodeposition of nickel—rhenium alloy was carried out on copper substrates under galvanostatic and potentiostatic conditions. Smooth and uniform deposits were obtained by galvanostatic deposition. X-ray diffraction analysis of the deposit confirmed it to be nickel-rhenium alloy (at −1.2 V) in amorphous form which upon annealing at 1000 °C crystallizes into hexagonal phase with concurrent morphology change from spherical particles to irregular polygons.
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