Zinc-nickel alloys, as protective coatings, are well known and a new citrate bath has been investigated. It was observed that boric acid favoured nickel deposition playing the dual role of specific adsorption and catalysis. The voltammetric behaviour of the alloy deposition in the presence of boric acid is described. The effect of Ni/Zn ratio, and potential scan range on the cathodic and anodic portions of the voltammograms are discussed. The presence of two cathodic peaks at high Ni/Zn ratios, which disappeared at lower ratios was identified.