A detailed study was made of the influence of the sulphate bath constituents: 0.3 - 0.0125 NiSO 4·7H 2O (I), 0.05 – 0.23 (NH 4) 2SO 4 (II), 0.1 – 0.4 H 3BO 3 (III) and 0.07 – 0.35 mol l −1 Na 2SO 4·10H 2O (IV) on the electrodeposition of nickel powder. The cathodic polarization, current efficiency, growth morphology, crystallite size and catalytic activity of the electrodeposited nickel powders were affected to different extents by the bath constituents. A highly pure nickel powder characterized by a small crystallite size (776 Å) and moderate catalytic activity was obtained from a bath containing: 0.0125 (I), 0.23 (II), 0.1 (III) and 0.07 mol l −1 (IV) at a current density of 10 A dm −2 and electrolysis time 60 min. at 25 °C. Structural studies with a scanning electron microscope are given and a reaction mechanism for the electrolytic powder deposition is discussed.