Abstract: Experiments were performed to investigate the effects of the key factors such as the mass concentrations of adding sulfur agent TS and additive SB as well as current density on the sulphur content and physical appearance of nickel buttons. Differences in electrochemical activity were analyzed between the 1^# electrolysis nickel and the products of activated nickel buttons. The process and the optimum parameters of adopting the soluble anode electrolysis with nickel sulfide were decided for developing the activated nickel buttons by experiment. The optimum technological conditions were obtained as follows:the mass concentrations of adding sulphur agent TS and additive SB are 7.53 mg·L^-1 and 36.97 mg·L^-1 respectively, the average apparent current density is 1300 A·m^-2, and other technological parameters are the same as those of the 1^# electrolytic nickel. Nickel buttons with smooth surface and regular shape were developed at the parameters above, which contain sulphur from 0.01% to 0.03%. The products possess high electrochemical activity, and their chemical composition accords with the requirements of the 1^# electrolysis nickel. The technology has been used in industry, and the products meet the requirements of special plating anodes for the precision electroplating industry.