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The study on the development of nickel electroplating technology and the reduction effect of a wastewater was performed. Through the experiments by emulsion solution of methanol/electrolyte/surfactant, the optimized electrolyte concentration was 60 wt% at constant concentrations of methanol and surfactant and the optimum concentration of surfactant was 10 wt% at constant concentration of electrolyte and methanol. With a conventional method, nickel nano-particles on the plated film were observed to be lumped. However, nickel particles were observed to be densely and constant with needlelike conformation and their durability was excellent with supercritical nano-plating system by using emulsion solution of 60 wt% electrolyte, 10 wt% surfactant, and 30 wt% methanol. Especially, the dispersion effect of nickel nano-particles was more improved with the agitation. A wastewater amount from the plating process by a supercritical plating system more decreased by 80% than that by a conventional method and the used amount of electrolyte more decreased by 20%, too.