Electroplating using a Ni-plating solution/CO2 macroemulsion was carried out at a supercritical condition. This method is that the Ni+2 ions in the macroemulsion using a surfactant have been deposited onto Cu. For forming the macroemulsion, we synthesized the fluorocarbonhydrocarbon surfactants, that is, sodium salt of bis (2,2,3,3,4,4,5,5-octafluoro-1-pentanol) sulfosuccinate with both ‘CO2 philic’ chains and the ‘hydrophilic' head group. The Cu plate, screw and chip as complicated shaped metals were plated by using this method. And the plated ware performed by this method was compared with that performed by the conventional method (electroplating at 1atm) to evaluate the effectiveness of the effective plating process.