Abstract: In this study, pulse electrodeposition method of Au-Bi alloy micro-target preparation was advanced by a cyanide-free alkaline plating system. The alloy composition can be effectively controlled (controlling of bismuth content from 1.5% to 9.5%) by the regulation of bath composition and pulse parameters, the using of sulfite-tartrate salt bath system. And the deposition of bismuth and gold was achieved. At the same time, impacting of temperature, current density and the concentration of bismuth on the content of alloy and surface morphology of coatings were researched. And optimal formula and process parameters of preparation of alloy micro-target were obtained through experiments. The corresponding optimum concentrations are as follows: Bismuth chloride 6 g/100 mL, gold 0.15 g/100 mL, potassium sodium tartrate 12.50 g/100 mL, ammonia 0.85 mL/100 mL, ammonium sulfite 6.50 mL/100 mL, kalium chloride 5.00 g/100 mL, potassium citrate 5.50 g/100 mL, SDS 0.002 g/100 mL, antimony potassium tartrate 0.035 g/100 mL, frequency 500 Hz, average current 65 μA, duty ratio 1∶7, temperature 45 ℃. And Au-Bi alloy micro-targets possess properties such as plane and bright surface, low porosity according to above optimal formular and process parameters.