ZnFeNi alloys were synthesized galvanostatically in a sulfate bath at constant current values of 1, 1.5, and 2 mA on the carbon steel surface. The synthesized alloys were characterized by scanning electron microscopy, energy-dispersive X-ray analysis, and linear sweep voltammetry methods. The corrosion performances of the alloys were examined by electrochemical impedance spectroscopy, anodic polarization curves, and open-circuit potential-time techniques. Based on the anodic polarization curves, it was determined that the alloy with the lowest corrosion current was the ZnFeNi-1.5 alloy synthesized at a constant current value of 1.5 mA. By electrochemical impedance spectroscopy, it was determined that the alloy with the highest polarization resistance during long exposure to a corrosive environment was ZnFeNi-1.5. By examining the anticorrosive properties, it was understood that the alloy that showed the best protective properties against the corrosion of carbon steel was ZnFeNi-1.5.