Simultaneous deposition of both nickel and chromium in the form of alloy is a subject with pronounced practical significance in automobile industries. Electroplating of Ni-Cr alloy has been carried out using suitable plating bath solution and working conditions. The alloys are partially crystalline and new phases appear on heat-treatment of the coating. Surface morphology and microstructure of the coating are closely related to the nature of the bath components, bath composition, alloy composition, and post-treatment of the coating. X-ray photoelectron spectroscopy studies indicated that the alloy contains nickel in +2 and +3 oxidation states, whereas it contains chromium in the +3 oxidation state in the deposited Ni-Cr coating. The sputtering of the coatings up to 20 min changed the nickel and chromium to metallic state. The coated alloys exhibited good corrosion resistance to acidic media, e. g., 0.5 M H2SO4, 1 M HCl, and 5% NaCl (pH 5), and heat-treatment of the coating enhanced the corrosion resistance. (c) 2006 The Electrochemical Society.