In this work, Cu atoms and Al2O3 nanoparticles were simultaneously incorporated into a Ni coating during an electrodeposition process to produce Ni-Cu/Al2O3 nano-composite coatings. Then, the effect of the additions of the Cu and Al2O3 species on some properties of these coatings was investigated. X-ray diffraction and scanning electron microscopy equipped with energy dispersive X-ray spectroscopy were employed for the structural characterization of the products. The mechanical properties of the deposited coatings were also investigated by Vickers microhardness and pin-on-disc wear testing. Also, the corrosion behavior of the produced coatings was investigated in a NaCl solution. Results showed that the addition of Cu atoms and Al2O3 nanoparticles changes the texture of the pure Ni coating and decreases the crystallite size from 91 nm for pure Ni to 16 nm for Ni-Cu/Al2O3 (20 g/L) nano-composite coating. It was also found that the microhardness, wear resistance, and corrosion resistance of the deposited coatings are increased by the incorporation of Cu atoms and Al2O3 nanoparticles in the Ni coating. Typically, the microhardness and wear resistance are increased about 2.4 and 3.75 times, respectively.