Here, 2% Cu + 2% Ni co-doped ZnO nanoparticles were synthesized using the hydrothermal method and were used as particle reinforcements of Cu-Ni nanocomposite coatings prepared by electroplating technology. The effects of the added (Cu, Ni) co-doped ZnO nanoparticles (2–8 g/L) on the phase structure, surface morphology, thickness, microhardness, corrosion resistance, and photocatalytic properties of the coatings were investigated. The nanocomposite coatings have obvious diffraction peaks on the crystal planes of (111), (200), and (220), showing a wurtzite structure. The surface of the nanocomposite coatings is cauliflower-like, and becomes smoother and denser with the increase in the addition of nanoparticles. The grain size, thickness, microhardness, corrosion resistance, and photocatalytic properties of the nanocomposite coating reach a peak value when the added (Cu, Ni) co-doped ZnO nanoparticles are 6 g/L. At this concentration, the mean crystallite size of the coating reaches a minimum of 15.31 nm, and the deposition efficiency of the coating is the highest. The (Cu, Ni) co-doped ZnO nanoparticle reinforcement makes the microhardness reach up to 658 HV. The addition of nanoparticles significantly improves the corrosion resistance and photocatalytic properties of nanocomposite coatings. The minimum corrosion current density is 2.36 × 10−6 A/cm2, the maximum corrosion potential is −0.301 V, and the highest decolorization rate of Rhodamine B is 28.73% after UV irradiation for 5 h.

2 at.% Cu + 2 at.% Ni were co-doped in ZnO nanoparticles by a simple hydrothermal method, and then the modified nanoparticles were compounded into Cu-Ni alloy coatings using an electroplating technique. The effects of the current density (15–45 mA/cm2) on the phase structure, surface morphology, thickness, microhardness, corrosion resistance, and photocatalytic properties of the coatings were investigated. The results show that the Cu-Ni-Zn0.96Ni0.02Cu0.02O nanocomposite coatings had the highest compactness and the best overall performance at a current density of 35 mA/cm2. At this point, the co-deposition rate reached its maximum, resulting in the deposition of more Zn0.96Ni0.02Cu0.02O nanoparticles in the coating. More nanoparticles were dispersed in the coating with a better particle strengthening effect, which resulted in a minimum crystallite size of 15.21 nm and a maximum microhardness of 558 HV. Moreover, the surface structure of the coatings became finer and denser. Therefore, the corrosion resistance was significantly improved with a corrosion current density of 2.21 × 10–3 mA/cm2, and the charge transfer resistance was up to 20.98 kΩ·cm2. The maximum decolorization rate of the rhodamine B solution was 24.08% under ultraviolet light irradiation for 5 h. The improvement in the comprehensive performance was mainly attributed to the greater concentration of Zn0.96Ni0.02Cu0.02O nanoparticles in the coating, which played the role of the particle-reinforced phase and reduced the microstructure defects.