Nickel‐cobalt alloys were electrodeposited on copper sheets in sulfate bath containing 288.5 g/l NiSO4·6H2O, 30 g/l CoSO4·7H2O, 40 g/l HBO3, 15 g/l NaCl and 0.08 g/l lauryl sodium sulfate. The effects of cobalt content on microstructure, microhardness, and wear resistance of electroplating nickel‐cobalt alloys were studied by using SEM and XRD techniques, and microhardness tester and wear tester. The relationship between the microhardness of nickel‐cobalt alloy coatings and heat treatment procedures was also investigated. The experimental results show that cobalt content (Wt) in coating increases with Co2+/(Co2+ + Ni2+)% (X) in plating solution. Fitted regression equation is as following: Wt = –0.7399 + 2.2847X – 0.0133X2. The increase of cobalt content leads to that the longitudinal section morphology of coating transforms from the cone into sphericity and at last into the shape of willow leaf, and its structure transforms from face centered cubic (fcc) nickel solid solution into fcc cobalt solid solution and at last into hcp cobalt solid solution. The increase of cobalt content results in the increase of microhardness of nickel‐cobalt alloy coatings, and the hardness reaches a maximum value (363 HV) when cobalt content is 54.9%. After heat treatment at 400°C and 600°C, the microhardness of coatings begins to decrease except the coating containing 79.2% Co. Moreover, the wear resistance of electroplated coatings increases with the increase of cobalt content.
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