Duplex Ni-P-TiO2/Ni coatings were deposited on the brass substrate by using two baths. Ni-P-TiO2 nanocomposite coatings were electroplated as the outer layer on the Ni-plated brass substrate by adding transparent TiO2 sol (0–50 mL/L) into the Ni-P plating solution. The microstructure, mechanical property and corrosion resistance of the duplex Ni-P-TiO2/Ni nanocomposite coatings were systemically investigated. The results show that the interface of duplex coating was uniform and the adhesion between two layers was extremely good. The microhardness of duplex Ni-P-12.5 mL/L TiO2 /Ni coating was [Formula: see text]616 HV[Formula: see text] compared to [Formula: see text]539 HV[Formula: see text] of Ni-P /Ni coating and [Formula: see text]307 HV[Formula: see text] of single Ni coating. Meanwhile, the wear resistance and the corrosion resistance of the duplex nanocomposite coating have also been improved remarkably compared with single Ni coating. However, adding excessive TiO2 sol (more than 12.5 mL/L) caused the agglomeration of TiO2 nanoparticles and led to a porous structure in the outer layer, resulting in the deterioration of coating properties.