The friction and wear behavior and microstructure of an Ni/MoS2 composite plating layer with high MoS2 content and sufficient thickness produced by a brush plating method were studied. Experiments were conducted using a 'pin-on-disc' testing machine in vacuum with a pressure of approximately (6-9) x 10(-4) Pa. The plating layer was produced on the surface of the disc. The experimental results show that the friction coefficient can only reach a lower stable value when the MoS2 content is more than 31.6% in volume, and the minimum friction coefficient of 0.014 can be obtained at 78% MoS2 content. In order to reveal the mechanism for the excellent solid lubrication properties of Ni/MoS2 plating layers, detailed analyses were conducted of the microstructure and orientation of grains by transmission electron microscopy. The codeposition process of both nickel and MoS2 phases is also discussed.