A contrastive experiment was conducted by using 4 key process parameters, i.e. concentration of sodium tungstate, current density, pH value and temperature that have greater influences on the electro deposition of Ni-W alloy nanocrystalline. Influences on the deposition rate, microhardness and surface of plating were studied respectively, which would provide basis for the preparation of Ni-W alloy nanocrystalline. At the same time, the plating of Ni-W alloy nanocrystalline was obtained, the size of which was10.09 nm.