Nanocrystalline nickel and Ni-Fe alloy coatings were synthesized by brush plating using soluble anode. The corrosion characteristics of nanocrystalline nickel, Ni-5.84%Fe and Ni-13.49%Fe alloys were investigated by soak a method and an electrochemical polarization method, respectively. The experimental results indicate that the typical nanocrystalline nickel and Ni-Fe alloy coatings can be synthesized by brush plating, and the alloying element Fe has the effects of solution strengthening and grain size refinement. The nanocrystalline Ni-13.49%Fe alloy is dense in nature and pore free, and exhibits better corrosion resistance in a 3.5 wt% NaCl solution than the nanocrystalline nickel. In 10 wt% HCl solution, the nanocrystalline Ni-13.49%Fe alloy also shows a good corrosion resistance as the nanocrystalline nickel. The surface morphology of all samples after corrosion show a spot corrosion feature in 3.5 wt% NaCl solution, however, the samples are uniformly corroded in 10 wt% HCl solution.