The electroless nickel-phosphor coatings containing molybdenum disulfide nanoparticles were prepared and analyzed in this paper. The effects of incorporation of MoS2 into the Ni-P coating on the morphology of the coating surface and corrosion properties were also studied. Corrosion tests were conducted inside a salt spray box with NaCl solution (5.0 wt%). The corrosional surfaces were studied and analyzed through optical microscope, X-ray spectrometer (XRD) and scanning electron microscopy (SEM). The investigation on the relationship between heat-treatment and the corrosion resistance of the coatings showed that the corrosion resistance of the composite coating became worse because of the occurrence of transformation from non-crystalline to crystalline, and then increased the metastable intergradation of the composite coating. Meanwhile, the experimental results also showed that corrosion resistance of the coating containing MoS2 was higher than that of steel substrate. The corrosion mechanism of the composite coatings was mainly ascribed to the formation of micro-cell around the nanosized MoS2 particles, and the active ion like Cl- destroyed the surface film and induced the corrosion towards the inside part of coating.