The corrosion properties of Ni-Cr-W-Mo-B alloy sprayed by the high velocity oxy-fuel spraying (HVOF) was studied as a function of heat treatment by using both potentiodynamic polarization and immersion tests in the H₂SO₄ solution. The mechanical property was also evaluated by a microhardness tester. Microstructural characteristics of te as-sprayed and annealed coatings at 550, 750 and 950℃ have been analyzed by means of OM, XRD, SEM and TEM. The results showed that the corrosion resistance was improved by increasing the annealing temperature. As-sprayed coating had metastable and heterogeneous phases such as amorphous, nanocrystalline and very refined grain and precipitates, which induced a localized corrosion. The localized corrosion occurred preferentially at the unmelted particles which were composed of Ni matrix and Cr, W and Mo riched phase segregated in the boundaries. As annealing temperature was increased, the microstructure had shown some changes - reduction of porosity and s[plat boundary decomposition and crystallization of amorphous/nanocrystalline phases, grain coarsening,, formation and growth of precipitates such as {TEX}$M_{23}C_{6}${/TEX} and {TEX}$M_{7}C_{3}${/TEX}. In addition, the compositional difference between matrix and boundary phases gradually disappeared, which changed the corrosion type from localized corrosion to general corrosion and thus enhanced corrosion resistance.