The Ni-B-Mo coating on steel by electroless plating and the evaluation of the morphology and corrosion performance after applying heat treatments at different temperatures for 1 h were investigated in this study. The 25-lm-thick coating was uniform and adhesion between the substrate and the coating was good. The coating consisted of an amorphous-like structure in their as-plated condition, and after annealing at 400°C for 1 h, crystallized nickel, nickel borides, and molybdenum carbide were formed. Immersion tests in 10% HCl solution and potentiodynamic polarization measurements in 3.5% NaCl aqueous solution were applied to investigate corrosion resistance. The corrosion performance of heat-treated coatings was compared with steel and the as-plated coating. By increasing the annealing temperature, corrosion potential shifted toward a noble direction, corrosion current density decreased and the weight loss of specimens decreased, demonstrating an increase in corrosion resistance. Best corrosion performance was achieved by the coating heat treated at 550°C .