A tri-layer amorphous Ni-P alloy coating was prepared in the same bath by changing the temperatures and currents, followed by heat treament. We studied the behavior of corrosion-resistance of the tri-layer coating before and after heat-treatment at 360°C for different time in the 5% NaCl solution. The result showed that: the tri-layer amorphous Ni-P coating has the excellent performance of anti-corrosion compare with single electroless or electrodeposited Ni-P amorphous coating. The performance of anti-corrosion of the coating was improved by controlling the coating’s structure and the role of electrochemical protection. After being heat-treated at 360°C for 1 hour ,the coating’s structure changed from amorphous to crystalloid and the corrosion resistance of the heat-treated coatings was higher than as-plated tri-layer Ni-P coating.