Abstract. AZ31B was used as the basic material in electroless Plating of Ni-Co-P, The optimium formula and process conditions were obtained by using the orthogonal experiment methods. XRD, SEM and EDS were used to characterize phase structure,compositon and morphology of Ni-Co-P coating. The morphology,corrosion resistance, composition ,hardness,thickness and binding force of coating are measured and analysed. The optimum formula and the technological conditions were gained as follows:26.0g/L NiSO 4 ·6H 2 O ,28.0g/L CoSO 4 ·7H 2 O,24.0g/L NaH 2 PO 2 ·H 2 O,80.0g/L Na 3 C 6 H 5 O 7 ·2H 2 O,60.0g/L NH 4 F ,temperature of 90.0℃,0.001g/L KI, 0.05g/L SDBS ,the plating time of 2.0 h and pH of 8.0.Under this condition, the coating had stronger corrosion resistance, drop time for KMnO 4 solution was 272s; The hardnesses was 229.60HV ;the deposition rate was faster, up to 53.33 g·m -2 ·h -1 ;thickness was 12.43 μm;the surface of the coating was uniform;the distribution of porosity was smaller;there was well-bonded with the substrate.