AbstractIn this study, a simple pickling process in H3PO4 and NH4HF2 solution was used for electroless Ni–P plating on AZ61 magnesium alloy. It is found that the corrosion rate of magnesium alloy during pickling significantly decreased because NH4HF2 was added into H3PO4 pickling solution. Ni–P coating plated only with pickling process shows poor adhesion because of the low F/O ratio of the substrate surface. However, F/O ratio, adhesion, and corrosion resistance of Ni–P coating are obviously enhanced after pickling followed by activation. The optimal pretreatment process is pickling for 120 s and activation for 4 min, under which the Ni–P coating has an optimum F/O ratio of 1.8 and the coating gets a dense structure, better adhesion, and higher corrosion resistance.