A kind of novel Ni–P gradient coating/stannate conversion film was deposited on AZ91D magnesium alloy (AZ91D alloy) by an integrative method involved stannate conversion and electroless plating. The results indicated that using sodium hypophosphite concentrations varied as 5, 10, 22, 46, and 60 g/L in the bath, the electroless Ni–P gradient coating with typical cell morphologies was successfully prepared, and the structures transited from crystalline → microcrystalline → amorphous were obtained as increasing P content from 3.31 to 12.58 wt%. Furthermore, the corrosion morphologies, polarization curves, and the electrochemical impedance spectroscopy result indicated that the corrosion resistance of AZ91D alloy substrate was significantly improved and the corrosion resistance of Ni–P gradient coating was superior than that of stannate conversion film, which might be attributed to the gradient structure and rising P content with unique function.
