Electroless Ni-P/nano-CeO 2 composite coating was prepared in acidic condition, and its microstructure and corrosive property were compared with its CeO 2 -free counterpart. Scanning electronic microscopy (SEM), transmission electronic microscopy (TEM) and differential scanning calorimeter (DSC) were used to examine surface morphology and microstructure of the coating. Aqueous corrosion was done in 3%NaCl+5%H 2 SO 4 solution and high temperature oxidation was done at 750 in air. The results showed that Ni ℃ -P coating had partial amorphous structure mixed with nano-crystals, while the Ni-P/CeO 2 coating had perfect amorphous structure. At high temperature, Ni 3 P precipitation and Ni crystallization took place in both coatings at different temperatures. Aqueous corrosion property and high temperature oxidation property of the composite coating were remarkably improved due to the coating's microstructure change and the rare earth doping effect. During the co-deposition process, some Ce n+ (n=3, 4) ions may be adsorbed to metal/solution interface and hinder nickel deposition. Ni-P/CeO 2 coating's perfect amorphous structure results from the hindered crystal-typed deposition of nickel and the promoted deposition of phosphorous.