Abstract: Effects of the deposition parameters such as bath composition, pH and time on the element contents and deposition rate of the electroless Ni-Cu-P deposits were studied. The electroless Ni-Cu-P deposits with various copper contents from 0 to 56.18 wt% were prepared by choosing the proper deposition parameters. The effect of copper sulfate concentration in the bath on the composition and microstructure of the electroless Ni-Cu-P deposits was studied by X-ray energy dispersive spectroscopy (EDS) and X-ray diffraction(XRD). Ni-Cu-P deposits with phosphorus content more than7.05 wt% are amorphous, in the situation that the copper sulfate concentration in the bath is lower than 3 g/l.