Electroless Ni-Cu-P deposits were deposited on the Si substrate in a basic hypophosphite-type plating bath. The effects of pH value and the metal source composition, Ni and Cu, in the plating bath on the kinetics of the Ni-Cu-P deposition were studied. The electroless Ni-Cu-P deposits were characterized by a scanning electron microscope, a transmission electron microscope, an energy dispersive X-ray spectroscope, and an X-ray diffractometer. The results showed that the pH value of the plating bath had no obvious effect on the morphology and composition of electroless Ni-Cu-P deposits. However, the composition of the metal source, Ni and Cu, in the plating bath had great effect on the kinetics of electroless Ni-Cu-P deposition.