Nickel/ultra-dispersed PTFE composite films with various PTFE content are electrochemically prepared from a Watt's nickel plating bath in which the PTFE particles (mean diameter 0.3 μm) are suspended using a cationic fluorocarbon surfactant. The microstructures of Ni-PTFE composite films are analyzed by means of XRD, SEM and TEM, and their water-repellencies are also measured. The results indicate that the PTFE particles take a homogeneous distribution within all the composite films. The PTFE particle content in the composite films is dependent upon the particle concentration in the plating bath and the plating parameters, and strongly influence the physical properties of Ni-PTFE composite films such as water-repellency. The contact angle of a water drop on the surface of composite film with maximum PTFE content of about 47.4 vol% reaches 154.9°, showing a superior water-repellency.