Diamond films which have high hardness and thermal conductivity can be used to improve the performance of WC-Co as a cutting tool material. However, it is difficult to get such coatings of good uniformity and adhesiveness due to the surface characteristics of WC-Co. To get better coatings, some techniques, such as the surface treatment of substrate or the formation of interlayer between substrate and diamond film, have been tried. In the present work, the nickel interlayer is formed onto WC-Co by electroless Ni-P plating, which is introduced as a new method, and then diamond film is deposited on the interlayer. Formation and uniformity of three layers, i.e., substrate, electroless plate, and diamond film, and the adhesiveness of interlayers were studied. To investigate the effects of pretreatment on electroless plating, two different methods such as acid treatment and diamond powder treatment were used. The effects of heat treatment of the electroless plated surface on adhesiveness between the substrate and the interlayer were examined. It was found that as the temperature increases, the Ni crystals grow and then result in improved adhesiveness. Diamond film coatings of pure diamond phase were obtained at 800℃. It is concluded that the heat treated electroless Ni-P plating can be effectively used as a interlayer between WC-Co substrate and diamond film.