A microwave plasma technique has been employed to deposit polycrystalline diamond film over a molybdenum substrate button using a gas mixture of hydrogen and methane at a substrate temperature of 851°C. A CVD diamond coated molybdenum substrate button was mounted with a load against hot nickel plate and rotated for 3.45 h in a hydrogen ambient. Hot tungsten filament was used as a heat source to maintain the temperature of the nickel block and CVD diamond coated molybdenum button at 848°C. This experiment has reproducibly shown the successful polishing of polycrystalline CVD diamond by hot nickel. A Tencor profilometer and scanning electron microscope have been used to evaluate the surface smoothness and morphology before and after polishing the polycrystalline diamond thin films.