Effect of oxygen on degradation of defects on ta-C coatings deposited by filtered arc deposition

Among diamond-like carbon (DLC) coatings, tetrahedral amorphous carbon (ta-C) coatings show particularly high thermal stability and oxidation resistance due to their high sp3 content and hydrogen-free structure. On the other hand, it is well known that high-temperature annealing leads to degradation of the ta-C structure, resulting in a release of stress, decrease of hardness, increase in surface roughness, and transformation of the coating nature. Although optical observation is a powerful candidate for imaging the surface conditions of ta-C coatings, strong light emission due to high temperature prevents the acquisition of clear images. In this paper, we establish a novel in situ observation method using environment scanning electron microscopy (ESEM), which allows us to view ta-C surface defects and droplets at 650 °C. A heater embedded in the ESEM increased the temperature on ta-C coatings to 650 °C at gas pressure of 120 Pa. Using a variety of gas conditions including ambient air, dry nitrogen, or dry oxygen, we clarified the effect of the gases on the degradation of the defects. In a dry oxygen atmosphere, defects grew dramatically with annealing time, whereas nitrogen caused no significant transformation to ta-C surfaces. Raman spectroscopy analysis revealed significant structural change in one type of defect, while no noticeable Raman shift was detected in the other type. A focused ion beam created a cross-section of an annealed defect on the ta-C coating. Subsequently, energy dispersive X-ray spectroscopy (EDS) revealed the characteristics of defect growth; one type of defect was associated with a droplet on the interlayer, and the other with graphitization due to oxidization of ta-C on the droplets.