Influence of Nitrogen Flow Ratio on the Microstructure, Composition, and Mechanical Properties of DC Magnetron Sputtered Zr–B–O–N Films

Nanocrystalline ZrB2 film and nanocomposite Zr–B–O–N films were prepared by non-reactive as well as reactive magnetron sputtering techniques, respectively. By means of X-ray diffraction analysis, electron probe microanalysis, X-ray photoelectron spectroscopy, and scanning electron microscopy, the influence of nitrogen flow ratio on the film microstructure and characteristics were investigated systematically, including the deposition rate, chemical compositions, phase constituents, grain size, chemical bonding, as well as cross-sectional morphologies. Meanwhile, the hardness and adhesion of above films were also evaluated by micro-indentation method and a scratch tester. With increasing the nitrogen flow ratio, the deposition rate of above films decreased approximately linearly, whereas the contents of N and O in the films increased gradually and tended to saturation. Moreover, the film microstructure was also altered gradually from a fine columnar microstructure to a featureless glass-structure. As the nitrogen flow ratio was 11.7%, the Zr–B–O–N film possessed an typical nanocomposite structure and presented good mechanical properties. During the process of reactive sputtering of metal borides, the introduction of nitrogen can show a pronounced suppression of columnar grain growth and strong nanocomposite structure forming ability.