Nanocrystalline ZrB2 film and nanocomposite Zr-B-O-N films were prepared by non-reactive as well as re- active 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 depo- sition 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 de- creased 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.
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