The effect of thermal annealing on structure and mechanical properties of amorphous SiC
xN
y (
y ≥ 0) thin films was investigated up to 1500°C in air and Ar. The SiC
xN
y films (2.2–3.4 μm) were deposited by reactive DC magnetron sputtering on Si, Al
2O
3 and α‐SiC substrates without intentional heating and at 600°C. The SiC target with small excess of carbon was sputtered at various N
2/Ar gas flow ratios (0–0.48). The nitrogen content in the films changes in the range 0–43 at.%. Hardness and elastic modulus (nanoindentation), change in film thickness, film composition, and structure (Raman spectroscopy, XRD) were investigated in dependence on annealing temperature and nitrogen content. All SiC
xN
y films preserve their amorphous structure up to 1500°C. The hardness of all as‐deposited and both air‐ and Ar‐annealed SiC
xN
y films decreases with growth of nitrogen content. The annealing in Ar at temperatures of 1100°C–1300°C results in noticeable hardness growth despite the ordering of graphite‐like structure in carbon clusters in nitrogen free films. Unlike the SiC, this graphitization leads to hardness saturation of SiCN films starting above 900°C, especially for films with higher nitrogen content (deposited at higher N
2/Ar). This indicates the practical hardness limit achievable by thermal treatment for SiC
xN
y films deposited on unheated substrates. The ordering in carbon phase is facilitated by the presence of nitrogen in the films and its extent is controlled by the N/C atomic ratio. The suppression of graphitization was observed for N/C ranging between 0.5–0.7. Films deposited at 600°C show higher hardness and oxidation resistance after annealing in comparison with those deposited on unheated substrates. Hardness reaches 40 GPa for SiC and ~28 GPa for SiC
xN
y (35 at.% of nitrogen). Such a high hardness of SiC film stems from its partial crystallization. Annealing of SiC
xN
y film (35 at.% of N) in Ar at 1400°C is accompanied by formation of numerous hillocks (indicating heterogeneous structure of amorphous films) and redistribution of film material.
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