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SiOx/DLC films were deposited on Si substrates using CH4/(C2H5O)4Si/Ar gas mixtures by PECVD. The films deposited were identified as atomic-scale composite networks consisting mainly of diamond-like a-C:H and silica-like a-Si:O structures with a smaller contribution of Si-C and C-O bonds. Structural modifications of SiOx/DLC films were monitored under thermal annealing in an Ar atmosphere. The structural transitions of the amorphous carbon matrix in the SiOx/DLC films were investigated by a Raman spectrometer. The relationships between the microstructural modifications and mechanical properties are discussed.