Amorphous Si1-xCx /SiC multilayer films were prepared by alternating deposition of Si-rich Si1-xCx and near-stoichiometric SiC layers by using magnetron sputtering. The as-deposited films were annealed at different temperatures Ta from 800 to 1100 oC. The influence of Ta and Si content in the Si-rich layer on the layered structural stability and on the formation of Si and/or SiC nanocrystals NCs is investigated by a variety of analytical techniques, including x-ray reflectivity XRR, x-ray diffraction XRD, transmission electron microscopy TEM, Raman spectroscopy, and Fourier transform infrared spectrometry FTIR. XRR showed that Si1-xCx /SiC multilayers annealed at temperatures of up to 800 oC retain their layered structure. XRD revealed that Si NCs were formed in samples with a high Si content in the Si-rich layer for Ta 800 oC. At annealing temperatures of 900 oC or greater, the formation of Si NCs was accompanied by the formation of -SiC NCs. Additionally, the formation of Si and SiC NCs was confirmed by TEM imaging and Raman spectroscopy. The Si-NC size obtained from the TEM micrographs is within the range of 3-5 nm. The -SiC NCs are smaller 2-3 nm than Si NCs. Raman analysis identified an 9 cm-1 Raman peak shift in the Si-NC peak to a lower energy with respect to that for bulk Si. FTIR Si-C bond absorption spectra exhibited narrowing of the full width at half maximum and a peak shift toward a higher wave number with increasing Ta. This behavior can be explained by an increase in order as well as an increase in the number of Si-C bonds.