Amorphous and microcrystalline films of silicon and silicon carbide have been deposited by means of PECVD at low substrate temperature (200°C), with reactive gases highly diluted in H2. Devices quality a-Si:H films have been annealed in vacuum at temperatures in the range 200- 1000 °C. The transition from amorphous to crystalline structure was studied by X-ray, Raman and I.R. spectroscopies, optical analysis in UV-VIS-NIR region, Transmission Electron Microscopy, Differential Scanning Calorimetry and Electron Spin Resonance measurements. By comparing the results of the two methods to obtain microcrystalline films we have deduced information on the process of growth of Si and SiC microcrystals.