This paper presents the results of the non-contact and non-destructive characterization of micro-porous SiC layers subjected to reactive ion treatment using Raman scattering, Scanning Electron Microscopy, and Atomic Force Microscopy. A comparative study of the Raman spectroscopy on the SiC wafer and the porous SiC layers has shown a number of new features specific for nano-crystallite materials, such as crystal disordering, changes of Raman polarizability tensors, appearance of the surface polariton modes and enhancement of the LO phonon-plasmon coupling. The influence of all these effects on modification of Raman scattering spectra have been discussed.