The technique of ultra-small angle x-ray scattering (USAXS) has been applied in parallel with the x-ray diffraction (XRD) method for structural studies of bulk nanoporous carbon (NPC) materials chemically produced from polycrystalline SiC powders. It is shown that graphite-like quasi-2D nanoclusters can be formed on carbonization of the SiC precursor under certain technological conditions. The size parameters of the clusters, their concentration, and volume fraction have been estimated.