By using the solid-phase pyrolysis of phthalocyanines the nickel-carbon nanocomposites have been synthesized. The composition, structure, and morphology of samples were investigated by scanning electron microscopy and Raman spectroscopy. The first-order Raman shifts of prepared materials were measured with laser excitation at 514.5 nm in the frequency range from 900 to 2000 cm-1. It is shown that the degree of graphitization in nanocomposites essentially depends on the pyrolysis temperature. By analyzing the intensity ratio of Raman D- and G-bands the mean sizes of graphitic nanocrystallites in prepared samples were estimated.© (2010) COPYRIGHT SPIE--The International Society for Optical Engineering. Downloading of the abstract is permitted for personal use only.