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<sup>-1</sup>. 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.