Abstract⎯Using solid-phase pyrolysis of Zn-phthalocyanine (ZnC 32 H 16 N 8 ), we have prepared zinc and zinc cyanide nanoparticles in carbon matrices with a zinc concentration of 3 at %. The structure and composition of samples were investigated by the methods of scanning electron microscopy, X-ray diffraction, and Raman spectroscopy. It is shown that at low pyrolysis temperature (700°C) only the Zn nanoparticles are formed, whereas at higher temperature (900°C) a certain amount of Zn(CN) 2 nanoparticles are also synthesized. The mean diameter of nanoparticles is about 150 nm, and their size distribution has a logarithmically normal shape.