N. BARNAKOV, G. P. KHOKHLOVA, A. N. POPOVA, S. A. SOZINOV and Z. R. ISMAGILOV Institute of Coal Chemistry and Material Science, Federal Research Center of Coal and Coal Chemistry, Siberian Branch, Russian Academy of Sciences, Kemerovo, Russia E-mail: barnakov@rambler.ru Abstract X-ray powder diffraction is one of the most potential characterization tools and a nondestructive technique for characterizing carbon based materials and their composite properties. <...> The method is used to measure phase identification, quantitative analysis and to determine structure imperfections of samples. <...> As it turned out the carbonaceous materials obtained by the low-temperature graphitization of coal-tar pitch contain contemporaneously several phases of crystalline carbon and amorphous carbon with turbostratic structure. <...> In the present report, to explain the heterogeneous structure of carbonaceous materials we compare data of X-ray diffraction analysis for the (00l) reflection from the main crystal face. <...> It was found that the (002) and (004) reflections are the superpositions of components, which correspond to the structural phases of crystalline carbon and amorphous carbon with different interplanar spacing. <...> The ratio between the integrated intensities of separated reflection components accounts for the ratio between these phases; along with interplanar spacing, this ratio characterizes carbonaceous materials and makes it possible to detect difference between them. <...> The degree of ordering, the interlayer spacing (d002), and the crystalline sizes (La and Lc) are considered the key parameters for evaluating the stacking structure of carbonaceous materials. <...> Key words: coal pitch, graphite additives, carbonization, X-ray diffraction analysis 569 INTRODUCTION The crystal structures of carbonaceous materials are commonly studied by the X-ray diffraction analysis (XRD), which produces a profile associated with the crystallite size and arrangement of atoms. <...> Numerous investigations have estimated the sizes of carbon layers and the stacking structure of carbonaceous materials using XRD [16]. <...> This review presents the results of the comparative studies of the one structure of carbonaceous materials (CM) by means of XRD analysis using the method of the asymmetric peak deconvolution. <...> The carbonaceous materials obtained by the low-temperature graphitization of coal-tar pitch and some commercial graphite samples were used for study. <...> The coal-tar pitch graphitization process was carried out in the presence of the following catalytic <...>