In this work, the results of investigations of manufacturing ceramic materials on the basis of Ti, B, C and N containing systems are presented. The nanocrystalline ceramics were synthesized using a non-hydrolytic sol-gel method. The process was carried out in two stages. In the first low-temperature stage the precursor was obtained. The synthesis of ceramic phases, however, was conducted in the second high-temperature stage, in an argon atmosphere. Depending on the initial composition of the mixtures, the temperature and the time, the following products were obtained: TiCx, TiCxN1−x, TiB2 and B4C.The course of the process was investigated by thermogravimetric and differential scanning calorimetry methods (TG-DSC) coupled with mass spectrometry (MS). The solid state products were identified with use of X-ray diffraction (XRD). The size of the crystallites was estimated by the Scherrer method. The structure and morphology images of nanocrystalline powders were obtained using scanning electron microscopy (SEM) and transmission electron microscopy (TEM).