The paper presents results of an analysis conducted over heating of nc-Ti-Si-C-N/C powder in argon atmosphere. TG-DSC-MS measurements were carried out under non-isothermal and isothermal conditions. The samples were heated up in series to 1573, 1673 and 1773 K. Four stages of the process were distinguished. In the first, endothermic stage, evolution of volatile products contained in raw samples took place. In the second, exothermic stage, oxidation of nc-Ti-Si-C-N/C contained in raw samples occured by the oxygen present in argon at a trace level. At the third stage pyrolysis of organic compounds, present in the samples, and carbonization of nc-Ti-Si-C-N/C, and in the fourth stage oxidation of purified composite by oxygen occurring in argon proceeded. Kinetic description of the process was presented at the example of series heated up to 1773 K. Coats-Redfern equation was applied. The kinetic models (forms of g(α) function) and Arrhenius parameters A and E were determined for the stages. An analysis of the process was performed using the obtained kinetic data.