In this work, the physicochemical properties of mechano-activated composites (hereinafterreferred to as the mechanocomposites)obtained by mechanical activation of commercial tungsten disulfide powder in a planetary emill were studied. Mechanical activation was carried out for 2, 4 and 8 h, but this work presents the results for the last two experiments. The acceleration of the grinding media was controlled through frequency adjustment; a frequency value of 15.5 Hz, ac-cording to calculations, corresponds to an acceleration of the grinding media of 50 m/s2or 5G. The material of the balls from which the grinding balls are made is stainless steel. Due to the relatively low acceleration values, the problem of contamination of the sample with stainless steel compo-nents does not occur as a result of surface erosion that occurs when the balls collide with each other and with the walls of the grinding bowl. Mechanical activation was carried out in an inert argon environment, since these were preliminary studies and therefore there was a need to mini-mize the environmental parameters taken into account. However, the oxidation process will occur during the process of discharging the sample from the grinding bowl of the planetary mill. The resulting mechanocomposites are precursors for the synthesis of monocomponent catalysts for the processing of heavy oil residue. For this purpose, it is necessary to obtain mechanocomposites con-taining tungsten trioxide and tungsten disulfide. The results of an experimental study of the influ-ence, mainly, of the duration of mechanical activation on the production of tungsten mechanocom-posites are presented. The resulting compounds were characterized by X-ray phase analysis (XRD), IR spectroscopy, scanning electron microscopy (SEM), thermogravimetry (TGA) and simultaneous thermal analysis (STA)