The paper presents the coal activation effect as disintegration in the nano-submicron range and destruction carbon structure. The Slovak brown coal activated in planetary mill is characterised by destruction of organic structure of coal. The biggest activation effect connected with the destruction of C-C bonds of sp(3) carbons has been confirmed by C-13 NMR spectroscopy in the chemical structure of humic acids extracted from the coal sample activated for a period of 60 min. The specific surface of humic acids is much smaller then that of mechanically activated sample from which they were extracted. The black Czech coal was activated by two stage disintegration. In the first stage of mechanochemical activation using Grinding Aqueous Caustic Leaching, GACL method a fine dispersed semiproduct is formed with the size of particles from 2.5 to 9000 nm. The additional disintegration using water jet increases the effect of disintegration in the submicron area of the coal product. The volume distribution maximum achieves in this stage about 60 wt% of 750 nm grains. (C) 2004 Kluwer Academic Publishers.