Abstract Mechanical activation of solid substances is one of the component of the modern scientific discipline of mechanochemistry. At present, mechanochemistry appears to be a science with a sound theoretical foundation which exhibits a wide range of potential aplication. Amongst the commercially operating processes: modification of the properties of building materials, a new method of producing slow – dispensing medical drugs, new method for obtaining of fertilizers, a method of activation and regeneration of catalysts, control of reactions in chemical technology and preparation of advanced materials. During the history of development of mechanochemistry the number of applied identification methods gradually increased. At the beginning, these methods were directed to at obtaining the characteristics of mechanically activated solid substances, mostly in integral form. This activity encompassed for example, the measurement of specific surface area by sorption methods and the determination of the content of crystalline phase by the methods of X – ray diffraction, etc. At present, the number of methods applied in investigation of mechanically activated substances comprises a few tens. These methods are thoroughly analyzed in special monographs. The paper deals with a present knowledge about the use of selected methods for characterization of nanostructure and surface properties of materials. STM (scanning tunneling microscopy), AFM (Atomic force microscopy), TEM and HRTEM (Transmision electron microscopy and High – resolution transmission electron microscopy) as progressive methods for identification in the field of nanoscience are described. Further, principles and advantages of particulary methods are clarified and several applications for synthesis of iron (II) sulphide and cadmium (II) sulphate are given .