Mechanochemical synthesis (mechanosynthesis) by high-energy ball milling enables mixing of components on atomic level and preparation of materials with unique properties. The aim of this work is directed to evaluation of composition and properties of Zn,,De, Sn and Mb sulphides prepared by mechanochemical route. The results have shown that ZnS, Ni3S2, FeS(5C), SnS2 and Nb1-xS can be synthetized together with the by-products of surface mechanochemical oxidation. Contamination from mill atmosphere (air) and grinding media (Fe) strongly influences the quality of mechanosynthetized products. The method of XRD, XPS and Mossbauer spectroscopy were used for surface and bulk characterization of new structures as well as wear from grinding media.