Nanocrystalline semiconductor particles MeS (Me=Pb, Zn, Cd, Cu) were successfully synthesized by the mechanochemical route from the corresponding metal acetates and sodium sulphide in an industrial eccentric vibratory mill. Structure properties of the as-prepared products were characterized by X-ray powder diffraction which reveals the crystalline nature of MeS nanoparticles. The methods of TEM, particle size analysis and low temperature nitrogen sorption were used to analyze particle morphology and surface area measurement. The average sizes of MeS particles at 4-18 nm were estimated by Scherrer's formula. The main advantage of the application of an industrial mill is that it is a "quantity" process permitting kilograms of material to be produced in an ambient temperature in a very short processing time. (c) 2006 Elsevier B.V. All rights reserved.