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Procedures to obtain nanocrystalline molybdenum disulfide were developed. The effect of the duration of mechanical alloying and heat treatment parameters on the structure and morphology of powders resulted was analyzed. The process was conducted in the Spex8000 mill under argon. The mixture of powdered molybdenum and sulfur of stoichiometric composition was milled. The structure and the morphology of the obtained materials were studied by SEM and XRD measurements. The diffraction lines of sulfur vanished after 75 h of the mechanical alloying. The additional heat treatment affected both the structure and the morphology of the powders. As result, nanoplates of molybdenum sulfide were obtained. After the heat treatment at 900 deg C, the nanoplates had an average thickness of about 50 nm.