Abstract The study investigated the influence of the method of mechanical milling (milling in a ball mill and in an intensive attritor) on the size and structure of particles of Cu powder in preparation of ultrafine dispersion strengthened Cu powder mixture - 5% by volume CuO.Al2O3 using a mechanical-chemical method. The experimental observations indicated that the preparation of the powder mixture in question by mechanical milling in a ball mill was unsuitable because, due to low energy of milling, an uniform distribution of dispersoid particles could not be reached and the presence of particle agglomerates in the structure of the material decreased the effective volumetric proportion of particles of the secondary phase. The mechanical milling in an intensive attritor was suitable for preparation of the powder mixture mentioned as it enabled to obtain sufficient fineness of particles of the matrix metal as well as uniform distribution of fine dispersoid particles in the matrix. The study also discusses the influence of the method of milling on the character of structure of the compact material prepared from the given powder mixtures. The structure of the powder mixture entering the process of compacting affects significantly the character of structure of the resulting compact material. The compact material prepared from the powder mixture, subjected previously to grinding in a ball mill, exhibited a coarser structure and a more pronounced deformation texture in comparison with the material prepared from the attritor-ground mixture.