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Increasing the hardness and wear resistance of powder alloys and coatings through the use of ultrafine-grained powders and metastable phases is a promising way in powder metallurgy. This paper presents the results of the studies of the process of obtaining ultrafine powders by the electric discharge erosion of the cemented carbide waste WC-5TiC-10Co on a special installation. An empirical model that describes the dependence of the productivity of the process on the discharge energy and properties of the liquid is provided. The dependence of the chemical and phase compositions of the obtained powder on the composition of the used liquid and specific energy consumption has been investigated. The effect of the discharge energy on the morphological composition and average particle diameter has been examined. It is revealed that the formation of a metastable solid solution (W, Ti)C and a decrease in the concentration of cobalt induce an increase in the hardness of the resulting spherical particles from 1410HV0.05 to 2540HV0.05.