Diffusion and homogenization in powder systems of varying degrees of dispersion «iron (5 μm) – nickel (5 μm or 50 nm)» during sintering (900 and 1000 °C), as well as spark plasma sintering using the Matano-Boltzmann method were studied. In these systems, the calculated diffusion coefficients in pairs of micron powders, sintered without application of pressure (900 °C, 6 h) and the spark plasma method (900 °C, 5 min), were equal to 7·10–10 cm2/s. It is shown that in diffusion pairs based on microdispersed iron powder, the use of nanodispersed nickel powder instead of microdispersed one contributes to an increase in the diffusion coefficient at a temperature of 900 °C by a factor of 2. The constants in the sintering kinetics equation of V.A. Ivensen are calculated for iron–nickel powder systems. Through them the factors activating the sintering of these systems were established. The dependences of the structure-phase composition and physicomechanical properties of carbides of the Fe (base) system — 14 wt.% Ni – 8 wt.% TiC system on the sintering temperature in the interval t = 900÷1200 °C, dispersion and homogeneity of the structure were determined. The dependences of grain size, porosity, hardness, microhardness, toughness, bending strength on sintering temperature are shown. The established dependences of the tribotechnical properties on the degree of homogeneity of the solid solution and the volume of the phase transformation of the metastable austenite to deformation martensite during friction on the abrasive were similar for carbide steels and diamond tools based on carbide steels. The optimal values of the coefficient of variation of nickel concentration in austenite in carbidostils of the same chemical composition, but different dispersion, providing the maximum amount of austenite decomposition and high values of the diamond tool grinding coefficient were 5 in both systems, but the sintering parameters differed. It is shown that the physicomechanical properties of the studied systems depend on the porosity and dispersion of the structure, and the tribotechnical properties are subjected to the homogeneity of the structure of the steel.