The article discusses the microstructure of the ZnSb intermetallic compound obtained by powder technology and the results of the study of charge transfer processes in it. Also, the article proposes a method of preparing a Zn-Sb intermetallic compound with a stem-shaped polycrystalline structure using powder technology. Semiconductor Zn-Sb polycrystalline structure preparation method is carried out by pressing Zn-Sb particles together, followed by thermal treatment in several stages. It was found that the stages and temperature of heat treatment have a significant effect on its electrophysical properties. Electrical conductivity (σ), charge carrier concentration (n) suddenly decreases with temperature increase at the initial stage of heat treatment. Such a process is not observed in the subsequent stages of heat treatment. At all stages of heat treatment, the mobility of charge carriers (μ) decreases. In this case, the residence time of charge carriers in the crystal lattice is π~1,52÷1,1·10-12 sec. was determined to change between The results of the study were explained on the basis of the influence of intergranular boundary areas on charge transfer processes. Studies show that at T=300÷700 K, the potential barrier height (φ) in the intergranular boundary areas increases linearly with temperature. For example, φ~0,436 eV at the initial stages of thermal treatment at T=300 K, and φ~0,469 eV at later stages, and at T=700 K, it increases to φ~0,92 eV in all cases. It was shown that it depends on the amount of charges trapped in the localized traps in the intergranular boundary regions.