In the present research, the process of the formation of the active components of Pd-Zn catalysts supported on carbonaceous material Sibunit prepared by the joint impregnation (Pd:Zn=1) is studied. It was shown by means of TPR and EXAFS techniques that the interaction between palladium and zinc begins already at T > 200 degrees C. During the reduction in hydrogen at temperatures of 200-300 degrees C the surface of particles being formed is enriched with oxidized zinc. In the temperature range of 400-500 degrees C zinc is completely reduced, and the crystal lattice of a substitutional solid solution based on fcc lattice of palladium is restructured in tetragonal lattice of PdZn. However, an increase of the calcination temperature in H-2 atmosphere (500 degrees C) significantly rises up the probability of partial destruction of bimetallic phase due to the partial migration of zinc atoms from the surface into the bulk of particles.