Earlier we showed [2] that hcp-phase Re0,30lr0,70 was metastable. This phase under the pressure of 1 GPa and the temperature of 1900 °C undergoes a structure transformation forming the phase for 5 minutes with fee lattice of the same composition. Study of possible phase transformations of Re0,67Rh0,33 solid solution nanosized powder under high pressurehad been carried out in this work. It was specified that two-phase mixture formed under the pressure of 1.5 GPa, the temperature of 2000 °C and the exposition time of 3 and 5.5 minutes consist of RexRh1-x (x = 0.57 и 0.60) solid solution based on initial structure of Re0 67Rho 33 and hcp-phase which is hypothetically intrusion solid solution based on rhenium and carbon elements. Under the pressure of 4 GPa, temperature of 2000 °C and exposition time of 3 minutes single-phase solid solution that coincided with the composition of initial Re0,67Rh0,33 (a = 2.748(1), с = 4.384(2) A) was obtained. Value of microhardness in the obtained sample was 800 kg/mm2.