The PtCo/C electrocatalyst obtained by the method of simultaneous reduction of metal precursors using sodium borohydride was treated at a temperature of 350 ˚C in an argon atmosphere for 1 hour. The results of X-ray phase analysis and transmission electron microscopy indicate an increase in the average size of crystallites and the formation of nanoparticle agglomerates after heat treatment. The shift in the reflection of Pt (111) after treatment indicates the possible segregation of metal components during the heating of the sample. An increase in the catalyst activity after heat treatment is shown, both mass activity and specific activity. The stability of the sample after heat treatment, according to the results of the stress test in the potential range of 0.6–1.4 V, showed a higher value than the material in the “as prepared” state.