Cobalt and nickel alloy powders were obtained by electrochemical deposition on a titanium cathode from an ammonium solution of cobalt and nickel sulfate. Powders of a specific chemical structure and composition, particle shape and size were obtained by an appropriate choice of electrolysis parameters, current density, deposit growth rate and solution temperature and composition. Within the current density range of 5 - 450 mAcm-2, the current density did not significantly affect the chemical composition of the powders, but had a significant effect on the particle structure, shape and size. Crystal particles formed at a current density lower than 30 mAcm-2. Amorphous powders were obtained at a current density higher than 50 mAcm-2. Structural changes of the obtained amorphous powder of 55mol.% Ni, 45 mol.% Co, pressed under the pressure of 100 MPa, were investigated by measuring the temperature dependence of electrical resistance in isothermal and non-isothermal conditions varying from room temperature to 750°C. The process of thermal stabilization of defects that appeared during pressing occurred within the temperature range of 200-390 C. The DSC method was used to determine that the powder crystallization process occurred in two stages with peak temperatures of the exothermal maximum in the first and second stage of T1 = 438 C and T2 = 573 C, respectively. A distinct correlation between the change of electrical resistance and the crystallization process was established. The reduction of electrical resistively occurs during each crystallization stage.