The influence of cyclic treatment in reducing and oxidizing gas atmospheres (redox cycling) at temperatures of 600 and 800°C on the structure, strength, and conductivity of YSZ–NiO ceramics for the anode substrates of ceramic fuel cells is investigated. At a temperature of 600°C, we observe the formation of a structure guaranteeing the improved physical and mechanical properties of the material. However, the anode structure with a grid of microcracks is formed after treatment at 800°C. This significantly reduces the strength and the conductivity of the material. According to the data of thermodynamic and X-ray analyses, the accumulated results are referred to the effect of the elevation of temperature on the intensification of the process of oxidation of nickel phase and on the growth of residual stresses.