The cyclic treatment technique (redox cycling) comprising stages of material exposition in reducing and oxidizing high-temperature environments and intermediate degassing between these stages has been developed to improve the structural integrity of YSZ-NiO ceramic anode substrates for solid oxide fuel cells. A series of specimens were singly reduced in a hydrogenous environment (the Ar-5 vol% Н2 mixture or hydrogen of 99.99 vol% H2 purity) under the pressure of 0.15 MPa or subjected to redox cycling at 600 or 800 °C. The influence of redox cycling at the treatment temperatures of 600 and 800 °C on the structure, strength and electrical conductivity of the material has been analysed. Using the treatment temperature 600 °C, a structure providing improved physical and mechanical properties of the material was formed. However, at the treatment temperature 800 °C, an anode structure with an array of microcracks was formed that significantly reduced the strength and electrical conductivity of the material.