Microstructural characterization of Ni/YSZ based SOFC anodes after cyclic reduction and oxidation using electron microscopy

The effect of redox cycling on the microstructure, of an SOFC anode, was studied using two approaches. Bulk samples were redox cycled and then examined in the SEM. In addition, electron transparent samples were prepared, redox cycled, and then examined in the TEM. Significant microstructural changes were observed. The anode in the as received condition consists of NiO particles several microns in size, YSZ grains about one micron in size and intergranular porosity. After the first reduction, the overall Ni grain size remains the same as the consumed NiO and epitaxial growth of Ni crystals on NiO grains is observed. The amount of intergranular porosity increases and very fine (50 nm) intragranular pores are formed throughout the Ni grains. This increase in the amount of porosity is expected due to the large volume change that occurs upon reduction. When samples are reoxidized the NiO particles in the SEM images appear spongy with much smaller pores than the as received, oxidized samples. The reoxidized anode consists of fine (<100 nm), randomly oriented grains of NiO. The grain refinement that occurs upon reoxidation is likely due to the large number of intragranular pores that occur upon reduction, which serve as nucleation sites. Rereduced samples were also very fine grained (<200 nm) and contained significant amounts of small intergranular porosity. The YSZ grains were unaffected by the redox cycles. (author)