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In this paper we show how reliable measurements on porous ceramic films can be made by appropriate nanoindentation experiments and analysis. Room-temperature mechanical properties of the mixed-conducting perovskite material LSCF6428 were investigated by nanoindentation of porous bulk samples and porous films sintered at temperatures from 900-1200C. A spherical indenter was used so that the contact area was much greater than the scale of the porous microstructure. The elastic modulus of the bulk samples was found to increase from 33.8-174.3 GPa and hardness from 0.64-5.32 GPa as the porosity decreased from 45-5% after sintering at 900-1200C. Densification under the indenter was found to have little influence on the measured elastic modulus. The residual porosity in the dense sample was found to account for the discrepancy between the elastic moduli measured by indentation and by impulse excitation. Crack-free LSCF6428 films of acceptable surface roughness for indentation were also prepared by sintering at 900-1200C. Reliable measurements of the true properties of the films were obtained by data extrapolation provided that the ratio of indentation depth to film thickness was in the range 0.1 to 0.2. The elastic moduli of the films and bulk materials were approximately equal for a given porosity. The 3D microstructures of films before and after indentation were characterized using FIB-SEM tomography. Finite element modelling of the elastic deformation of the actual microstructures showed excellent agreement with the nanoindentation results., Comment: journal paper published

Sandwich specimens were prepared by firing a thin inter-layer of porous La0.6Sr0.4Co0.2Fe0.8O3-d (LSCF) to bond a thin tetragonal yttria-stabilised zirconia (YSZ) beam to a thick YSZ substrate. Fracture of the joint was evaluated by introducing a wedge between the two YSZ adherands so that the stored energy in the thin YSZ cantilever beam drives a stable crack in the adhesive bond and allows the critical energy release rate for crack extension (fracture toughness) to be measured. The crack path in most specimens showed a mixture of adhesive failure (at the YSZ-LSCF interface) and cohesive failure (within the LSCF). It was found that the extent of adhesive fracture increased with firing temperature and decreased with LSCF layer thickness. The adhesive failures were mainly at the interface between the LSCF and the thin YSZ beam and FEM modelling revealed that this is due to asymmetric stresses in the LSCF. Within the firing temperature range of 1000-1150C, the bonding fracture toughness appears to have a strong dependence on firing temperature. However, the intrinsic adhesive fracture toughness of the LSCF/YSZ interface was estimated to be 11 Jm2 and was not firing temperature dependent within the temperature range investigated., Comment: 13 figures, 1 table, journal paper published

The reliability of perovskite material LSCF to be used as cathode parts in solid oxide fuel cells also relies on its mechanical properties. Adequate surface conditions are desired when the as-sintered porous thin films are subjected to nanoindentation for mechanical property determination. In this study, extensive cracks and considerable surface roughness were found in the LSCF films after sintering at high temperatures. This would significantly scatter the nanoindentation data and result in unreliable measurements. Various attempts including the comparison of film deposition methods, drying and sintering processes, and reformulating the ink were made to improve the surface quality. Results revealed little dependence of cracking and surface roughness on deposition methods, drying or sintering processes. It was found that the critical factor for obtaining crack-free and smooth LSCF films was the ability of the ink to be self-levelling in the earlier wet state. Reproducible nanoindentation measurements were obtained for the films with improved surface quality., Comment: 16 figures, 2 tables, journal paper published

The manufacture of solid oxide fuel cells (SOFCs) involves fabrication of a multilayer ceramic structure, for which constrained sintering is a key processing step in many cases. Defects are often observed in the sintered structure, but their formation during sintering is not well understood. In this work, various ceramic films were fabricated by screen printing and a variety of defects observed. Some films showed mud-cracking defects, whereas others presented distributed large pores. Mud cracking defects were found to originate from a network of fine cracks present in the green film and formed during drying and binder burn-out. Control of these early stages is essential for producing crack-free films. In order to investigate how defects evolve during sintering, artificial cracks were introduced in the green films using indentation. It was observed that crack opening always increased during constrained sintering. In contrast, similar initial cracks could be closed and healed during co-sintering., Comment: 12 figures, 1 table

Mechanical properties of porous SOFC electrodes are largely determined by their microstructures. Measurements of the elastic properties and microstructural parameters can be achieved by modelling of the digitally reconstructed 3D volumes based on the real electrode microstructures. However, the reliability of such measurements is greatly dependent on the processing of raw images acquired for reconstruction. In this work, the actual microstructures of La0.6Sr0.4Co0.2Fe0.8O3-d (LSCF) cathodes sintered at an elevated temperature were reconstructed based on dual-beam FIB/SEM tomography. Key microstructural and elastic parameters were estimated and correlated. Analyses of their sensitivity to the grayscale threshold value applied in the image segmentation were performed. The important microstructural parameters included porosity, tortuosity, specific surface area, particle and pore size distributions, and inter-particle neck size distribution, which may have varying extent of effect on the elastic properties simulated from the microstructures using FEM. Results showed that different threshold value range would result in different degree of sensitivity for a specific parameter. The estimated porosity and tortuosity were more sensitive than surface area to volume ratio. Pore and neck size were found to be less sensitive than particle size. Results also showed that the modulus was essentially sensitive to the porosity which was largely controlled by the threshold value., Comment: 21 pages, 14 figures, 2 tables, journal paper published in Journal of Power Sources