Volume 51, Issue 9

Microstructural characterization by combined EBSD and X-ray diffraction analysis is shown for an FCC material deformed by rolling and further heat treatment on air. The wide variety of x-rays sources combined with EBSD allows some correlations between microstructural parameters to be withdrawn by carefully analyzing x-ray peak broadening. The combination of both techniques provides a deeper understanding of anisotropic accumulation of dislocation arrays on a deformed F 138 stainless steel. The anisotropy results in a smaller peak breadth for crystal orientations with [110] planes contained on the rolling plane, further explained as resulting from a lower storage of dislocations. After heat treatment the effect is reverted and the formerly less misoriented orientations become more uniformly oriented revealing a faster dislocation migration and annihilation and/or trapping.

The different microstructures typically found in nuclear components made of zirconium alloys are discussed in this paper. These include material in a variety of thermo-mechanical conditions, e. g., cold rolled, stress relieved, recrystallized, welded, biphasic, together with minority second phases belonging to the original material or incorporated due to in-service conditions. The anisotropic crystalline structure of zirconium is exploited in microscopical observations by means of polarizer filters that enhance the contrast between different grains, and greatly aid the identification in most microstructures. Most microstructural variations across a wide range of length-scales, such as those produced by welding processes, can be effectively resolved by traditional optical microscopy (OM). However, some finer microstructures like those found in CANDU 1 (CANada Deuterium Uranium) reactor pressure tube material, or some minority second phase particles like the Zr(Fe, Cr) 2 precipitates in Zircaloy-4 cannot be completely resolved by this technique. Thus, scanning electron microscopy (SEM), and transmission electron microscopy (TEM) are required in such cases. For SEM observations we show the valuable issue of the scale in specific microstructural studies, which allows quantifying microstructural parameters using image analysis. For TEM observations, we have greatly benefited from the electron diffraction diagrams, which have allowed us to investigate the crystalline structure of irradiated second phase particles, which would remain unnoticed to both, OM or SEM observations.

The Focused Ion Beam (FIB) technique was used to prepare site-specific samples from interfacial regions of different solid oxide fuel cells assemblies. Transmission and Scanning Electron Microscopy on the FIB foils combined with Electrochemical Impedance Spectroscopy (EIS) allowed the characterization of the electrode/electrolyte interphases and the determination of its influence on the cell performance after long-term operation conditions. This work reviews two cases: on one hand, Ln 2 NiO 4+d (Ln= La, Nd) cathodes deposited on both Y 0.08 Zr 0.92 O 1.96 and Ce 0.9 Gd 0.1 O 1.95 electrolytes, that react at 900 °C during the adhesion treatment and at temperatures higher than 650 °C during the EIS measurements. These samples present a reaction layer of 10 nm thickness, which contains elements of both phases and was found responsible of the cell performance degradation. On the other hand, La 0.4 Sr 0.6 Co 0.8 Fe 0.2 O 3-δ cathodes showed excelent performance on Ceria electrolytes, even after 1 000 h at operation conditions. In that case, the microscopic analyses of FIB foils showed a semi-coherent interphase growth.

UNS 31603 austenitic stainless steel was nitrided using different techniques, and pitting corrosion resistance was analysed in a chloride solution. All nitriding techniques, LEII, PI· and convectional DC nitriding produced a nitrided layer called S phase which is corrosion resistant. Pits morphology and layer structure was investigated using optical and electronic microscopy, SEM-FIB, EDS, and a 3D reconstruction of a pit was assessed using FIB tomography. It was concluded that pits are initiated in MnS inclusions and a channel was generated passing through the nitrided layer, connecting the steel with the electrolyte. Base alloy dissolution was observed beneath the nitrided layer.