It is well-known that steels always oxidize faster in the environments containing water vapour than in dry oxygen. Due to the difficulties in obtaining necessary experimental scale of observations, the mechanisms responsible for the steam-accelerated oxidation are still unclear. Through a combination of multiscale characterization techniques, the surface oxide film formed on an Fe-17Cr-9Ni stainless steel after exposure to high-temperature steam has been studied in detail. The characterization results obtained in this study reveal that the formation of the inner oxide layer, which is critical in protecting the base metal, is due to internal oxidation instead of external oxidation. The classic internal oxidation model underestimates the thickness of the inner oxide layer by one order of magnitude. This difference can be explained by the existence of fast diffusion channels in the inner oxide layer. This study provides direct evidence of a high density of nanopores in the oxide phase of the internal oxide layer, which can act as fast-diffusion channels if interconnected, and proposes their mechanisms of formation, a consequence of water dissociation-induced protons promoting the formation, migration, and clustering of both cation and anion vacancies.
Multicrystalline silicon (mc-Si) is a cost effective feedstock for solar photovoltaic devices but is limited by the presence of defects and impurities. Imaging impurities segregated to nanometre-scale dislocations and grain boundaries is a challenge that few materials characterisation techniques can achieve. Atom Probe Tomography (APT) is a 3-dimensional time-of-flight microscopy technique that can image the distribution of elements at the atomic scale, however one of the most challenging factors when using APT is the complexity of specimen preparation for specific regions of interest. Atom probe specimen preparation methods have been developed in a dual FIB/SEM system that enable a specific extended defect such as an isolated dislocation or a section of a grain boundary to be selected for APT analysis. The methods were used to fabricate APT specimens from an isolated dislocation and a grain boundary in mc-Si samples. Complementary TEM images confirm the presence of the defects in both specimens, whilst APT analyses also reveal segregation of impurities to the defects.
The crack initiation on a cold-worked surface of Alloy 600, exposed to simulated pressurized water reactor primary water, was mechanistically studied through high-resolution characterization. Mechanical polishing introduced a thin recrystallization layer on the specimen surface, which lead to the crack initiation along highlydeformed recrystallization grain boundaries after preferential oxidation. Intergranular crack propagation occurred once the initiation cracks met the matrix grain boundaries under the external loading and the residual stress introduced by the prior 20% cold working. The controlling mechanism of SCC crack propagation was believed to be an intergranular selective oxidation mechanism.
In this paper, the physical mechanisms involved in electron-beam-induced current (EBIC) imaging of semiconductor pn-junctions are reviewed to propose a model and optimize the acquisition of experimental data. Insights are drawn on the dependence of the EBIC signal with electron accelerating voltage and surface conditions. It is concluded that improvements in the resolution of EBIC are possible when the surface conditions of the specimens are carefully considered and optimized. A lower accelerating voltage and an increase of the surface recombination velocities are quantitatively shown to maximize the EBIC lateral resolution in locating the pn-junction. The effect of surface band bending is included in the model, and it is seen to primarily affect the surface recombination. Introducing controlled surface damage is shown as a potential method for resolution enhancement via focused ion beam milling with Ga+ ions. These findings contribute to the understanding of this technique and can produce further improvements to its application in semiconductor device technology.
It is often assumed that internal oxidation cannot occur at temperatures below 400ºC. However, in the present work, internal oxidation was observed in a 20% cold-worked Fe-17Cr-12Ni stainless steel (SS) after exposure to simulated primary water of a pressurized water reactor at 340ºC and not in a similarly tested sample without prior cold-work. The formation of discrete Cr-oxide precipitates and the role of cold-work are discussed. The internal oxidation model is also proposed as a plausible stress corrosion cracking mechanism of Fe-17Cr-12Ni SS at that temperature.
Hydrogen passivation is a key industrial technique used to reduce the recombination activity of defects in multicrystalline silicon (mc-Si). However, not all dislocations and grain boundaries respond well to traditional hydrogen passivation techniques. In order to understand the reasons for these different behaviours, and how superior passivation might be achieved, a method is required for the direct observation of hydrogen at these defects. Here, we present a novel characterisation technique based on a combination of transmission Kikuchi diffraction (TKD), atom probe tomography (APT), and isotopic substitution that enables unambiguous detection and quantification of hydrogen atoms present at crystallographic defects in mc-Si.
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