Boundary selectivity of crack paths in corrosion fatigue of stainless steel

Stress corrosion and corrosion fatigue cracks are frequently very branched and there have been extensive attempts to define the characteristics of crack-stopping features. EBSD has been used to examine the full length (~8mm) of a corrosion fatigue crack in stainless steel. The grain boundary character distribution of the cracked boundaries is compared to that of the rest of the material and observations presented on the effect of grain boundary character on the choice of crack path at grain boundary junctions of different configurations and orientations with restect to the principle stres

High resolution characterisation of microstructural evolution in Rbx_{x}Fe2−y_{2-y}Se2_{2} crystals on annealing

The superconducting and magnetic properties of phase-separated A$_x$Fe$_{2-y}$Se$_2$ compounds are known to depend on post-growth heat treatments and cooling profiles. This paper focusses on the evolution of microstructure on annealing, and how this influences the superconducting properties of Rb$_x$Fe$_2-y$Se$_2$ crystals. We find that the minority phase in the as-grown crystal has increased unit cell anisotropy (c/a ratio), reduced Rb content and increased Fe content compared to the matrix. The microstructure is rather complex, with two-phase mesoscopic plate-shaped features aligned along {113} habit planes. The minority phase are strongly facetted on the {113} planes, which we have shown to be driven by minimising the volume strain energy introduced as a result of the phase transformation. Annealing at 488K results in coarsening of the mesoscopic plate-shaped features and the formation of a third distinct phase. The subtle differences in structure and chemistry of the minority phase(s) in the crystals are thought to be responsible for changes in the superconducting transition temperature. In addition, scanning photoemission microscopy has clearly shown that the electronic structure of the minority phase has a higher occupied density of states of the low binding energy Fe3d orbitals, characteristic of crystals that exhibit superconductivity. This demonstrates a clear correlation between the Fe-vacancy-free phase with high c/a ratio and the electronic structure characteristics of the superconducting phase.Comment: 6 figures v2 is exactly the same as v1. The typesetting errors in the abstract have been correcte

Individual grain boundary properties and overall performance of metal-organic deposition coated conductors

have investigated single grain boundaries (GBs) isolated in coated conductors produced by metal-organic deposition. When a magnetic field is swept in the film plane, an angle-dependent crossover from boundary to grain limited critical current density J(c) is found. In the force-free orientation, even at fields as high as 8 T, the GBs still limit Jc. We deduce that this effect is a direct consequence of GB meandering. We have employed these single GB results to explain the dependence of Jc of polycrystalline tracks on their width: in-plane measurements become flatter as the tracks are narrowed down. This result is consistent with the stronger GB limitation at field configurations close to force-free found from the isolated boundaries. Our study shows that for certain geometries even at high fields the effect of GBs cannot be neglected.This work was supported by the Engineering and Physical Sciences Research Council [grant numbers EP/C011546/1 and EP/C011554/1

Microstructural analysis of phase separation in iron chalcogenide superconductors

The interplay between superconductivity, magnetism and crystal structure in iron-based superconductors is a topic of great interest amongst the condensed matter physics community as it is thought to be the key to understanding the mechanisms responsible for high temperature superconductivity. Alkali metal doped iron chalcogenide superconductors exhibit several unique characteristics which are not found in other iron-based superconducting materials such as antiferromagnetic ordering at room temperature, the presence of ordered iron vacancies and high resistivity normal state properties. Detailed microstructural analysis is essential in order to understand the origin of these unusual properties. Here we have used a range of complementary scanning electron microscope based techniques, including high-resolution electron backscatter di raction mapping, to assess local variations in composition and lattice parameter with high precision and sub-micron spatial resolution. Phase separation is observed in the Csx Fe2-ySe2 crystals, with the minor phase distributed in a plate-like morphology throughout the crystal. Our results are consistent with superconductivity occurring only in the minority phase.Comment: Accepted for publication in a special edition of Supercond. Sci. Techno

A Trapped Field of >3T in Bulk MgB2 Fabricated by Uniaxial Hot Pressing

A trapped field of over 3 T has been measured at 17.5 K in a magnetised stack of two disc-shaped bulk MgB2 superconductors of diameter 25 mm and thickness 5.4 mm. The bulk MgB2 samples were fabricated by uniaxial hot pressing, which is a readily scalable, industrial technique, to 91% of their maximum theoretical density. The macroscopic critical current density derived from the trapped field data using the Biot-Savart law is consistent with the measured local critical current density. From this we conclude that critical current density, and therefore trapped field performance, is limited by the flux pinning available in MgB2, rather than by lack of connectivity. This suggests strongly that both increasing sample size and enhancing pinning through doping will allow further increases in trapped field performance of bulk MgB2.Comment: 10 pages, 4 figures. Accepted as a Rapid Publication in Superconductor Science and Technology (Final version after peer review

Specimen preparation methods for elemental characterisation of grain boundaries and isolated dislocations in multicrystalline silicon using atom probe tomography

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

Removal and Reoccurrence of LLZTO Surface Contaminants under Glovebox Conditions

The reactivity of Li6.4La3Zr1.4Ta0.6O12 (LLZTO) solid electrolytes to form lithio-phobic species such as Li2CO3 on their surface when exposed to trace amounts of H2O and CO2 limits the progress of LLZTO-based solid-state batteries. Various treatments, such as annealing LLZTO within a glovebox or acid etching, aim at removing the surface contaminants, but a comprehensive understanding of the evolving LLZTO surface chemistry during and after these treatments is lacking. Here, glovebox-like H2O and CO2 conditions were recreated in a near ambient pressure X-ray photoelectron spectroscopy chamber to analyze the LLZTO surface under realistic conditions. We find that annealing LLZTO at 600 °C in this atmosphere effectively removes the surface contaminants, but a significant level of contamination reappears upon cooling down. In contrast, HCl(aq) acid etching demonstrates superior Li2CO3 removal and stable surface chemistry post treatment. To avoid air exposure during the acid treatment, an anhydrous HCl solution in diethyl ether was used directly within the glovebox. This novel acid etching strategy delivers the lowest lithium/LLZTO interfacial resistance and the highest critical current density

Initiation of dendritic failure of LLZTO via sub-surface lithium deposition

The occurrence of lithium deposition in occluded spaces within ceramic electrolytes due to electronic leakage currents can jeopardise the commercialization of power-dense solid-state batteries. Here, we utilize plasma-FIB serial sectioning to visualize the surface and sub-surface of a garnet solid electrolyte (LLZTO) after lithium plating. We study the morphology of surface spallation cracks, which represent the initial stage of dendrite formation. Employing a LiMg anode, we track the magnesium diffusion around these surface cracks with EDS. The absence of magnesium in early-stage cracks suggests they form due to the pressure build-up from the deposition of pure lithium in occluded pores near the electrolyte surface. These spallation cracks act as current focusing and stress concentration hot spots. Electron beam induced current imaging demonstrates that short-circuiting lithium dendrites grow from the spallations during plating. Thus, the sub-surface deposition of lithium is a possible explanation for the initiation of lithium dendrites in LLZTO

Lateral electrical transport, optical properties and photocurrent measurements in two-dimensional arrays of silicon nanocrystals embedded in SiO2

In this study we investigate the electronic transport, the optical properties, and photocurrent in two-dimensional arrays of silicon nanocrystals (Si NCs) embedded in silicon dioxide, grown on quartz and having sizes in the range between less than 2 and 20 nm. Electronic transport is determined by the collective effect of Coulomb blockade gaps in the Si NCs. Absorption spectra show the well-known upshift of the energy bandgap with decreasing NC size. Photocurrent follows the absorption spectra confirming that it is composed of photo-generated carriers within the Si NCs. In films containing Si NCs with sizes less than 2 nm, strong quantum confinement and exciton localization are observed, resulting in light emission and absence of photocurrent. Our results show that Si NCs are useful building blocks of photovoltaic devices for use as better absorbers than bulk Si in the visible and ultraviolet spectral range. However, when strong quantum confinement effects come into play, carrier transport is significantly reduced due to strong exciton localization and Coulomb blockade effects, thus leading to limited photocurrent

The Postpartum Specific Anxiety Scale: development and preliminary validation

Perinatal symptoms of anxiety are increasingly recognised due to their high prevalence and impact. Studies using pregnancy-specific anxiety measures have found that they may predict perinatal outcomes more effectively than general measures. However, no such measure exists to assess anxieties specific to the postpartum. This study aimed to develop and validate a measure (Postpartum Specific Anxiety Scale; PSAS) that accurately represents the specific anxieties faced by postpartum women, using a four-stage methodology: (1) 51 items were generated from interviews conducted with a group of 19 postpartum women at two time points, (2) the scale was reviewed and refined by a diverse expert panel, (3) an online pilot study (n = 146) was conducted to assess comprehensibility and acceptability and (4) an online sample of 1282 mothers of infants up to 6 months old completed the PSAS against a battery of convergent measures. A subsample (n = 262) repeated the PSAS 2 weeks later. The PSAS possessed good face and content validity and was comprehensible and acceptable to postpartum women. PSAS scores were significantly correlated with other measures indicating good convergent validity. Principal component analyses (PCA) revealed a simple four-factor structure. Reliability of the overall scale and individual PSAS factors proved to be good to excellent. A preliminary receiver operating characteristic (ROC) analysis also suggested that the PSAS may be a useful screening tool. The psychometric evidence suggests that the PSAS is an acceptable, valid, and reliable research tool to assess anxieties, which are specific to the postpartum period. Next steps in the iterative validation process are considered for both research and screening purposes