Open Access

Show Abstract ▼

Abstract: The distinct molecular architecture and thermomechanical properties of polyurethane block copolymers make them suitable for applications ranging from textile fibers to temperature sensors. In the present study, differential scanning calorimetry (DSC) analysis and macroscopic stress relaxation measurements are used to identify the key internal processes occurring in the temperature ranges between −10 °C and 0 °C and between 60 °C and 70 °C. The underlying physical phenomena are elucidated by the small-angle X-ray scattering (SAXS) and wide-angle X-ray scattering (WAXS) study of synchrotron beams, allowing the exploration of the structure-property relationships as a function of temperature. In situ multiscale deformation analysis under uniaxial cyclic thermomechanical loading reveals a significant anomaly in the strain evolution at the nanoscale (assessed via SAXS) in the range between −10 °C and 0 °C owing to the ‘melting’ of the soft matrix. Furthermore, WAXS measurement of crystal strain within the hard regions reveals significant compressive residual strains arising from unloading at ∼60 °C, which are associated with the dynamic shape memory effect in polyurethane at these temperatures.

Show Abstract ▼

Abstract: Residual stresses in thin films and multi-layered coatings fabricated by physical vapour deposition largely affect their mechanical and thermal reliability during operation in numerous fields of applications. By changing the argon working pressure in between each multilayer planar DC magnetron sputter deposition step, it is possible to control the residual stress distribution within coatings. A combination of FIB-DIC ring-core strain analysis, synchrotron XRD analysis based on the sin2(Ψ) method and micro-cantilever deflection analysis is used to reconstruct the in-plane stress state of multilayer coatings at different deposition pressures, with a residual stress depth profile resolution of 50 nm. A clear transition from compressive to tensile residual stresses is observed with an increase of working pressure, with pronounced stress peaks near the substrate-coating interface. These peak stresses resolved by FIB-DIC ring-core analysis exceed the average XRD stress measurements significantly, thus providing a reasonable explanation for multilayer failure. Experimental results are presented and comprehensively discussed in the context of deposition conditions for different thin film applications.

Show Abstract ▼

Abstract: Fundamental understanding of the generation and multiplication of basal plane dislocations (BPDs) in PVT-grown 4H-SiC crystals is critical for design of growth strategies to control their densities during PVT growth of 4H-SiC crystals. Direct observation of thermal gradient induced motion of basal plane dislocations by in-situ synchrotron X-ray topography imaging of PVT-grown 4H-SiC wafers subject to high temperature treatment has provided an opportunity to analyze the movement of dislocations. Dislocations with Burgers vector along the off-cut [11-20] direction were found to be the only dislocations involved in deformation during heat treatment and the segments of dislocations used for velocity measurements were found to be either pure screw comprised of both Si- and C- core partials or 60° dislocations comprised of purely Si cores. Using the kink-diffusion model, the activation energies for dislocation motion have been estimated from the velocity data for each of these dislocation types and found to be 2.21 eV for 60° and 3.28 eV for pure screw segments, respectively. These values are in good agreement with the macroscopic studies of yielding of semiconductor crystals during high temperature compression and indentation experiments. Quantitative expression of the temperature dependent critical resolved shear stress required for dislocation motion has been derived from this analysis.

Show Abstract ▼

Abstract: Objectives: Yttria Partially Stabilised Zirconia (YPSZ) is a high strength ceramic which has become widely used in porcelain veneered dental copings due to its exceptional toughness. Within these components the residual stress and crystallographic phase of YPSZ close to the interface are highly influential in the primary failure mode; near interface porcelain chipping. In order to improve present understanding of this behaviour, characterisation of these parameters is needed at an improved spatial resolution. Methods: In this study transmission micro-focus X-ray Diffraction, Raman spectroscopy, and focused ion beam milling residual stress analysis techniques have, for the first time, been used to quantify and cross-validate the microscale spatial variation of phase and residual stress of YPSZ in a prosthesis cross-section. Results: The results of all techniques were found to be comparable and complementary. Monoclinic YPSZ was observed within the first 10 μm of the YPSZ-porcelain interface with a maximum volume fraction of 60%. Tensile stresses were observed within the first 150μm of the interface with a maximum value of ≈300MPa at 50μm from the interface. The remainder of the coping was in mild compression at ≈ − 30 MPa, with shear stresses of a similar magnitude also being induced by the YPSZ phase transformation. Significance: The analysis indicates that the interaction between phase transformation, residual stress and porcelain creep at YPSZ-porcelain interface results in a localised porcelain fracture toughness reduction. This explains the increased propensity of failure at this location, and can be used as a basis for improving prosthesis design.

Open Access

Show Abstract ▼

Abstract: Diffraction data were collected using synchrotron X-ray scattering (sXRD) and electron back-scattered diffraction (EBSD) during in situ tensile-compressive deformation of Mg alloy AZ31B dogbone samples. The onset and evolution of twinning and detwinning were monitored based on intensity changes in sXRD 2D scattering patterns (which also provided average elastic strain values through the calculation of orientation-specific lattice spacing changes), and EBSD, that revealed the micro-scale grain morphology changes. The observations were interpreted and analysed with the help of crystal plasticity finite element modelling (CP-FEM), as reported in the published article (https://doi.org/10.1016/j.ijplas.2019.02.018).