I12 is the Joint Engineering, Environmental and Processing (JEEP) beamline, constructed during Phase II of the Diamond Light Source. I12 is located on a short (5 m) straight section of the Diamond storage ring and uses a 4.2 T superconducting wiggler to provide polychromatic and monochromatic X-rays in the energy range 50-150 keV. The beam energy enables good penetration through large or dense samples, combined with a large beam size (1 mrad horizontally  0.3 mrad vertically). The beam characteristics permit the study of materials and processes inside environmental chambers without unacceptable attenuation of the beam and without the need to use sample sizes which are atypically small for the process under study. X-ray techniques available to users are radiography, tomography, energy-dispersive diffraction, monochromatic and white-beam two-dimensional diffraction/scattering and small-angle X-ray scattering. Since commencing operations in November 2009, I12 has established a broad user community in materials science and processing, chemical processing, biomedical engineering, civil engineering, environmental science, palaeontology and physics.
Synchrotron X-ray microtomography has been utilized for the in-situ observation of steady state plane strain fatigue crack growth. A high resolution experimental configuration and phase contrast imaging technique have enabled the reconstruction of crack images with an isotropic voxel with a 0.7 µm edge. The details of a crack are readily observed, along with evidence of the incidence and mechanical influence of closure. After preliminary investigations of the achievable accuracy and reproducibility, a variety of measurement methods are used to quantify crack opening displacement (COD) and closure from the tomography data. Utilization of the physical displacements of microstructural features is proposed to obtain detailed COD data, and its feasibility is confirmed. Loss of fracture surface contact occurs gradually up to the maximum load. This is significantly different from tendencies reported where a single definable opening level is essentially assumed to exist. The closure behaviour is found to be attributable mainly to remarkable generation of mode III displacement which may be caused by local crack topology. Many small points of closure still remain near the crack-tip, suggesting that the near-tip contact induces crack growth resistance. The effects of overloading are also discussed.
Nanosized, carbon-coated LiFePO4 (LFP) is a promising cathode for Li-ion batteries. However, nano-particles are problematic for electrode design, optimized electrodes requiring high tap densities, good electronic wiring, and a low tortuosity for efficient Li diffusion in the electrolyte in between the solid particles, conditions that are difficult to achieve simultaneously. Using in situ energy-dispersive X-ray diffraction, we map the evolution of the inhomogeneous electrochemical reaction in LFP-electrodes. On the first cycle, the dynamics are limited by Li diffusion in the electrolyte at a cycle rate of C/7. On the second cycle, there appear to be two rate-limiting processes: Li diffusion in the electrolyte and electronic conductivity through the electrode. Three-dimensional modeling based on porous electrode theory shows that this change in dynamics can be reproduced by reducing the electronic conductivity of the composite electrode by a factor of 8 compared to the first cycle. The poorer electronic wiring could result from the expansion and contraction of the particles upon cycling and/or the formation of a solid-electrolyte interphase layer. A lag was also observed perpendicular to the direction of the current: the LFP particles at the edges of the cathode reacted preferentially to those in the middle, owing to the closer proximity to the electrolyte source. Simulations show that, at low charge rates, the reaction becomes more uniformly distributed across the electrode as the porosity or the width of the particle-size distribution is increased. However, at higher rates, the reaction becomes less uniform and independent of the particle-size distribution.
The natural initiation and growth of short cracks in Inconel ® 718 U-notch specimens has been studied at 600 o C in air. U notches were introduced through broaching, and hardness traces and optical microscopy on cross sections through the U notch broaching showed that the broaching process had introduced a deformed, work hardened layer. Fatigue tests were conducted under load control using a 1-1-1-1 trapezoidal waveform, on specimens with as-broached and polished U-notches. Multi-site crack initiation occurred in the notch root. Many of the cracks initiated at bulge-like features formed by volume expansion of oxidising (Nb,Ti)C particles. In unstressed samples, oxidation of (Nb,Ti)C particles occurred readily, producing characteristic surface eruptions. Scanning electron microscopy on metallographic sections revealed some sub-surface (Nb,Ti)C oxidation and localised matrix deformation around oxidised particles. A mechanism for crack initiation by carbide expansion during oxidation is discussed. Surface short crack growth rates in the notch root of polished specimens were measured using an acetate replica technique. Observed short crack growth rates were approximately constant across a wide range of crack lengths. However, there was a transition to rapid, accelerating crack growth once cracks reached several hundred microns in length. This rapid propagation in the latter stages of the fatigue life was assisted by crack coalescence. Polishing the U-notch to remove broaching marks resulted in a pronounced increase in fatigue life. IntroductionNickel-base superalloys like Inconel ® 718 (IN718) are used extensively for turbine discs and other components in industrial and aerospace gas turbines. Since turbine discs are safety-critical components, considerable effort is expended in determining their safe operating life. The lifing procedure adopted must enable the reliable prediction of the safe life of the disc, without being overly conservative. Once engines are in service, regular inspection of the engines and refinements of lifing models may enable life-extension programs to be considered. In the traditional predicted safe life philosophy, the life is declared based on laboratory specimen and component testing. In recent years a damage-tolerant approach to lifing has been adopted, in which it is accepted that components contain defects or inhomogeneities from which cracks can initiate. Assuming an initial flaw size c o , the fatigue life is determined as the number of cycles required to propagate the crack to some critical size c c . The initial size c o can be based on the maximum defect size present in the material, or on the minimum defect size detectable by nondestructive testing (NDT) [1]. Selection of c c is based on knowledge of the fracture toughness of the material, the limit load, the maximum allowable strain or maximum permitted compliance change for a particular component. Damage-tolerant lifing requires accurate information on fatigue crack initiation and growth rates. Fatigue lives are determi...
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