T. Connolley

Assessment of the fatigue crack closure phenomenon in damage-tolerant aluminium alloy by in-situ high-resolution synchrotron X-ray microtomography

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, together 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 pronounced 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.

I12: the Joint Engineering, Environment and Processing (JEEP) beamline at Diamond Light Source

JEEP is a high-energy (50–150 keV) multi-purpose beamline offering polychromatic and monochromatic modes. It can accommodate large samples and experimental rigs, enabling in situ studies using radiography, tomography, energy-dispersive diffraction, monochromatic and white-beam two-dimensional diffraction/scattering and small-angle X-ray scattering.

Short crack initiation and growth at 600 °C in notched specimens of Inconel718

The natural initiation and growth of short cracks in Inconel®718 U-notch specimens has been studied at 600 °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 micrometers 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.

Revealing the micromechanisms behind semi-solid metal deformation with time-resolved X-ray tomography

The behaviour of granular solid–liquid mixtures is key when deforming a wide range of materials from cornstarch slurries to soils, rock and magma flows. Here we demonstrate that treating semi-solid alloys as a granular fluid is critical to understanding flow behaviour and defect formation during casting. Using synchrotron X-ray tomography, we directly measure the discrete grain response during uniaxial compression. We show that the stress–strain response at 64–93% solid is due to the shear-induced dilation of discrete rearranging grains. This leads to the counter-intuitive result that, in unfed samples, compression can open internal pores and draw the free surface into the liquid, resulting in cracking. A soil mechanics approach shows that, irrespective of initial solid fraction, the solid packing density moves towards a constant value during deformation, consistent with the existence of a critical state in mushy alloys analogous to soils.

Region-of-interest tomography using filtered backprojection: assessing the practical limits

There are many cases where it is desirable to reconstruct at high resolution a small volume from a larger sample. Here we describe the outcomes of a reconstruction trial based on real samples aimed at delineating the practical limits to which a small region of interest can be viewed from a large sample. Our approach has been to artificially truncate the sinograms of whole sample scans to simulate region of interest tomography. A simple filtered back projection algorithm has been applied, with the sinograms extended laterally in a simple manner to make up for the truncated portions. The impact of the degree of truncation (from 0% down to 99%), the number of projections used, as well as the position of the region of interest, on the faithfulness of the reconstruction is evaluated for a range of sample types. We have assessed the nature of, and extent to which, artefacts are introduced and the degree to which simple strategies can minimize them to an acceptable level without the need for complex reconstruction algorithms, projection stitching strategies or very large detectors. It is found that for a wide range of objects the effect of truncation on feature detection is negligible and that excellent images can be reconstructed if the number of projections is calculated not on the basis of the number of pixels on the camera, but on the number of pixels that would be required to scan the whole sample at the chosen pixel resolution. This paper demonstrates that in many cases more sophisticated reconstruction strategies are not necessary.

Transgranular liquation cracking of grains in the semi-solid state

Grain refinement via semi-solid deformation is desired to obtain superior mechanical properties of cast components. Using quantitative in situ synchrotron X-ray tomographic microscopy, we show an additional mechanism for the reduction of grain size, via liquation assisted transgranular cracking of semi-solid globular microstructures. Here we perform localized indentation of Al-15wt.%Cu globular microstructures, with an average grain size of ∼480 μm, at 555 °C (74% solid fraction). Although transgranular fracture has been observed in brittle materials, our results show transgranular fracture can also occur in metallic alloys in semi-solid state. This transgranular liquation cracking (TLC) occurs at very low contact stresses (between 1.1 and 38 MPa). With increasing strain, TLC continues to refine the size of the microstructure until the grain distribution reaches log-normal packing. The results demonstrate that this refinement, previously attributed to fragmentation of secondary arms by melt-shearing, is also controlled by an additional TLC mechanism.

Finite element comparison of performance related characteristics of balloon expandable stents

Cardiovascular stents are commonly made from 316L stainless steel and are deployed within stenosed arterial lesions using balloon expansion. Deployment involves inflating the balloon and plastically deforming the stent until the required diameter is obtained. This plastic deformation induces static stresses in the stent, which will remain for the lifetime of the device. In order to determine these stresses, finite element models of the unit cells of geometrically different, commercially available balloon expandable stents have been created, and deployment and elastic recoil have been simulated. In this work the residual stresses associated with deployment and recoil are compared for the various stent geometries, with a view to establishing appropriate initial stress states for fatigue loading for the stents. The maximum, minimum, and mean stresses induced in the stent due to systolic/diastolic pressure are evaluated, as are performance measures such as radial and longitudinal recoil.

Complete elliptical ring geometry provides energy and instrument calibration for synchrotron-based two-dimensional X-ray diffraction

A complete method for calibrating a two-dimensional flat-panel detector for use in X-ray diffraction is described. The method provides both the beam energy and the sample-to-detector distance. The geometry for the intersection of a cone’s axis and its elliptical conic section is also presented.

Understanding the deformation mechanism of individual phases of a ZrTi-based bulk metallic glass matrix composite using in situ diffraction and imaging methods

The plasticity of a ZrTi-based bulk metallic glass composite consisting of glassy matrix and crystalline dendritic phase was studied in-situ under identical tensile loading conditions using scanning electron microscopy and synchrotron X-ray diffraction. A generic procedure was developed to separate the diffraction information of the crystalline phases away from that of the matrix and to precisely calculate the microscopic strains of the two phases at different macroscopic load steps. In this way, the time-evolved quantitative links between shear bands nucleation/propagation and the corresponding microscopic stress fields around them are established, providing more quantitative understanding on (1) how the shear bands are driven by the local stress field, and (2) the critical stresses required for the shear bands to nucleate in the crystalline phase, propagate through the crystalline/matrix interface, and finally into the matrix.

Visualization of membrane protein crystals in lipid cubic phase using X-ray imaging.

A comparison of X-ray diffraction and radiographic techniques for the location and characterization of protein crystals is demonstrated on membrane protein crystals mounted within lipid cubic phase material.