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An understanding of the mechanical response of modern engineering alloys to complex loading conditions is essential for the design of load-bearing components in high-performance safety-critical aerospace applications. A detailed knowledge of how material behaviour is modified by fatigue and the ability to predict failure reliably are vital for enhanced component performance. Unlike macroscopic bulk properties ( e.g. stiffness, yield stress, etc.) that depend on the average behaviour of many grains, material failure is governed by `weakest link'-type mechanisms. It is strongly dependent on the anisotropic single-crystal elastic-plastic behaviour, local morphology and microstructure, and grain-to-grain interactions. For the development and validation of models that capture these complex phenomena, the ability to probe deformation behaviour at the micro-scale is key. The diffraction of highly penetrating synchrotron X-rays is well suited to this purpose and micro-beam Laue diffraction is a particularly powerful tool that has emerged in recent years. Typically it uses photon energies of 5-25 keV, limiting penetration into the material, so that only thin samples or near-surface regions can be studied. In this paper the development of high-energy transmission Laue (HETL) micro-beam X-ray diffraction is described, extending the micro-beam Laue technique to significantly higher photon energies (50-150 keV). It allows the probing of thicker sample sections, with the potential for grain-level characterization of real engineering components. The new HETL technique is used to study the deformation behaviour of individual grains in a large-grained polycrystalline nickel sample during in situ tensile loading. Refinement of the Laue diffraction patterns yields lattice orientations and qualitative information about elastic strains. After deformation, bands of high lattice misorientation can be identified in the sample. Orientation spread within individual scattering volumes is studied using a pattern-matching approach. The results highlight the inability of a simple Schmid-factor model to capture the behaviour of individual grains and illustrate the need for complementary mechanical modelling. [ABSTRACT FROM AUTHOR]

When subjected to plastic deformation, grains within ductile face-centred cubic polycrystals fragment into “soft”, low dislocation density cells separated by “hard”, dislocation-rich walls. Using a narrow-bandwidth, sub-micrometre X-ray beam, we have mapped the deformation structure inside a single grain within a deformed Ni polycrystal. Dislocation multiplication and entanglement was found to vary depending on the physical dimensions of the grain. The method we use overcomes current limitations in classical X-ray topography allowing topographic images to be formed from small, highly deformed grains. [ABSTRACT FROM AUTHOR]

Laue diffraction, energy scanning and reciprocal space mapping are three micro-beam synchrotron X-ray diffraction techniques allowing the investigation of local misorientation induced by the dislocation substructure. In this paper a comparison between the three methods is presented, based on the mapping of a single 311 reflection from a grain within a Ni polycrystal specimen deformed to a tensile plastic strain of ~9%. Qualitatively it is observed that the maps obtained by different techniques all share the same features, although some deviations exist due to experimental limitations associated with each of the measurement techniques. [ABSTRACT FROM AUTHOR]

Elemental, chemical, and structural analysis of polycrystalline materials at the micron scale is frequently carried out using microfocused synchrotron X-ray beams, sometimes on multiple instruments. The Maia pixelated energy-dispersive X-ray area detector enables the simultaneous collection of X-ray fluorescence (XRF) and diffraction because of the relatively large solid angle and number of pixels when compared with other systems. The large solid angle also permits extraction of surface topography because of changes in self-absorption. This work demonstrates the capability of the Maia detector for simultaneous measurement of XRF and diffraction for mapping the short- and long-range order across the grain structure in a Ni polycrystalline foil. [ABSTRACT FROM AUTHOR]

Abstract: Monotonic and cyclic loading of polycrystals causes a complex evolution of the dislocation structure and internal stresses. These phenomena were studied in sheet samples of commercially pure (CP) Ni in heat-treated (large-grained) states. Various microscopy tools were used, namely, scanning electron microscopy (SEM) with electron back-scattered diffraction (EBSD) to image the surface grain structure; Focused Ion Beam (FIB) with channelling contrast to visualise the through-thickness grain arrangement; and synchrotron scanning transmission X-ray microscopy (STXM) to obtain absorption-contrast images. In order to investigate the internal defects and lattice distortion caused by them, synchrotron X-ray diffraction was used in a variety of modes. Reciprocal space mapping (RSM) was used to quantify the amount of lattice re-orientation (rotation) due to plastic deformation. Micro-beam Laue diffraction was used to obtain 2D images containing multiple reflections that undergo “streaking” due to plastic deformation. The combination of reciprocal space mapping and Laue micro-diffraction provided improved insight into the deformation processes within individual grains during plastic deformation. The results are interpreted and discussed in conjunction with dislocation dynamics and finite element modelling of plastic deformation by crystal slip. [Copyright &y& Elsevier]

Abstract: Non-destructive, quantitative and precise determination of internal strain distributions within structural materials and components can be accomplished by only a few experimental techniques, amongst which diffraction of penetrating radiation (X-ray and neutron beams) plays a central role. However, due to the various limitations of these methods, the 2-D and 3-D mapping of internal strains within bulk cross-sections at a spatial resolution of 0.1mm or better has long remained a challenge. The principle of “strain tomography” proposed by the present authors (an instance of broader “rich” tomography methodology) makes use of the reconstruction tomography technique widely employed in imaging applications. In the present paper we report successful practical implementation of this principle to the study of bending strains in sintered polycrystalline zirconia used in the fabrication of multi-unit fixed prosthetic dentures. The results demonstrate the power of the technique, and pave the way to wider application of this approach to cross-sectional strain mapping in complex-shaped components under various loading conditions. [Copyright &y& Elsevier]

Abstract: Better understanding of the distribution of elastic and plastic strains in deformed polycrystalline, multiphase materials is important for structural engineering. The deformation response depends upon the interaction of grains of different orientations, and the anisotropy associated with each phase. Strain partitioning and tensile-compressive hardening asymmetry arises due to mismatches in modulus and ductility between grains and phases in alloys such as Ti–6Al–4V that displays both strong anisotropy within one phase and significant differences of properties between phases. Simple four-point bent beam samples were studied using the newly available energy-dispersive X-ray diffraction setup at the high energy white-beam synchrotron beamline I12 (JEEP) at Diamond Light Source. Diffraction patterns from the bent polycrystalline Ti6Al4V samples were collected using the new 23-cell “horseshoe” detector and interpreted using Pawley refinement to extract unit cell parameters, thus allowing elastic strain to be determined. The tensile-compressive hardening asymmetry was quantified for the grains oriented with the basal plane perpendicular to the loading direction. Initial evaluation of the performance of the new instrument is reported. [Copyright &y& Elsevier]