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Abstract: A spatially resolved X-ray diffraction method – with a submicron 3D resolution together with SEM and OIM analysis are applied to understand the arrangements of voids, geometrically necessary dislocations and strain gradient distributions in samples of Al (123) and Cu (001) single crystals shocked to incipient spallation fracture. We describe how geometrically necessary dislocations and the effective strain gradient alter white beam Laue patterns of the shocked materials. Several distinct structural zones are observed at different depths under the impact surface. The density of geometrically necessary dislocations (GNDs) is extremely high near the impact and back surface of the shock recovered crystals. The spall region is characterized by a large density of mesoscale voids and GNDs. The spall region is separated from the impact and back surfaces by compressed regions with high total dislocation density but lower GNDs density. Self-organization of shear bands is observed in the shock recovered Cu single crystal. [Copyright &y& Elsevier]

Abstract: Timely development of materials for the demanding fusion energy environment requires a broad range of advanced scientific tools, including advanced structural characterization methods. The current state-of-the-art and emerging capabilities in electron microscopy, atom probe tomography, neutron scattering and X-ray scattering are reviewed with respect to potential applications in fusion materials research and development. Recent dramatic advances in capabilities in all four of these characterization tools are transforming the spatial precision and quantitative information that can be extracted during structural characterization. Examples include spectroscopic identification of single atoms in bulk materials, three-dimensional mapping of millimeter-scale volumes of materials with nanometer resolution, and high-resolution in situ measurements of internal stress and strain during mechanical testing. [Copyright &y& Elsevier]

Abstract: Polychromatic microdiffraction uses small X-ray beams to characterize the local crystallographic structure of materials. When combined with a depth resolving technique called differential aperture microscopy, the phase and local orientation of femto-liter volumes (0.5×0.5×0.7μm3) can be resolved beneath the surface of a sample. In addition, the local elastic strain and dislocation tensors can also be determined and the local dislocation type can be modeled. Here we present recent technical developments, including example applications and emerging research directions. [Copyright &y& Elsevier]

Abstract: Variations in the local crystallographic orientation due to the presence of geometrically necessary dislocations and dislocation boundaries smear the distribution of intensity near Laue reflections. Here, some simple model distributions of geometrically necessary dislocations, GNDs, are used to estimate the dislocation tensor field from the intensity distribution of Laue peaks. Streaking of the Laue spots is found to be quantitatively and qualitatively distinct depending on the ratio between the absorption coefficient and the GND density gradient. In addition, different slip systems cause distinctly different Laue-pattern streaking. Experimental Laue patterns are therefore sensitive to stored dislocations and GNDs. As an example, white beam microdiffraction was applied to characterize the dislocation arrangement in a deformed polycrystalline Ni grain during in situ uniaxial tension. [Copyright &y& Elsevier]

Abstract: Three-dimensional (3D) measurements of strain tensor distributions with subgrain resolution are now possible due to an emerging class of instrumentation: the 3D X-ray crystal microscopes. These instruments combine ultra-intense synchrotron X-ray sources and advanced X-ray optics to probe polycrystalline materials with submicron spatial resolution. By employing polychromatic X-ray beams and a virtual pinhole camera method, called differential aperture microscopy, 3D distributions of the local crystalline phase, orientation (local texture) and elastic and plastic strain tensor distributions can be measured with resolution below the grain size of most materials. The elastic strain tensor elements can typically be determined with uncertainties less than 100ppm in brittle materials. Orientations can be quantified to ∼0.01° and the local unpaired dislocation density can be measured in ductile materials. Efforts are underway to improve the spatial resolution and increase the depth probed. Because the 3D X-ray crystal microscope is a penetrating nondestructive tool, it is ideal for studies of mesoscale structural evolution in materials. The unprecedented information that can be obtained with this new class of instrumentation is certain to advance our understanding of the materials physics underpinning the behavior of polycrystalline materials. [Copyright &y& Elsevier]

Abstract: Advanced polychromatic microdiffraction is sensitive to the organization of dislocations and other defects that rotate the lattice planes. Using ultra-brilliant third-generation synchrotron sources and non-dispersive X-ray focusing optics, it is now possible to analyze individual dislocation cells and walls at a submicron scale that cannot be probed by traditional methods. The method is applied to an Ir weld sample to illustrate how microdiffraction can be used to determine the locally active dislocation system. [Copyright &y& Elsevier]

Abstract: X-ray microdiffraction is a non-destructive technique that allows for depth-resolved, strain measurements with submicron spatial resolution. These capabilities make this technique promising for understanding the mechanical properties of MicroElectroMechancial Systems (MEMS). This investigation examined the local strain induced by irradiating a polycrystalline diamond thin film with a dose of 2×1017 H+/cm2 protons. Preliminary results indicate that a measurable strain, on the order of 10−3, was introduced into the film near the End of Range (EOR) region of the protons. [Copyright &y& Elsevier]

Abstract: We report on three-dimensional spatially resolved X-ray microdiffraction measurements of inhomogeneous deformation within individual polycrystalline grains. These measurements provide new insights into the role of grain boundaries. Particularly striking is the qualitatively different mechanical behavior of subgrain volumes near grain boundaries and triple junctions compared to bulk-grain mechanical behavior. These differences are studied by characterizing the evolution of the local orientation distribution in a polycrystalline Ni sample using polychromatic synchrotron X-ray microdiffraction. Dependence of deformation on grain boundary types and triple junctions is determined. Quantitative distinctions in deformation behavior between low-angle boundaries, special low-energy high-angle boundaries, general high-angle boundaries and triple junctions are characterized in terms of spatially resolved misorientation development and extensions of grain boundary effects. In general, larger lattice misorientations are observed near boundaries with higher grain boundary energy. Special high-coincidence grain boundaries exhibit smaller deformation misorientations than general high-angle grain boundaries. These observations are consistent with the observed increases in ductility in grain boundary engineered materials. [Copyright &y& Elsevier]

The depth-dependent strain gradients near buried interfaces in a model system of NiAl–Mo composite were nondestructively probed with 3-D X-ray microdiffraction. Coupled with micromechanical analysis, our study shows that the relaxation of the residual thermal strains in the NiAl–Mo composites results in the formation of a near-surface “slip zone” with large strain gradients in both the reinforcing Mo fibers and NiAl matrix. Based on these results an approach to calculate the fiber–matrix interface strength for composite materials is suggested. [ABSTRACT FROM AUTHOR]

Abstract: Three-dimensional spatially resolved strains were mapped in a model NiAl/Mo composite after nanoindentation. The depth-dependent strain distributed in the two phases and partitioned across the composite interfaces is directly measured at submicron length scale using X-ray microdiffraction and compared with a detailed micromechanical stress analysis. It is shown that indentation-induced deformation in the composite material is distinct from deformation expected in a single-phase material. This difference arises in part from residual thermal strains in both phases of the composite in the as-grown state. Interplay between residual thermal strains and external mechanical strain results in a complex distribution of dilatational strain in the Mo fibers and NiAl matrix and is distinct in different locations within the indented area. Reversal of the strain sign (e.g., alternating tensile/compressive/tensile strain distribution) is observed in the NiAl matrix. Bending of the Mo fibers during indentation creates relatively large ∼1.5° misorientations between the different fibers and NiAl matrix. Compressive strain along the 〈001〉 direction reached −0.017 in the Mo fibers and −0.007 in the NiAl matrix. [ABSTRACT FROM AUTHOR]

Abstract: We compare experimental measurements of inhomogeneous plastic deformation in a Ni bicrystal with crystal plasticity simulations. Polychromatic X-ray microdiffraction, orientation imaging microscopy and scanning electron microscopy, were used to characterize the geometrically necessary dislocation distribution of the bicrystal after uniaxial tensile deformation. Changes in the local crystallographic orientations within the sample reflect its plastic response during the tensile test. Elastic strain in both grains increases near the grain boundary. Finite element simulations were used to understand the influence of initial grain orientation and structural inhomogeneities on the geometrically necessary dislocations arrangement and distribution and to understand the underlying materials physics. [Copyright &y& Elsevier]

A recently developed differential-aperture X-ray microscopy (DAXM) technique provides local structure and crystallographic orientation with submicron spatial resolution in three-dimensions; it further provides angular precision of ∼0.01° and local elastic strain with an accuracy of ∼1.0×10−4 using microbeams from high brilliance third generation synchrotron X-ray sources. DAXM is a powerful tool for inter- and intra-granular studies of lattice distortions and lattice rotations on mesoscopic length scales of tenths of microns to hundreds of microns that are largely above the range of traditional electron microscopy probes. Nondestructive, point-to-point, spatially resolved measurements of local lattice orientations in bulk materials provide direct information on geometrically necessary dislocation density distributions through measurements of the lattice curvature in plastically deformed materials. This paper reviews the DAXM measurement technique and discusses recent demonstrations of DAXM capabilities for measurements of microtexture, local elastic strain, and plastic deformation microstructure. [Copyright &y& Elsevier]

X-ray microbeams have been used to perform nondestructive measurements of the local orientations and microstructure in single-crystal and grain-boundary regions in a columnar Al (0.2 wt.% Mg) tri-crystal deformed 20% in plane-strain. The measurements were made using a recently developed differential-aperture X-ray microscopy (DAXM) technique providing high angular resolution determinations of local orientations with micron 3-D spatial resolution using focused microbeams. The X-ray microbeam technique is described, three-dimensional spatially resolved pole-figures and lattice rotation distributions in single-crystal and grain-boundary regions are presented, and the potential of micron resolution 3-D X-ray structural microscopy for plastic deformation investigations is discussed. [Copyright &y& Elsevier]