Advanced materials and processing techniques are based largely on the generation and control of non-homogeneous microstructures, such as precipitates and grain boundaries. X-ray tomography can provide three-dimensional density and chemical distributions of such structures with submicrometre resolution; structural methods exist that give submicrometre resolution in two dimensions; and techniques are available for obtaining grain-centroid positions and grain-average strains in three dimensions. But non-destructive point-to-point three-dimensional structural probes have not hitherto been available for investigations at the critical mesoscopic length scales (tenths to hundreds of micrometres). As a result, investigations of three-dimensional mesoscale phenomena--such as grain growth, deformation, crumpling and strain-gradient effects--rely increasingly on computation and modelling without direct experimental input. Here we describe a three-dimensional X-ray microscopy technique that uses polychromatic synchrotron X-ray microbeams to probe local crystal structure, orientation and strain tensors with submicrometre spatial resolution. We demonstrate the utility of this approach with micrometre-resolution three-dimensional measurements of grain orientations and sizes in polycrystalline aluminium, and with micrometre depth-resolved measurements of elastic strain tensors in cylindrically bent silicon. This technique is applicable to single-crystal, polycrystalline, composite and functionally graded materials.

We present a unified model for thin film epitaxy where single crystal films with small and large lattice misfits are grown by domain matching epitaxy (DME). The DME involves matching of lattice planes between the film and the substrate having similar crystal symmetry. In this framework, the conventional lattice matching epitaxy becomes a special case where a matching of lattice constants or the same planes is involved with a small misfit of less than 7%–8%. In large lattice mismatch systems, we show that epitaxial growth of thin films is possible by matching of domains where integral multiples of major lattice planes match across the interface. We illustrate this concept with atomic-level details in the TiN/Si(100) with 3/4 matching, the AlN/Si(100)with 4/5 matching, and the ZnO/α−Al2O3(0001) with 6/7 matching of major planes across the film/substrate interface. By varying the domain size, which is equal to intregral multiple of lattice planes, in a periodic fashion, it is possible to accommodate additional misfit beyond perfect domain matching. Thus, we can potentially design epitaxial growth of films with any lattice misfit on a given substrate with atomically clean surfaces. In situ x-ray diffraction studies on initial stages of growth of ZnO films on sapphire correctly identify a compressive stress and a rapid relaxation within 1 to 2 monolayers, consistent with the DME framework and the fact that the critical thickness is less than 1 monolayer. DME examples ranging from the Ge–Si/Si(100) system with 49/50 matching (2% strain) to metal/Si systems with 1/2 matching (50% strain) are tabulated, strategies for growing strain-free films by engineering the misfit to be confined near the interface are presented, and the potential for epitaxial growth of films with any lattice misfit on a given substrate with atomically clean surfaces is discussed.

The distribution of elastic strains (and thus stresses) at the submicrometre length scale within deformed metal single crystals has remarkably broad implications for our understanding of important physical phenomena. These include the evolution of the complex dislocation structures that govern mechanical behaviour within individual grains, the transport of dislocations through such structures, changes in mechanical properties that occur during reverse loading (for example, sheet-metal forming and fatigue), and the analyses of diffraction line profiles for microstructural studies of these phenomena. We present the first direct, spatially resolved measurements of the elastic strains within individual dislocation cells in copper single crystals deformed in tension and compression along <001> axes. Broad distributions of elastic strains are found, with important implications for theories of dislocation structure evolution, dislocation transport, and the extraction of dislocation parameters from X-ray line profiles.

Nonresonant inelastic x-ray scattering measurements on NiO and CoO show that strong dipole-forbidden d-d excitations appear within the Mott gap at large wave vectors. These dominant excitations are highly anisotropic, and have [001] nodal directions for NiO. Theoretical analyses based on a novel, energy-resolved Wannier function (within the local density approximation+Hubbard U) show that the anisotropy reflects the local exciton wave functions and local point-group symmetry. The sensitivity to weak symmetry breaking in particle-hole wave functions suggests a wide application to strongly correlated systems.

Abstract