This issue of MRS Bulletin focuses on the rapid progress that is ongoing in the development of hard x-ray microscopies with three-dimensional spatial resolutions ranging from micrometers to nanometers. The individual articles provide a crosscut of developments in hard x-ray projection tomography microscopy for imaging density and chemical fluctuations in crystalline and noncrystalline materials; large-angle diffractionbased, spatially resolved imaging of local structure, orientation, and strain distributions in crystalline materials; and emerging coherent diffraction imaging for nanometer-range Fourier transform imaging of crystalline and noncrystalline materials.

The key strength of hard x-ray full-field microscopy is the large penetration depth of hard x-rays into matter, which allows one to image the interior of opaque objects. Combined with tomographic techniques, the three-dimensional inner structure of an object can be reconstructed without the need for difficult and destructive sample preparation. Projection microscopy and microtomography are now routinely available at synchrotron radiation sources. The resolution of these techniques is limited by that of the detector to 1 µm or slightly less. X-ray images and tomograms at higher spatial resolution can be obtained by x-ray optical magnification, for example, by using parabolic refractive x-ray lenses as a magnifying optic. Combining magnifying x-ray imaging with tomography allows one to reconstruct the three-dimensional structure of an object, such as a microprocessor chip, with resolution well below 1 µm. In x-ray scanning microscopy, the sample is scanned through a small-diameter beam. The great advantage of scanning microscopy is that x-ray analytical techniques such as fluorescence analysis, diffraction, and absorption spectroscopy can be used as contrast mechanisms in the microscope. In combination with tomography, fluorescence analysis makes it possible to reconstruct the distribution of different chemical elements inside an object (fluorescence microtomography), while combining absorption spectroscopy with tomography yields the distribution of different oxidation states of atomic species.

Three-dimensional x-ray diffraction (3DXRD) microscopy is a tool for fast and nondestructive characterization of the individual grains, subgrains, and domains inside bulk materials. The method is based on diffraction with very penetrating hard x-rays (E ≥ 50 keV), enabling 3D studies of millimeter-to-centimeter-thick specimens.The position, volume, orientation, and elastic and plastic strain can be derived for hundreds of grains simultaneously. Furthermore, by applying novel reconstruction methods, 3D maps of the grain boundaries can be generated. The 3DXRD microscope in use at the European Synchrotron Radiation Facility in Grenoble, France, has a spatial resolution of ∼5 μm and can detect grains as small as 150 nm. The technique enables, for the first time, dynamic studies of the individual grains within polycrystalline materials. In this article, some fundamental materials science applications of 3DXRD are reviewed: studies of nucleation and growth kinetics during recrystallization, recovery, and phase transformations, as well as studies of polycrystal deformation.

In this article, the authors describe the principle and application of differential-aperture x-ray microscopy (DAXM). This recently developed scanning x-ray microprobe technique uses a confocal or traveling pinhole camera approach to determine the crystal structure, crystallographic orientation, and elastic and plastic strain tensors within bulk materials. The penetrating properties of x-rays make the technique applicable to optically opaque as well as transparent materials, and it is nondestructive; this provides for in situ, submicrometer-resolution characterization of local crystal structure and for measurements of microstructure evolution on mesoscopic length scales from tenths to hundreds of micrometers. Examples are presented that illustrate the use of DAXM to study grain and subgrain morphology, grain-boundary types and networks, and local intra- and intergranular elastic and plastic deformation. Information of this type now provides a direct link between the actual structure and evolution in materials and increasingly powerful computer simulations and multiscale modeling of materials microstructure and evolution.

X-rays have been widely used in the structural analysis of materials because of their significant penetration ability, at least on the length scale of the granularity of most materials. This allows, in principle, for fully three-dimensional characterization of the bulk properties of a material. One of the main advantages of x-ray diffraction over electron microscopy is that destructive sample preparation to create thin sections is often avoidable. A major disadvantage of x-ray diffraction with respect to electron microscopy is its inability to produce real-space images of the materials under investigation—there are simply no suitable lenses available. There has been significant progress in x-ray microscopy associated with the development of lenses, usually based on zone plates, Kirkpatrick–Baez mirrors, or compound refractive lenses. These technologies are far behind the development of electron optics, particularly for the large magnification ratios needed to attain high resolution. In this article, the authors report progress toward the development of an alternative general approach to imaging, the direct inversion of diffraction patterns by computation methods. By avoiding the use of an objective lens altogether, the technique is free from aberrations that limit the resolution, and it can be highly efficient with respect to radiation damage of the samples. It can take full advantage of the three-dimensional capability that comes from the x-ray penetration. The inversion step employs computational methods based on oversampling to obtain a general solution of the diffraction phase problem.