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.2015 Jan 14:6:6098.
doi: 10.1038/ncomms7098.

Dark-field X-ray microscopy for multiscale structural characterization

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Dark-field X-ray microscopy for multiscale structural characterization

H Simons et al. Nat Commun..

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Abstract

Many physical and mechanical properties of crystalline materials depend strongly on their internal structure, which is typically organized into grains and domains on several length scales. Here we present dark-field X-ray microscopy; a non-destructive microscopy technique for the three-dimensional mapping of orientations and stresses on lengths scales from 100 nm to 1 mm within embedded sampling volumes. The technique, which allows 'zooming' in and out in both direct and angular space, is demonstrated by an annealing study of plastically deformed aluminium. Facilitating the direct study of the interactions between crystalline elements is a key step towards the formulation and validation of multiscale models that account for the entire heterogeneity of a material. Furthermore, dark-field X-ray microscopy is well suited to applied topics, where the structural evolution of internal nanoscale elements (for example, positioned at interfaces) is crucial to the performance and lifetime of macro-scale devices and components thereof.

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Figures

Figure 1
Figure 1. Principle of dark-field X-ray microscopy.
A monochromatic beam from a synchrotron source illuminates the sample. An embedded crystalline element (for example, a grain or domain) of choice (green) is aligned such that the beam is diffracted. The objective magnifies the diffracted beam by a factorM=q′/p′ and generates an inverted 2D projection of the grain. Through repeated exposures during a 360° rotation of the element around an axis parallel to the diffraction vector, G, several 2D projections of the grain are obtained from various angles. A 3D map is then obtained by combining these projections using reconstruction algorithms similar to those developed for CT scanning. If the lattice of the crystalline element exhibits an internal orientation spread, this procedure is repeated for a number of sample tilts, indicated by the anglesα andβ. Using a compound refractive lens as the objective enables one to enlarge or reduce the spatial resolution and field of view within the sample by varying the number of individual lenses and adjustingp′ andq′ correspondingly. The diffraction angle 2θ is typically 10–30°.
Figure 2
Figure 2. Multiscale mapping of 10% tensile deformed aluminium.
Above: (a) Part of the X-ray mapping of all grains in the specimen. (b) Zooming in on one embedded grain and mapping the intrinsic variation in orientation. A vertical section through the grain is shown for ease of inspection of the spatial heterogeneity. (c) Condensing the incoming beam vertically defines a sub-micron layer within the grain. Mapping individual subgrains in 3D is then obtained by ‘stacking’ these layers. The spatial resolution from left to right is 3.5 μm, 1.5 μm and 300 nm, and the angular resolution is 0.5°, 0.15° and 0.03°, respectively. Below: The corresponding keys for the orientation maps. (a) the colour scheme is represented in an inverse pole figure. (b,c) the colour schemes symbolize the required tiltsα andβ to align the [200] direction with the diffraction vector.
Figure 3
Figure 3. Study of recovery in tensile deformed aluminium.
Shown is a 2D map of one layer in the sample, (a) after annealing for 0.5 h at 246 °C, and (b) after additional annealing for 0.5 h at 257 °C. The colours symbolize the orientation of the [200] direction of the crystalline lattice with respect to the specimen reference system,cf.Fig. 1. Shown in (c) is a difference map with white, blue and red representing local changes in orientation below 0.01° between 0.01° and 0.2° and above 0.2°, respectively. The spatial resolution is 300 nm.
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