Synchrotron X-ray Diffraction Imaging Research Articles

Brittle fracture studied by ultra-high-speed synchrotron X-ray diffraction imaging.

In situ investigations of cracks propagating at up to 2.5 km s-1 along an (001) plane of a silicon single crystal are reported, using X-ray diffraction megahertz imaging with intense and time-structured synchrotron radiation. The studied system is based on the Smart Cut process, where a buried layer in a material (typically Si) is weakened by microcracks and then used to drive a macroscopic crack (10-1 m) in a plane parallel to the surface with minimal deviation (10-9 m). A direct confirmation that the shape of the crack front is not affected by the distribution of the microcracks is provided. Instantaneous crack velocities over the centimetre-wide field of view were measured and showed an effect of local heating by the X-ray beam. The post-crack movements of the separated wafer parts could also be observed and explained using pneumatics and elasticity. A comprehensive view of controlled fracture propagation in a crystalline material is provided, paving the way for the in situ measurement of ultra-fast strain field propagation.

Quantitative texture analysis of slates: An insight into slate’s elastic properties and their contribution to the understanding of seismic wave reflections in anisotropic materials

Slates are low-grade metamorphic rocks characterized by an alignment of the phyllosilicates, resulting in the development of a marked foliation. A consequence of this is a strong directional dependence of their elastic properties, which are tightly bound to their texture. The Rietveld analysis applied to synchrotron x-ray diffraction images of slates from the Truchas Syncline (NW Iberian Peninsula) will provide us with the orientation distribution function (ODF) of the principal minerals that constitute the rock. This textural analysis shows an exceptional alignment of phyllosilicates (muscovite and chlorite) in contrast with a poor orientation of other minerals such as quartz. In a later treatment of the data, the elastic properties of the slates, as well the variations of the seismic wave velocities, have been calculated from the ODF and the single crystal stiffness tensors. The results of both the elastic properties and the wave velocities can be used for the construction of models that allow to understand the reflections of seismic waves in markedly anisotropic materials, which is a matter of a great interest in the studies of the Earth’s lithosphere with seismic methods.

Dynamic observation of dislocation evolution and interaction with twin boundaries in silicon crystal growth using in – situ synchrotron X-ray diffraction imaging

The grown-in dislocation dynamics and interaction mechanisms with growth twins are investigated in-situ during the directional solidification of silicon crystal. The melting, solidification and cooling down process is performed in a dedicated installation at the European synchrotron radiation facility and is followed by X-ray Bragg diffraction imaging techniques (X-ray topography) at the mesoscale in real-time. Existing dislocations in the seed are observed to propagate in the up-grown crystal via replicas. They expand vertically with the moving solid-liquid interface being always aligned perpendicular to the growth front. During the solidification process when they meet a growth twin lamella (Σ3{111}), they neither pile-up nor transmit through the boundary. They are blocked by the twin, but they continue to move laterally behind the growth front due to the thermomechanical stresses in the system. The existence of dislocations at the solid-liquid interface, their evolution and interaction with twin boundaries is discussed, as growth proceeds, based on a detailed crystallographic analysis of the system.

Simultaneous scanning near-field optical and X-ray diffraction microscopy for correlative nanoscale structure-property characterization.

A multimodal imaging instrument has been developed that integrates scanning near-field optical microscopy with nanofocused synchrotron X-ray diffraction imaging. The instrument allows for the simultaneous nanoscale characterization of electronic/near-field optical properties of materials together with their crystallographic structure, facilitating the investigation of local structure-property relationships. The design, implementation and operating procedures of this instrument are reported. The scientific capabilities are demonstrated in a proof-of-principle study of the insulator-metal phase transition in samarium sulfide (SmS) single crystals induced by applying mechanical pressure via a scanning tip. The multimodal imaging of an in situ tip-written region shows that the near-field optical reflectivity can be correlated with the heterogeneously transformed structure of the near-surface region of the crystal.

Slate – A new record for crystal preferred orientation

This report describes microstructures and preferred orientation of a Devonian slate from the Belgian Ardennes (La Fortelle quarry). The sample, composed largely of muscovite, chlorite, and quartz, displays extraordinary texture strength of muscovite, exceeding 100 multiples of random distribution (m.r.d.) for (001) pole figures and thus setting a new record for preferred orientation in rocks. Quantitative texture analysis was performed with the Rietveld method on synchrotron X-ray diffraction images. Interestingly, quartz also displays strong shape preferred orientation (SPO) as revealed by X-ray microtomography and SEM imaging but largely random crystallographic preferred orientation (CPO). Microstructural evidence suggests that this fine-grained rock formed by recrystallization of shale under stress, with growth of phyllosilicates and dissolution and growth of quartz.

Quantitative analysis of domain textures in ferroelectric ceramics from single high-energy synchrotron X-ray diffraction images

In this study, the possibility of determining the orientation distribution function (ODF) and quantifying the domain textures of polycrystalline ferroelectrics based on single high-energy X-ray diffraction images using a Rietveld refinement method is assessed. A spherical harmonics texture model is incorporated in the approach to determine the ODFs for phase constituents in poled lead-free ferroelectric ceramics (1 − x)(Bi0.5Na0.5)TiO3 − xBaTiO3 with x = 0.0625 and 0.075 from both single high-energy synchrotron diffraction images and full rotation diffraction data collected with the samples rotated perpendicular to the poling axis. A quantitative comparison is made between the complete pole figures and pole density profiles obtained from the ODFs extracted from the different diffraction data. The results show that a good approximation to the domain textures of fiber-type in poled ceramics as determined from the full rotation data can be obtained from single diffraction images, with the dominant pole densities within a maximum difference of ∼0.15 multiples of a random distribution. It thus demonstrates that single high-energy X-ray diffraction images are suitable for the quantification of domain texture in ferroelectric ceramics. The analysis validates the applicability of high-energy synchrotron X-day diffraction to observe the texture evolution in situ in ferroelectric ceramics under fast or continuous loading conditions.

Synchrotron X-ray diffraction imaging studies of dislocations in Kyropoulos grown Ti doped sapphire crystal

In this study, X-ray diffraction and X-ray topography, using synchrotron radiation source, were used to analyse the nature of defects in a sapphire single crystal sample grown by Kyropoulos method. Qualitative and quantitative analysis were carried out on the results of the topography experiments. The dislocation density was found to be around 103–104 dislocations/cm2 indicating a crystal of good crystalline quality. Also, the variation of dislocation density with respect to the position on the sample was observed and discussed.

Characterization of defects in mono-like silicon for photovoltaic applications using X-ray Bragg diffraction imaging.

Rocking curve imaging (projection and section X-ray topography) has been used to study the generation and propagation of defects at the junctions between and above the seed crystals in mono-like silicon ingots. The images of different kinds of defects such as precipitates, dislocations and twins in the integrated intensity, full width at half-maximum and peak position maps resulting from the experiment have been studied. The qualitative and quantitative information that can be extracted from these maps, in particular the contrast of the images of the various defects, is discussed. These defects have a detrimental effect on solar cell efficiency and their detailed investigation allows clues to be obtained in order to improve the growth process. This work shows that synchrotron X-ray diffraction imaging techniques, because of their high angular resolution (<10-4°) and large field of view (several mm2), constitute a powerful tool for investigating the initial stages of growth of directionally solidified mono-like silicon.

Mono-like silicon ingots grown on low angle misoriented seeds: Defect characterization by synchrotron X-ray diffraction imaging

The present work studies the generation and propagation of sub-grain boundaries and dislocations in mono-like silicon ingots grown on monocrystalline seeds with a very small relative misorientation between them (<0.06° around the x, y and z axes). Special emphasis is put on the region close to the area between the seeds at the bottom of the crucible, which appears to be crucial in determining the crystalline quality of the final ingot. For this investigation, X-ray rocking curve imaging (RCI) in transmission geometry, a directly quantitative version of monochromatic beam Bragg diffraction imaging (“topography”) has been used. This technique has been developed at the European Synchrotron Radiation Facility (ESRF), beamline BM05 and allows us to visualize the spatial distribution of the lattice distortion of a single crystal. It was found that the solidified ingot takes the crystallographic orientation of the seeds without creating any distorted area at the interface. However, dislocation bunches having a strong screw component are generated between the seeds and propagate along the growth direction. Sub-grain boundaries above the top of the seeds, mainly composed of edge dislocations, were also observed. These have a detrimental influence on the minority carrier lifetime of the ingot, since, as is known, sub-grain boundaries show active recombination. In this work taking advantage of the high angular resolution and the sensitivity of the technique it was shown that a relative misorientation between the seeds (δθx, δθy, δθz) as small as 0.02° can produce cascades of dislocations that propagate and multiply higher up in the ingot becoming electrically active.

Rietveld texture analysis from synchrotron diffraction images. II. Complex multiphase materials and diamond anvil cell experiments

Synchrotron X-ray diffraction images are increasingly used to characterize crystallographic preferred orientation distributions (texture) of fine-grained polyphase materials. Diffraction images can be analyzed quantitatively with the Rietveld method as implemented in the software package Materials Analysis Using Diffraction. Here we describe the analysis procedure for diffraction images collected with high energy X-rays for a complex, multiphase shale, and for those collectedin situin diamond anvil cells at high pressure and anisotropic stress.

Rietveld texture analysis from synchrotron diffraction images. I. Calibration and basic analysis

Synchrotron X-ray diffraction images are increasingly used to characterize not only structural and microstructural features of polycrystalline materials, but also crystal preferred orientation distributions. Diffraction data can be analyzed quantitatively and efficiently with the Rietveld method and here the detailed procedure is reported from the experiment to the calibration of the two-dimensional detector and full analysis of the sample. In particular, we emphasize the advantage of doing the calibration inside the Rietveld least-squares fitting instead of a preliminary graphical calibration. Then the procedure is described to quantify crystal preferred orientations with the Rietveld method implemented in software “Materials Analysis Using Diffraction”. The process is illustrated for a US “nickel” coin, a 75 at.% copper 25 at.% nickel alloy with face-centered cubic structure and a strong cube texture.

Rietveld quantification of γ-C2S conversion rate supported by synchrotron X-ray diffraction images

The pure γ-Ca2SiO4 (γ-C2S) phase was prepared at 1623 K of calcining temperature, 10 h of holding time and furnace cooling. The β-C2S phase was obtained through γ-C2S conversion with the following calcination system which was adopted at 1473 K of calcining temperature, 1 h of holding time and then water-cooling. The conversion rate of γ-C2S was studied by the Rietveld quantitative laboratory X-ray powder diffraction supported by synchrotron X-ray diffraction images. The refinement results show that the final conversion rate of γ-C2S is higher than 92%. The absolute error of the γ-C2S conversion rate between two Rietveld refinements (sample with or without α-Al2O3) is 3.6%, which shows that the Rietveld quantitative X-ray diffraction analysis is an appropriate and accurate method to quantify the γ-C2S conversion rate.

Distribution of enamel crystallite orientation through an entire tooth crown studied using synchrotron X‐ray diffraction

The biomineralization of human dental enamel has resulted in a highly anisotropic and heterogeneous distribution of hydroxyapatite crystallites, which in combination with its high mineral content has resulted in one of the most durable and hardest tissues in the human body. In this study, we used position-sensitive synchrotron X-ray diffraction to quantify the spatial variation in the direction and magnitude of the preferred orientation of enamel crystallites across a whole tooth crown. Two-dimensional synchrotron X-ray diffraction images were collected with 300 μm spatial resolution over a series of six sequential tooth sections obtained from a single maxillary first premolar and were analyzed using Rietveld refinement. Both the magnitude and the direction of the crystallite orientation were found to have a high spatial heterogeneity. Areas of high crystallite alignment were directed perpendicular to the biting surfaces, which is thought to meet the functional requirements of mastication. The results may assist in our understanding of the structure-function relationship and of the evolutionary development of enamel.

Enhancement of mercuric iodide detector performance through increases in wafer uniformity by purification and crystal growth in microgravity

Wafers from mercuric iodide crystals grown in microgravity on two occasions have previously been found to be characterized by a higher hole mobility-lifetime product, which enables energy dispersive radiation detectors with superior resolution. In the present work, we have identified the specific structural modifications that are responsible for this enhanced performance. As a result of this study, the performance of terrestrial wafers also has been improved but not yet to the level of wafers grown in microgravity. High resolution synchrotron x-ray diffraction images of a series of wafers, including those grown both in microgravity and on the ground, reveal two principal types of structural changes that are interrelated. One of these, arrays of inclusions, affects performance far more strongly than the other, variation in lattice orientation. Inclusions can be formed either from residual impurities or in response to deviations from ideal stoichiometry. The formation of both types is facilitated by gravity-driven convection during growth. As the level of inclusions is reduced, through growth from material of higher purity, through the achievement of balanced stoichiometry, or by suppression of convection mixing during crystal growth, the hole mobility-lifetime product is enhanced in spite of an accompanying decreased uniformity in lattice orientation. Sixfold enhancement in the performance of x- and γ-ray detectors has been accomplished to date. Further augmentation in performance appears likely.

Enhancement of Mercuric Iodide Detector Performance Through Crystal Growth in Microgravity: the Roles of Lattice Order

AbstractThe hole-mobility•carrier-lifetime product of α mercuric iodide high energy radiation detectors has been enhanced through vapor crystal growth in microgravity. This improvement is closely correlated with specific characteristics of the crystal lattice, which have been identified by high resolution synchrotron x-ray diffraction imaging. These structural features and the associated performance are now being approached in terrestrial growth of α mercuric iodide.Gravity may affect the uniformity of this crystal lattice in two distinct ways: 1) directly through deformation that it imposes on the lattice during growth and 2) indirectly through convection, which mixes any extraneous material. Inclusions associated with these processes harden the lattice and facilitate lattice folding. These changes affect the electronic parameters of detectors made from the crystals. As purification procedures are optimized, the incorporation of extraneous material is curtailed, enhancing electronic properties in spite of lattice flexing through loss of precipitation hardening.These studies provide insight into the contribution of various aspects of crystalline order in α-mercuric iodide crystals to property improvement. This knowledge has led to modification of requirements for starting materials, adjustment of physical vapor growth procedures, and change in crystal handling procedures. As a result, the electronic performance of terrestrially grown radiation detectors has been improved, and we provide evidence that further enhancement is still possible.

Growth and characteristics of tgs crystals grown aboard first international microgravity laboratory (IML-1)

Abstract The growth and detector characteristics of TGS crystals grown in a low gravity environment of space are presented. High resolution monochromatic synchrotron X-ray diffraction imaging of the space grown crystal indicates an extraordinary crystal quality.