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Preview: Journal of Applied Crystallography

Journal of Applied Crystallography



Journal of Applied Crystallography covers a wide range of crystallographic topics from the viewpoints of both techniques and theory. The journal presents articles on the application of crystallographic techniques and on the related apparatus and computer



Published: 2017-05-25

 



Threefold rotational symmetry in hexagonally shaped core–shell (In,Ga)As/GaAs nanowires revealed by coherent X-ray diffraction imaging

2017-04-13

Coherent X-ray diffraction imaging at symmetric hhh Bragg reflections was used to resolve the structure of GaAs/In0.15Ga0.85As/GaAs core–shell–shell nanowires grown on a silicon (111) substrate. Diffraction amplitudes in the vicinity of GaAs 111 and GaAs 333 reflections were used to reconstruct the lost phase information. It is demonstrated that the structure of the core–shell–shell nanowire can be identified by means of phase contrast. Interestingly, it is found that both scattered intensity in the (111) plane and the reconstructed scattering phase show an additional threefold symmetry superimposed with the shape function of the investigated hexagonal nanowires. In order to find the origin of this threefold symmetry, elasticity calculations were performed using the finite element method and subsequent kinematic diffraction simulations. These suggest that a non-hexagonal (In,Ga)As shell covering the hexagonal GaAs core might be responsible for the observation.



Incorporation of interfacial roughness into recursion matrix formalism of dynamical X-ray diffraction in multilayers and superlattices

2017-04-13

Diffraction in multilayers in the presence of interfacial roughness is studied theoretically, the roughness being considered as a transition layer. Exact (within the framework of the two-beam dynamical diffraction theory) differential equations for field amplitudes in a crystalline structure with varying properties along its surface normal are obtained. An iterative scheme for approximate solution of the equations is developed. The presented approach to interfacial roughness is incorporated into the recursion matrix formalism in a way that obviates possible numerical problems. Fitting of the experimental rocking curve is performed in order to test the possibility of reconstructing the roughness value from a diffraction scan. The developed algorithm works substantially faster than the traditional approach to dealing with a transition layer (dividing it into a finite number of thin lamellae). Calculations by the proposed approach are only two to three times longer than calculations for corresponding structures with ideally sharp interfaces.



X-ray dynamical diffraction in amino acid crystals: a step towards improving structural resolution of biological molecules via physical phase measurements

2017-05-08

In this work, experimental and data analysis procedures were developed and applied for studying amino acid crystals by means of X-ray phase measurements. The results clearly demonstrated the sensitivity of invariant triplet phases to electronic charge distribution in d-alanine crystals, providing useful information for molecular dynamics studies of intermolecular forces. The feasibility of using phase measurements to investigate radiation damage mechanisms is also discussed on experimental and theoretical grounds.



Reconstruction of the near-field distribution in an X-ray waveguide array

2017-05-16

Iterative phase retrieval has been used to reconstruct the near-field distribution behind tailored X-ray waveguide arrays, by inversion of the measured far-field pattern recorded under fully coherent conditions. It is thereby shown that multi-waveguide interference can be exploited to control the near-field distribution behind the waveguide exit. This can, for example, serve to create a secondary quasi-focal spot outside the waveguide structure. For this proof of concept, an array of seven planar Ni/C waveguides are used, with precisely varied guiding layer thickness and cladding layer thickness, as fabricated by high-precision magnetron sputtering systems. The controlled thickness variations in the range of 0.2 nm results in a desired phase shift of the different waveguide beams. Two kinds of samples, a one-dimensional waveguide array and periodic waveguide multilayers, were fabricated, each consisting of seven C layers as guiding layers and eight Ni layers as cladding layers. These are shown to yield distinctly different near-field patterns.



Interface-sensitive imaging by an image reconstruction aided X-ray reflectivity technique

2017-05-25

Recently, the authors have succeeded in realizing X-ray reflectivity imaging of heterogeneous ultrathin films at specific wavevector transfers by applying a wide parallel beam and an area detector. By combining in-plane angle and grazing-incidence angle scans, it is possible to reconstruct a series of interface-sensitive X-ray reflectivity images at different grazing-incidence angles (proportional to wavevector transfers). The physical meaning of a reconstructed X-ray reflectivity image at a specific wavevector transfer is the two-dimensional reflectivity distribution of the sample. In this manner, it is possible to retrieve the micro-X-ray reflectivity (where the pixel size is on the microscale) profiles at different local positions on the sample.



Structure diagnostics of heterostructures and multi-layered systems by X-ray multiple diffraction

2017-05-25

This article presents the results of research on multi-layered heterostructures by a modified calculation technique of multiple X-ray diffraction. The AlxIn1−xSb heterostructure and a Zn(Mn)Se/GaAs(001) multi-layered system were used as models to specify conditions for cases of coincidental coplanar three-beam or coincidental noncoplanar four-beam X-ray diffraction. These conditions provide the means for a high-precision determination of lattice parameters and strain anisotropy in layers.



Modelling and validation of particle size distributions of supported nanoparticles using the pair distribution function technique

2017-04-13

The particle size of supported catalysts is a key characteristic for determining structure–property relationships. It is a challenge to obtain this information accurately and in situ using crystallographic methods owing to the small size of such particles (<5 nm) and the fact that they are supported. In this work, the pair distribution function (PDF) technique was used to obtain the particle size distribution of supported Pt catalysts as they grow under typical synthesis conditions. The PDF of Pt nanoparticles grown on zeolite X was isolated and refined using two models: a monodisperse spherical model (single particle size) and a lognormal size distribution. The results were compared and validated using scanning transmission electron microscopy (STEM) results. Both models describe the same trends in average particle size with temperature, but the results of the number-weighted lognormal size distributions can also accurately describe the mean size and the width of the size distributions obtained from STEM. Since the PDF yields crystallite sizes, these results suggest that the grown Pt nanoparticles are monocrystalline. This work shows that refinement of the PDF of small supported monocrystalline nanoparticles can yield accurate mean particle sizes and distributions.



Simultaneous determination of high-temperature crystal structure and texture of synthetic porous cordierite

2017-04-13

The evolution of the crystal structure and crystallographic texture of porous synthetic cordierite was studied by in situ high-temperature neutron diffraction up to 1373 K, providing the first in situ high-temperature texture measurement of this technologically important material. It was observed that the crystal texture slightly weakens with increasing temperature, concurrently with subtle changes in the crystal structure. These changes are in agreement with previous work, leading the authors to the conclusion that high-temperature neutron diffraction allows reliable crystallographic characterization of materials with moderate texture. It was also observed that structural changes occur at about the glass transition temperature of the cordierite glass (between 973 and 1073 K). Crystal structure refinements were conducted with and without quantitative texture analysis being part of the Rietveld refinement, and a critical comparison of the results is presented, contributing to the sparse body of literature on combined texture and crystal structure refinements.



Growth of a bulk-size single crystal of sulphamic acid by an in-house developed seed rotation solution growth technique and its characterization

2017-04-27

A bulk sulphamic acid single crystal has been grown by a modified seed rotation technique. The lattice dimensions of the grown single crystal were confirmed using powder X-ray diffraction, and it was found that it crystallized in an orthorhombic structure with space group Pbca. The strain in the lattice was calculated by the Williamson–Hall equation. The crystalline perfection was examined by high-resolution X-ray diffraction and found to be extremely good (the single peak of the rocking curve having an FWHM of ∼8.0′′). The luminescence behaviour was recorded in the wavelength region between 400 and 630 nm using an Xe flash lamp which acts as an excitation source. The shock damage threshold was measured for the grown crystal in order to determine the mechanical capability of the title compound. The thermal parameter of sulphamic acid was calculated by photoacoustic spectroscopy.



Investigations into the phase composition of zirconia-based sinters with an axial texture

2017-04-27

Owing to the phase transition of the tetragonal form of ZrO2 into the monoclinic one, caused by mechanical stresses, preparation of powder samples for quantitative phase analysis by the X-ray diffraction method should be avoided. The process of grinding of zirconia sinters leads to considerable changes in their phase composition. For this reason, a quantitative phase analysis should be conducted on solid samples not subjected to mechanical stresses, irrespective of problems appearing during experiments and analysis. One such problem is preferred crystallographic orientation (texture). This paper describes the influence of a preferred crystallographic orientation on the quantitative phase analysis conducted on solid samples and presents the results of an analysis in which corrections for uniaxial and multiaxial textures were applied. It was found that the examined samples had a very weak but nonzero multiaxial texture. The share of the randomly oriented fraction in the examined sinters was determined to be ca 94 vol.% and the share of the textured fraction ca 6 vol.%. From the statistical point of view, in the case of small amounts of the textured fraction, a correction on one distinguished crystallographic plane can overcome this problem. In the case of the slightly textured sinters of metering nozzles subjected to investigation here, the correction related to all the unique directions was statistically insignificant because the textured part corresponds to only a small volume fraction. However, corrections related to all texture axes considerably improve the fit of the calculated X-ray pattern with the experimental one and help to better characterize the examined materials.



Bayesian approach to powder phase identification

2017-04-27

Identification of unknown materials using X-ray powder diffraction patterns is a commonly used and well established technique with a number of proved implementations. Generally, qualitative phase analysis of X-ray diffraction data includes ranking of candidate phases on the basis of similarity of their diffraction patterns to the measured one. A standard strategy of such a ranking by algorithmization of manual search criteria may become inconvenient for modification and adaptation for problems that are not supported by our intuition. Here, the problem of providing physically grounded expressions for candidate phase ranking is addressed. The approach is based on calculation of Bayesian posterior probabilities of the phases' presence in the sample. The choice of the expressions for the prior probabilities for deviations of phases' diffraction patterns from database entries determines the degree of physical detailing and may be made according to the specifics of the problem being solved. It is shown that even for simple exponential expressions for prior probabilities the approach identifies the phases for IUCr round robin cases correctly, as well as ensuring sufficient robustness of the results with respect to diffraction peak shifts and intensity variations.



Appearance of efficient luminescence energy transfer in doped orthovanadate nanocrystals

2017-04-27

This paper reports the detailed synthesis mechanism and the structural, morphological and optical characterization of ultraviolet (∼311 nm) excitable samarium doped gadolinium yttrium orthovanadate, (Gd,Y)VO4:Sm3+, nanocrystals. X-ray diffraction and Rietveld refinement studies confirmed that the synthesized samples crystallize in a tetragonal structure with I41/amd space group. The enhanced photoluminescence intensity of (Gd,Y)VO4:Sm3+ compared with the existing YVO4:Sm3+ phosphor clearly indicates the significant role of Gd3+ ions. This has been attributed to the sensitization of the 6PJ energy level of Gd3+ ions by energy transfer from orthovanadate (VO43−) ions and subsequent energy trapping by Sm3+ ions. The energy transfer from VO43− to Sm3+ via Gd3+ ions as intermediates and concentration quenching of Gd3+ luminescence are discussed in detail. The optical band gap of the as-prepared nanocrystals has been estimated using UV–vis–NIR absorption spectroscopy, which reveals a slightly higher band gap (3.75 eV) for YVO4 as compared to GdYVO4 (3.50 eV). Furthermore, confocal microcopy, decay parameters and Commission Internationale de l'Eclairage chromatic coordinates have supplemented these studies, which established the suitability of these nanophosphors for achieving spectral conversion in silicon solar cells.



The origin of striation in the metastable β phase of titanium alloys observed by transmission electron microscopy

2017-05-08

For the β phase of Ti-5553-type metastable β-Ti alloys, striations in transmission electron microscopy (TEM) bright- and dark-field images have been frequently observed but their origin has not been sufficiently investigated. In the present work, this phenomenon is studied in depth from the macroscopic scale by neutron diffraction to the atomic scale by high-resolution TEM. The results reveal that the β phase contains homogeneously distributed modulated structures, intermediate between that of the β phase (cubic) and that of the α phase or the ω phase (hexagonal), giving rise to the appearance of additional diffraction spots at 1/2, 1/3 and 2/3 β diffraction positions. The intermediate structure between β and α is formed by the atomic displacements on each second {110}β plane in the \langle 1{\overline 1}0\rangle_{\beta} direction, whereas that between β and ω is formed by atomic displacements on each second and third {112}β plane in the opposite \langle 11{\overline 1}\rangle_{\beta } direction. Because of these atomic displacements, the {110}β and {112}β planes become faulted, resulting in the streaking of β diffraction spots and the formation of extinction fringes in TEM bright- and dark-field images, the commonly observed striations. The present work reveals the origin of the striations and the intrinsic correlation with the additional electron reflections of the β phase.



Robust X-ray angular correlations for the study of meso-structures

2017-05-08

As self-assembling nanomaterials become more sophisticated, it is becoming increasingly important to measure the structural order of finite-sized assemblies of nano-objects. These mesoscale clusters represent an acute challenge to conventional structural probes, owing to the range of implicated size scales (10 nm to several micrometres), the weak scattering signal and the dynamic nature of meso-clusters in native solution environments. The high X-ray flux and coherence of modern synchrotrons present an opportunity to extract structural information from these challenging systems, but conventional ensemble X-ray scattering averages out crucial information about local particle configurations. Conversely, a single meso-cluster scatters too weakly to recover the full diffraction pattern. Using X-ray angular cross-correlation analysis, it is possible to combine multiple noisy measurements to obtain robust structural information. This paper explores the key theoretical limits and experimental challenges that constrain the application of these methods to probing structural order in real nanomaterials. A metric is presented to quantify the signal-to-noise ratio of angular correlations, and it is used to identify several experimental artifacts that arise. In particular, it is found that background scattering, data masking and inter-cluster interference profoundly affect the quality of correlation analyses. A robust workflow is demonstrated for mitigating these effects and extracting reliable angular correlations from realistic experimental data.



Quantitative phase analysis using observed integrated intensities and chemical composition data of individual crystalline phases: quantification of materials with indefinite chemical compositions

2017-05-08

In a previous report, a new method for quantitative phase analysis (QPA) of multi-component mixtures using a conventional X-ray powder diffractometer was proposed. The formula for deriving weight fractions of individual crystalline phases presented therein includes sets of observed integrated intensities measured in a wide 2\theta range, chemical formula weights and sums of squared numbers of electrons belonging to atoms in respective chemical formula units [Toraya (2016). J. Appl. Cryst. 49, 1508–1516]. The latter two parameters required to perform QPA could be calculated from only the information of chemical formulae of individual phases. In the present study, these two parameters are replaced with a single parameter in the form new parameter = (chemical formula weight)/(sum of squared numbers of electrons). As will be expected from this definition, the parameter has nearly equal values for groups of materials consisting of similar kinds of atoms, and its value becomes identical for polytypes or polymorphs having the same chemical composition. That characteristic of this parameter makes it possible to estimate the parameter value not only directly from the chemical composition of the target material itself but also from database-stored chemical analysis data sorted on the basis of mineral or chemical composition. The parameter value is also hardly changed as a result of small compositional variations of the target component material. Therefore, the present method can be applied to QPA of materials not only of definite chemical compositions but also of indefinite chemical compositions without degrading the accuracy of the analysis. This is expected to widen the application to QPA of, for example, natural products containing many kinds of trace elements, industrial materials with complex substitutional replacement of atoms, nonstoichiometric compounds etc. The theory and some examples of applications are presented. A procedure for quantifying unknown material is also proposed.



Epitaxial Ni nanoparticles on CaF2(001), (110) and (111) surfaces studied by three-dimensional RHEED, GIXD and GISAXS reciprocal-space mapping techniques

2017-05-16

The development of growth techniques aimed at the fabrication of nanoscale heterostructures with layers of ferroic 3d metals on semiconductor substrates is very important for their potential usage in magnetic media recording applications. A structural study is presented of single-crystal nickel island ensembles grown epitaxially on top of CaF2/Si insulator-on-semiconductor heteroepitaxial substrates with (111), (110) and (001) fluorite surface orientations. The CaF2 buffer layer in the studied multilayer system prevents the formation of nickel silicide, guides the nucleation of nickel islands and serves as an insulating layer in a potential tunneling spin injection device. The present study, employing both direct-space and reciprocal-space techniques, is a continuation of earlier research on ferromagnetic 3d transition metals grown epitaxially on non-magnetic and magnetically ordered fluorides. It is demonstrated that arrays of stand-alone faceted nickel islands with a face-centered cubic lattice can be grown controllably on CaF2 surfaces of (111), (110) and (001) orientations. The proposed two-stage nickel growth technique employs deposition of a thin seeding layer at low temperature followed by formation of the islands at high temperature. The application of an advanced three-dimensional mapping technique exploiting reflection high-energy electron diffraction (RHEED) has proved that the nickel islands tend to inherit the lattice orientation of the underlying fluorite layer, though they exhibit a certain amount of {111} twinning. As shown by scanning electron microscopy, grazing-incidence X-ray diffraction (GIXD) and grazing-incidence small-angle X-ray scattering (GISAXS), the islands are of similar shape, being faceted with {111} and {100} planes. The results obtained are compared with those from earlier studies of Co/CaF2 epitaxial nanoparticles, with special attention paid to the peculiarities related to the differences in lattice structure of the deposited metals: the dual-phase hexagonal close-packed/face-centered cubic lattice structure of cobalt as opposed to the single-phase face-centered cubic lattice structure of nickel.



Calculation of two-dimensional scattering patterns for oriented systems

2017-05-16

A versatile procedure to calculate two-dimensional scattering patterns of oriented systems is presented. The systems are represented by a set of dummy atoms with different scattering length densities, which allows the construction of very complex shapes either for single particles or for sets of particles. By the use of oriented pair distance distribution functions it is possible to perform a fast calculation of the scattering intensity from the oriented system in a given direction in the scattering vector (q) space and generate the two-dimensional scattering pattern on a given q plane. Several examples of the calculations are presented, demonstrating the method and its applicability. The presented results open new possibilities for the analysis of scattering patters obtained from oriented systems.



Path length dependent neutron diffraction peak shifts observed during residual strain measurements in U–8 wt% Mo castings

2017-05-16

This study reports an angular diffraction peak shift that scales linearly with the neutron beam path length traveled through a diffracting sample. This shift was observed in the context of mapping the residual stress state of a large U–8 wt% Mo casting, as well as during complementary measurements on a smaller casting of the same material. If uncorrected, this peak shift implies a non-physical level of residual stress. A hypothesis for the origin of this shift is presented, based upon non-ideal focusing of the neutron monochromator in combination with changes to the wavelength distribution reaching the detector due to factors such as attenuation. The magnitude of the shift is observed to vary linearly with the width of the diffraction peak reaching the detector. Consideration of this shift will be important for strain measurements requiring long path lengths through samples with significant attenuation. This effect can probably be reduced by selecting smaller voxel slit widths.



Crystallographic texture of straight-rolled α-uranium foils via neutron and X-ray diffraction

2017-05-25

The texture of recrystallized straight-rolled α-uranium foils, a component in prospective irradiation target designs for medical isotope production, has been measured by neutron diffraction, as well as X-ray diffraction using both Cu and Mo sources. Variations in the penetration depth of neutron and X-ray radiation allow for determination of both the bulk and surface textures. The bulk α-uranium foil texture is similar to the warm straight-rolled plate texture, with the addition of a notable splitting of the (001) poles along the transverse direction. The surface texture of the foils is similar to the bulk, with an additional (001) texture component that is oriented between the rolling and normal directions. Differences between the surface and bulk textures are expected to arise from shear forces during the rolling process and the influence that distinct strain histories have on subsequent texture evolution during recrystallization.



Instrumental resolution as a function of scattering angle and wavelength as exemplified for the POWGEN instrument

2017-05-25

The method of angular- and wavelength-dispersive (e.g. two-dimensional) Rietveld refinement is a new and emerging tool for the analysis of neutron diffraction data measured at time-of-flight instruments with large area detectors. Following the approach for one-dimensional refinements (using either scattering angle or time of flight), the first step at each beam time cycle is the calibration of the instrument including the determination of instrumental contributions to the peak shape variation to be expected for diffraction patterns measured by the users. The aim of this work is to provide the users with calibration files and – for the later Rietveld refinement of the measured data – with an instrumental resolution file (IRF). This article will elaborate on the necessary steps to generate such an IRF for the angular- and wavelength-dispersive case, exemplified for the POWGEN instrument. A dataset measured on a standard diamond sample is used to extract the profile function in the two-dimensional case. It is found that the variation of reflection width with 2θ and λ can be expressed by the standard equation used for evaluating the instrumental resolution, which yields a substantially more fundamental approach to the parameterization of the instrumental contribution to the peak shape. Geometrical considerations of the POWGEN instrument and sample effects lead to values for Δθ, Δt and ΔL that yield a very good match to the extracted FWHM values. In a final step the refinement results are compared with the one-dimensional, i.e. diffraction-focused, case.



CrystalWalk: crystal structures, step by step

2017-05-25

CrystalWalk is a crystal editor and visualization software designed for teaching materials science and engineering. Based on WebGL/HTML5, it provides an accessible and interactive platform to students and teachers by introducing a simplified crystallographic approach that creates crystal structures by combining a lattice with a motif without the use of its internal symmetry. CrystalWalk is the first software to use solely translational symmetry, aiming to introduce engineering students to the basic concepts of lattice and motif. Although very restrictive from the crystallographic point of view, CrystalWalk makes it simple for students to experiment, reproduce and visualize, in an interactive manner, most of the crystal structures that are commonly introduced in materials science and engineering curricula.



SLADS: a parallel code for direct simulations of scattering of large anisotropic dense nanoparticle systems

2017-04-13

SLADS (http://www.pims.ac.cn/Resources.html), a parallel code for direct simulations of X-ray scattering of large anisotropic dense nanoparticle systems of arbitrary species and atomic configurations, is presented. Particles can be of arbitrary shapes and dispersities, and interactions between particles are considered. Parallelization is achieved in real space for the sake of memory limitation. The system sizes attempted are up to one billion atoms, and particle concentrations in dense systems up to 0.36. Anisotropy is explored in terms of superlattices. One- and two-dimensional small-angle scattering or diffraction patterns are obtained. SLADS is validated self-consistently or against cases with analytical solutions.



Processing two-dimensional X-ray diffraction and small-angle scattering data in DAWN 2

2017-05-08

A software package for the calibration and processing of powder X-ray diffraction and small-angle X-ray scattering data is presented. It provides a multitude of data processing and visualization tools as well as a command-line scripting interface for on-the-fly processing and the incorporation of complex data treatment tasks. Customizable processing chains permit the execution of many data processing steps to convert a single image or a batch of raw two-dimensional data into meaningful data and one-dimensional diffractograms. The processed data files contain the full data provenance of each process applied to the data. The calibration routines can run automatically even for high energies and also for large detector tilt angles. Some of the functionalities are highlighted by specific use cases.



DxTools: processing large data files recorded with the Bruker D8 diffractometer

2017-05-16

Data processing is the daily reality for crystallographers, who often seek to automate this repetitive task. With modern commercial diffractometers allowing for more elaborate experiments to be performed, the use of commercial software is almost unavoidable for processing data, because these are often provided in a manufacturer-specific format. This is especially the case when the intensity is recorded as a function of more than one single scanning motor and/or when recording data with a one-dimensional detector. A simple, free and open-source alternative is here presented to process the type of diffraction data recorded with the Bruker D8 diffractometer. It allows handling of data files (in uxd and brml format) corresponding to reciprocal space maps (in the QxQz and QxQy planes), temperature-dependent scans, spatial scans, sin2ψ measurements and pole figures. The program is easy to use and can be extended to any file format. It can be downloaded from https://aboulle.github.io/DxTools/.



The ash heap of crystallography: restoring forgotten basic knowledge. Corrigendum

2017-04-27

One imprecise and one incomplete statement in the article by Nespolo [J. Appl. Cryst. (2015), 48, 1290–1298] are corrected.