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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: 2017-02-17


Energy-resolved small-angle neutron scattering from steel


Recent progress of pulsed neutron sources has enabled energy-resolved analysis of neutron attenuation spectra, which include information on neutron scattering. In this study, a new analysis technique for small-angle neutron scattering (SANS) is demonstrated. A clear difference is observed in the neutron attenuation spectra between steels with different nanostructures; this difference can be understood as arising from attenuation due to SANS. The neutron attenuation spectra calculated from the corresponding SANS profiles agree well with the experimentally observed attenuation spectra. This result indicates that measurement of neutron attenuation spectra may enable the development of a novel experimental technique, i.e. energy-resolved SANS.

Thermal expansion of deuterated monoclinic natrojarosite; a combined neutron–synchrotron powder diffraction study


A combination of time-of-flight neutron diffraction and synchrotron X-ray powder diffraction has been used to investigate the thermal expansion of a synthetic deuterated natrojarosite from 80 to 440 K under ambient-pressure conditions. The variation in unit-cell volume for monoclinic jarosite over this temperature range can be well represented by an Einstein expression of the form V = 515.308 (5) + 8.5 (4)/{exp[319 (4)/T] − 1}. Analysis of the behaviour of the polyhedra and hydrogen-bond network suggests that the strength of the hydrogen bonds connected to the sulfate tetrahedra is instrumental in determining the expansion of the structure, which manifests primarily in the c-axis direction.

Orientation relationships between α-zirconium and δ-hydride within a hydride blister


Both the expected and an additional orientation relationship between α-Zr and δ-hydride in blistered zirconium alloys are explored through the reconstruction of the parent α-Zr phase from electron backscatter diffraction maps of δ-hydride. Parent and child variant relationships for the transformation are presented with the aim of reconstruction of the parent α-Zr grain structure and texture from orientation maps of the δ-hydride at varying distances from the blister centre in a recrystallized Zircaloy-4 sample. Up to 13% of the δ-hydride is found to be variants of the additional orientation relationship, the fraction of which decreases with increasing distance from the blister centre. Texture reconstructions by other experimental methods are accordingly suggested to incorporate the additional orientation relationship.

On the use of two-time correlation functions for X-ray photon correlation spectroscopy data analysis


Multi-time correlation functions are especially well suited to study non-equilibrium processes. In particular, two-time correlation functions are widely used in X-ray photon correlation experiments on systems out of equilibrium. One-time correlations are often extracted from two-time correlation functions at different sample ages. However, this way of analysing two-time correlation functions is not unique. Here, two methods to analyse two-time correlation functions are scrutinized, and three illustrative examples are used to discuss the implications for the evaluation of the correlation times and functional shape of the correlations.

Twin domain imaging in topological insulator Bi2Te3 and Bi2Se3 epitaxial thin films by scanning X-ray nanobeam microscopy and electron backscatter diffraction


The twin distribution in topological insulators Bi2Te3 and Bi2Se3 was imaged by electron backscatter diffraction (EBSD) and scanning X-ray diffraction microscopy (SXRM). The crystal orientation at the surface, determined by EBSD, is correlated with the surface topography, which shows triangular pyramidal features with edges oriented in two different orientations rotated in the surface plane by 60°. The bulk crystal orientation is mapped out using SXRM by measuring the diffracted X-ray intensity of an asymmetric Bragg peak using a nano-focused X-ray beam scanned over the sample. By comparing bulk- and surface-sensitive measurements of the same area, buried twin domains not visible on the surface are identified. The lateral twin domain size is found to increase with the film thickness.

Crystallographic and optical study of PbHfO3 crystals


The symmetry of the intermediate high-temperature phase of PbHfO3 has been determined unambiguously to be orthorhombic using a combination of high-resolution X-ray diffraction and birefringence imaging microscopy measurements of crystal plates. While lattice parameter measurements as a function of temperature in the intermediate phase are consistent with either orthorhombic or tetragonal symmetry, domain orientations observed in birefringence imaging microscopy measurements utilizing the Metripol system are only consistent with orthorhombic symmetry with the unit cell in the rhombic orientation of the pseudocubic unit cell.

Debye–Waller coefficient of heavily deformed nanocrystalline iron


Synchrotron radiation X-ray diffraction (XRD) patterns from an extensively ball-milled iron alloy powder were collected at 100, 200 and 300 K. The results were analysed together with those using extended X-ray absorption fine structure, measured on the same sample at liquid nitrogen temperature (77 K) and at room temperature (300 K), to assess the contribution of static disorder to the Debye–Waller coefficient (Biso). Both techniques give an increase of ∼20% with respect to bulk reference iron, a noticeably smaller difference than reported by most of the literature for similar systems. Besides good quality XRD patterns, proper consideration of the temperature diffuse scattering seems to be the key to accurate values of the Debye–Waller coefficient. Molecular dynamics simulations of nanocrystalline iron aggregates, mapped on the evidence provided by XRD in terms of domain size distribution, shed light on the origin of the observed Biso increase. The main contribution to the static disorder is given by the grain boundary, while line and point defects have a much smaller effect.

Scanning X-ray nanodiffraction from ferroelectric domains in strained K0.75Na0.25NbO3 epitaxial films grown on (110) TbScO3


Scanning X-ray nanodiffraction on a highly periodic ferroelectric domain pattern of a strained K0.75Na0.25NbO3 epitaxial layer has been performed by using a focused X-ray beam of about 100 nm probe size. A 90°-rotated domain variant which is aligned along [1{\overline 1}2]TSO has been found in addition to the predominant domain variant where the domains are aligned along the [{\overline 1}12]TSO direction of the underlying (110) TbScO3 (TSO) orthorhombic substrate. Owing to the larger elastic strain energy density, the 90°-rotated domains appear with significantly reduced probability. Furthermore, the 90°-rotated variant shows a larger vertical lattice spacing than the 0°-rotated domain variant. Calculations based on linear elasticity theory substantiate that this difference is caused by the elastic anisotropy of the K0.75Na0.25NbO3 epitaxial layer.

Ind_X: program for indexing single-crystal diffraction patterns


Indexing is an essential step in analysis of diffraction patterns. Diffraction of monochromatic radiation by a single crystal provides approximate positions of some nodes of the reciprocal lattice of the crystal, and the indexing problem lies in determining a lattice matching these positions. Ind_X is a program for indexing diffraction data given in the form of several approximate reciprocal lattice nodes. The applied method relies on testing potential volumes of the primitive cell of the reciprocal lattice. A subset of reciprocal lattice vectors supporting a given test volume is used to obtain tentative lattice bases. These are bases of low-index superlattices of lattices based on triplets of supporting vectors. The Ind_X solution of the indexing problem consists of a list of best bases. The method turns out to be quite robust to data inaccuracies and spurious reflections. The program is relatively versatile, easily operated and freely accessible.