Showing papers in "Journal of Applied Crystallography in 2017"

ATSAS 2.8: a comprehensive data analysis suite for small-angle scattering from macromolecular solutions

Abstract: ATSAS is a comprehensive software suite for the analysis of small-angle scattering data from dilute solutions of biological macromolecules or nanoparticles. It contains applications for primary data processing and assessment, ab initio bead modelling, and model validation, as well as methods for the analysis of flexibility and mixtures. In addition, approaches are supported that utilize information from X-ray crystallography, nuclear magnetic resonance spectroscopy or atomistic homology modelling to construct hybrid models based on the scattering data. This article summarizes the progress made during the 2.5–2.8 ATSAS release series and highlights the latest developments. These include AMBIMETER, an assessment of the reconstruction ambiguity of experimental data; DATCLASS, a multiclass shape classification based on experimental data; SASRES, for estimating the resolution of ab initio model reconstructions; CHROMIXS, a convenient interface to analyse in-line size exclusion chromatography data; SHANUM, to evaluate the useful angular range in measured data; SREFLEX, to refine available high-resolution models using normal mode analysis; SUPALM for a rapid superposition of low- and high-resolution models; and SASPy, the ATSAS plugin for interactive modelling in PyMOL. All these features and other improvements are included in the ATSAS release 2.8, freely available for academic users from https://www.embl-hamburg.de/biosaxs/software.html.

BioXTAS RAW: improvements to a free open-source program for small-angle X-ray scattering data reduction and analysis

Abstract: BioXTAS RAW is a graphical-user-interface-based free open-source Python program for reduction and analysis of small-angle X-ray solution scattering (SAXS) data. The software is designed for biological SAXS data and enables creation and plotting of one-dimensional scattering profiles from two-dimensional detector images, standard data operations such as averaging and subtraction and analysis of radius of gyration and molecular weight, and advanced analysis such as calculation of inverse Fourier transforms and envelopes. It also allows easy processing of inline size-exclusion chromatography coupled SAXS data and data deconvolution using the evolving factor analysis method. It provides an alternative to closed-source programs such as Primus and ScAtter for primary data analysis. Because it can calibrate, mask and integrate images it also provides an alternative to synchrotron beamline pipelines that scientists can install on their own computers and use both at home and at the beamline.

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

Abstract: 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.

More features, more tools, more CrysTBox

Abstract: A new release of the CrysTBox software is introduced. The original toolbox allows for an automated analysis of transmission electron microscope (TEM) images and for crystallographic visualization. The existing tools, which are capable of highly precise analyses of high-resolution TEM images, as well as spot, disc and ring diffraction patterns, are extended to include a tool for automatically measuring TEM sample thickness using convergent beam electron diffraction in a two-beam approximation. An implementation of geometric phase analysis is newly available, employing one of the existing tools to identify parameters and indices of crystallographic planes depicted in the input image and allowing easier and more accurate analysis. The crystallographic visualization capabilities are extended as well. Along with the simulated diffraction pattern and atomic structure, a stereographic projection and inverse pole figure tool is newly offered. A new tool able to visualize the atomic structure of two different phases and their interface is also introduced.

Double crystallographic groups and their representations on the Bilbao Crystallographic Server

Abstract: A new section of databases and programs devoted to double crystallographic groups (point and space groups) has been implemented in the Bilbao Crystallographic Server (http://www.cryst.ehu.es). The double crystallographic groups are required in the study of physical systems whose Hamiltonian includes spin-dependent terms. In the symmetry analysis of such systems, instead of the irreducible representations of the space groups, it is necessary to consider the single- and double-valued irreducible representations of the double space groups. The new section includes databases of symmetry operations (DGENPOS) and of irreducible representations of the double (point and space) groups (REPRESENTATIONS DPG and REPRESENTATIONS DSG). The tool DCOMPREL provides compatibility relations between the irreducible representations of double space groups at different k vectors of the Brillouin zone when there is a group–subgroup relation between the corresponding little groups. The program DSITESYM implements the so-called site-symmetry approach, which establishes symmetry relations between localized and extended crystal states, using representations of the double groups. As an application of this approach, the program BANDREP calculates the band representations and the elementary band representations induced from any Wyckoff position of any of the 230 double space groups, giving information about the properties of these bands. Recently, the results of BANDREP have been extensively applied in the description of and the search for topological insulators.

The modular small-angle X-ray scattering data correction sequence.

Abstract: Data correction is probably the least favourite activity amongst users experimenting with small-angle X-ray scattering: if it is not done sufficiently well, this may become evident only during the data analysis stage, necessitating the repetition of the data corrections from scratch. A recommended comprehensive sequence of elementary data correction steps is presented here to alleviate the difficulties associated with data correction, both in the laboratory and at the synchrotron. When applied in the proposed order to the raw signals, the resulting absolute scattering cross section will provide a high degree of accuracy for a very wide range of samples, with its values accompanied by uncertainty estimates. The method can be applied without modification to any pinhole-collimated instruments with photon-counting direct-detection area detectors.

Quantitative X-ray pair distribution function analysis of nanocrystalline calcium silicate hydrates: a contribution to the understanding of cement chemistry

Abstract: The structural evolution of nanocrystalline calcium silicate hydrate (C–S–H) as a function of its calcium to silicon (Ca/Si) ratio has been probed using qualitative and quantitative X-ray atomic pair distribution function analysis of synchrotron X-ray scattering data. Whatever the Ca/Si ratio, the C–S–H structure is similar to that of tobermorite. When the Ca/Si ratio increases from ∼0.6 to ∼1.2, Si wollastonite-like chains progressively depolymerize through preferential omission of Si bridging tetrahedra. When the Ca/Si ratio approaches ∼1.5, nanosheets of portlandite are detected in samples aged for 1 d, while microcrystalline portlandite is detected in samples aged for 1 year. High-resolution transmission electron microscopy imaging shows that the tobermorite-like structure is maintained to Ca/Si > 3.

Oscail, a program package for small-molecule single-crystal crystallography with crystal morphology prediction and molecular modelling

Abstract: Oscail is a program for small-molecule crystallography which includes crystal morphology prediction and an interface to molecular modelling. The Oscail graphical user interface can drive SHELX and Superflip for structure solution and SHELXL for structure refinement. The lattice analysis includes hydrogen bonding, halogen bonding and van der Waals contact stacking. Other facilities include interactive bar charts of space-group frequencies in the Cambridge Structural Database, powder diffraction pattern calculation and reduced cell cluster analysis of structures. The graphics output includes thermal ellipsoid plots and rendered OpenGL and Raster3D photorealism in stills and movies. The molecular modelling includes quantum calculations (MOPAC, extended Huckel and density functional theory) and TINKER molecular mechanics.

Nanoparticle size distribution quantification: results of a small-angle X-ray scattering inter-laboratory comparison

Abstract: This paper presents the first worldwide inter-laboratory comparison of small-angle X-ray scattering (SAXS) for nanoparticle sizing. The measurands in this comparison are the mean particle radius, the width of the size distribution and the particle concentration. The investigated sample consists of dispersed silver nanoparticles, surrounded by a stabilizing polymeric shell of poly(acrylic acid). The silver cores dominate the X-ray scattering pattern, leading to the determination of their radius size distribution using (i) the generalized indirect Fourier transformation method, (ii) classical model fitting using SASfit and (iii) a Monte Carlo fitting approach using McSAS. The application of these three methods to the collected data sets from the various laboratories produces consistent mean number- and volume-weighted core radii of Rn = 2.76 (6) nm and Rv = 3.20 (4) nm, respectively. The corresponding widths of the lognormal radius distribution of the particles were σn = 0.65 (1) nm and σv = 0.71 (1) nm. The particle concentration determined using this method was 3.0 (4) g l−1 or 4.2 (7) × 10−6 mol l−1. These results are affected slightly by the choice of data evaluation procedure, but not by the instruments: the participating laboratories at synchrotron SAXS beamlines, commercial and in-house-designed instruments were all able to provide highly consistent data. This demonstrates that SAXS is a suitable method for revealing particle size distributions in the sub-20 nm region (at minimum), out of reach for most other analytical methods.

X‐ray diffraction microscopy based on refractive optics

Abstract: A formalism is presented for dark-field X-ray microscopy using refractive optics. The new technique can produce three-dimensional maps of lattice orientation and axial strain within millimetre-sized sampling volumes and is particularly suited to in situ studies of materials at hard X-ray energies. An objective lens in the diffracted beam magnifies the image and acts as a very efficient filter in reciprocal space, enabling the imaging of individual domains of interest with a resolution of 100 nm. Analytical expressions for optical parameters such as numerical aperture, vignetting, and the resolution in both direct and reciprocal spaces are provided. It is shown that the resolution function in reciprocal space can be highly anisotropic and varies as a function of position in the field of view. Inserting a square aperture in front of the objective lens facilitates disjunct and space-filling sampling, which is key for three-dimensional reconstruction and analysis procedures based on the conservation of integrated intensity. A procedure for strain scanning is presented. Finally the formalism is validated experimentally at an X-ray energy of 17 keV.

NIST Standard Reference Material 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering

Abstract: The certification of a new standard reference material for small-angle scattering [NIST Standard Reference Material (SRM) 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering (SAXS)], based on glassy carbon, is presented. Creation of this SRM relies on the intrinsic primary calibration capabilities of the ultra-small-angle X-ray scattering technique. This article describes how the intensity calibration has been achieved and validated in the certified Q range, Q = 0.008–0.25 A−1, together with the purpose, use and availability of the SRM. The intensity calibration afforded by this robust and stable SRM should be applicable universally to all SAXS instruments that employ a transmission measurement geometry, working with a wide range of X-ray energies or wavelengths. The validation of the SRM SAXS intensity calibration using small-angle neutron scattering (SANS) is discussed, together with the prospects for including SANS in a future renewal certification.

Modelling of glass-like carbon structure and its experimental verification by neutron and X-ray diffraction

Abstract: Glass-like carbon is a well known carbon form that still poses many challenges for structural characterization owing to a very complex internal atomic organization. Recent research suggests that glassy carbon has a fullerene-related structure that evolves with the synthesis temperature. This article reports on direct evidence of curved planes in glassy carbons using neutron and X-ray diffraction measurements and their analysis in real space using the atomic pair distribution function formalism. Changes in the structure including the degree of curvature of the non-graphitizing glassy carbons as a function of the pyrolysis temperature in the range 800–2500°C (1073–2773 K) are studied using optimized models of the atomic structure. Averaged models of single coherent scattering domains as well as larger structural fragments consisting of thousands of atoms were relaxed using classical molecular dynamics. For such models the diffraction intensities and the pair distribution functions were computed. The compatibility of the computer-generated models was verified by comparison of the simulations with the experimental diffraction data in both reciprocal and real spaces. On the basis of features of the developed structural models for glass-like carbons, the origin of the properties such as high strength and hardness and low gas permeability can be better understood.

Joint small-angle X-ray and neutron scattering data analysis of asymmetric lipid vesicles

Abstract: Low- and high-resolution models describing the internal transbilayer structure of asymmetric lipid vesicles have been developed. These models can be used for the joint analysis of small-angle neutron and X-ray scattering data. The models describe the underlying scattering length density/electron density profiles either in terms of slabs or through the so-called scattering density profile, previously applied to symmetric lipid vesicles. Both models yield structural details of asymmetric membranes, such as the individual area per lipid, and the hydrocarbon thickness of the inner and outer bilayer leaflets. The scattering density profile model, however, comes at a cost of increased computational effort but results in greater structural resolution, showing a slightly lower packing of lipids in the outer bilayer leaflet of ∼120 nm diameter palmitoyl­oleoyl phosphatidyl­choline (POPC) vesicles, compared to the inner leaflet. Analysis of asymmetric dipalmitoyl phosphatidylcholine/POPC vesicles did not reveal evidence of transbilayer coupling between the inner and outer leaflets at 323 K, i.e. above the melting transition temperature of the two lipids.

Synchrotron Bragg diffraction imaging characterization of synthetic diamond crystals for optical and electronic power device applications

Abstract: Bragg diffraction imaging enables the quality of synthetic single-crystal diamond substrates and their overgrown, mostly doped, diamond layers to be characterized. This is very important for improving diamond-based devices produced for X-ray optics and power electronics applications. The usual first step for this characterization is white-beam X-ray diffraction topography, which is a simple and fast method to identify the extended defects (dislocations, growth sectors, boundaries, stacking faults, overall curvature etc.) within the crystal. This allows easy and quick comparison of the crystal quality of diamond plates available from various commercial suppliers. When needed, rocking curve imaging (RCI) is also employed, which is the quantitative counterpart of monochromatic Bragg diffraction imaging. RCI enables the local determination of both the effective misorientation, which results from lattice parameter variation and the local lattice tilt, and the local Bragg position. Maps derived from these parameters are used to measure the magnitude of the distortions associated with polishing damage and the depth of this damage within the volume of the crystal. For overgrown layers, these maps also reveal the distortion induced by the incorporation of impurities such as boron, or the lattice parameter variations associated with the presence of growth-incorporated nitrogen. These techniques are described, and their capabilities for studying the quality of diamond substrates and overgrown layers, and the surface damage caused by mechanical polishing, are illustrated by examples.

SUePDF: a program to obtain quantitative pair distribution functions from electron diffraction data

Abstract: SUePDF is a graphical user interface program written in MATLAB to achieve quantitative pair distribution functions (PDFs) from electron diffraction data. The program facilitates structural studies of amorphous materials and small nanoparticles using electron diffraction data from transmission electron microscopes. It is based on the physics of electron scattering as well as the total scattering methodology. A method of background modeling is introduced to treat the intensity tail of the direct beam, inelastic scattering and incoherent multiple scattering. Kinematical electron scattering intensity is scaled using the electron scattering factors. The PDFs obtained after Fourier transforms are normalized with respect to number density, nanoparticle form factor and the non-negativity of probability density. SUePDF is distributed as free software for academic users.

SAXS analysis of single- and multi-core iron oxide magnetic nanoparticles.

Abstract: This article reports on the characterization of four superparamagnetic iron oxide nanoparticles stabilized with dimercaptosuccinic acid, which are suitable candidates for reference materials for magnetic properties. Particles p1 and p2 are single-core particles, while p3 and p4 are multi-core particles. Small-angle X-ray scattering analysis reveals a lognormal type of size distribution for the iron oxide cores of the particles. Their mean radii are 6.9 nm (p1), 10.6 nm (p2), 5.5 nm (p3) and 4.1 nm (p4), with narrow relative distribution widths of 0.08, 0.13, 0.08 and 0.12. The cores are arranged as a clustered network in the form of dense mass fractals with a fractal dimension of 2.9 in the multi-core particles p3 and p4, but the cores are well separated from each other by a protecting organic shell. The radii of gyration of the mass fractals are 48 and 44 nm, and each network contains 117 and 186 primary particles, respectively. The radius distributions of the primary particle were confirmed with transmission electron microscopy. All particles contain purely maghemite, as shown by X-ray absorption fine structure spectroscopy.

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

Abstract: 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

Abstract: 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.

Scattering from surface fractals in terms of composing mass fractals

Abstract: It is argued that a finite iteration of any surface fractal can be composed of mass-fractal iterations of the same fractal dimension. Within this assertion, the scattering amplitude of a surface fractal is shown to be a sum of the amplitudes of the composing mass fractals. Various approximations for the scattering intensity of surface fractals are considered. It is shown that small-angle scattering (SAS) from a surface fractal can be explained in terms of a power-law distribution of sizes of objects composing the fractal (internal polydispersity), provided the distance between objects is much larger than their size for each composing mass fractal. The power-law decay of the scattering intensity I(q) ∝ q^{D_{\rm s}-6}, where 2 < Ds < 3 is the surface-fractal dimension of the system, is realized as a non-coherent sum of scattering amplitudes of three-dimensional objects composing the fractal and obeying a power-law distribution dN(r) ∝ r−τdr, with Ds = τ − 1. The distribution is continuous for random fractals and discrete for deterministic fractals. A model of the surface deterministic fractal is suggested, the surface Cantor-like fractal, which is a sum of three-dimensional Cantor dusts at various iterations, and its scattering properties are studied. The present analysis allows one to extract additional information from SAS intensity for dilute aggregates of single-scaled surface fractals, such as the fractal iteration number and the scaling factor.

Hierarchical clustering for multiple-crystal macromolecular crystallography experiments: the ccCluster program.

Abstract: This article describes ccCluster, a software providing an intuitive graphical user interface (GUI) and multiple functions to perform hierarchical cluster analysis on multiple crystallographic datasets. The program makes it easier for users to choose, in the case of multi-crystal data collection, those datasets that will be merged together to give good final statistics. It provides a simple GUI to analyse the dendrogram and various options for automated clustering and data merging.

Structure evolution of aluminosilicate sol and its structure-directing effect on the synthesis of NaY zeolite

Abstract: Understanding the growth behaviour of an aluminosilicate sol during ageing is necessary for the design of the sol and the synthesis of NaY zeolite. Herein, aluminosilicate sols with three different SiO2/Al2O3 ratios were prepared and aged for varying times at 293 K. The sol was then introduced as a structure-directing agent in the feedstock gel to generate NaY zeolite. The structure evolution of the sol species during the ageing process was studied by in situ small-angle X-ray scattering (SAXS) using synchrotron radiation. SAXS data, in combination with transmission electron microscopy images, Raman spectra and X-ray diffraction patterns, present a detailed description of the sol species, revealing an interplay between the fractal structure and reactivity to generate NaY zeolite. The SiO2/Al2O3 ratios in the sol play a critical role in the structure evolution of the aluminosilicate species during the ageing, particularly with respect to their size distributions and the fractal dimensions. The species with suitable size and compactness in the sol are found to be an active precursor for achieving a highly crystalline NaY zeolite. The sol with an SiO2/Al2O3 ratio of 20 possesses active species with a mass fractal dimension Dm of 2.0–2.6 after ageing, which leads to the formation of a well crystallized NaY zeolite. However, the high-silica sol-25, with an SiO2/Al2O3 ratio of 25, and alumina rich sol-10, with a ratio of 10, experience growth at either slow or fast rates. In these cases the active species have smaller Dm (1.1–1.9) or larger Dm (2.6–2.8), respectively, displaying low/poor activity to generate NaY zeolite. The mechanisms regulating the growth behaviour of the sols during ageing are proposed.

Extended model for the reconstruction of periodic multilayers from extreme ultraviolet and X-ray reflectivity data

Abstract: An extended model for the reconstruction of multilayer nanostructures from reflectometry data in the X-ray and extreme ultraviolet ranges is proposed. In contrast to the standard model approach, where the transitional region is defined in advance as a specific function, the transition layer is sought as a linear combination of several functions at once in the extended model. This allows one to describe a much wider class of multilayer structures with different dominant physical mechanisms for the formation of transition regions. The extended model occupies an intermediate position between the classical model approach and the so-called model-free methods. The efficiency of the described method is illustrated in detail in numerical simulations and in a real experiment on the annealing of a multilayer Mo/Be mirror.

Comparative study of structural phase transitions in bulk and powdered Fe–27Ga alloy by real-time neutron thermodiffractometry

Abstract: Phase transformations in an iron–gallium alloy have been analyzed by in situ real-time neutron diffraction in the temperature range from 293 to 1223 K. Two compositionally identical samples were studied: the first was in the as-cast bulk state, and the second was ground into a powdered state. In both samples, the same sequence of structural transitions was recorded on heating with a constant heating rate (D03 → A2 → L12 → D019 → A2), and the same structural state (D03 + L12) was recorded after slow cooling to room temperature. Owing to strong texture in the bulk sample, only diffraction patterns of the powdered sample were treated with the Rietveld method to determine the volume fractions of the coexisting phases, the coefficients of thermal expansion, and the thermal and static atomic disorder parameters. The occupancy of Ga positions and the ordered iron magnetic moment were refined at selected temperatures. The level of microstrain in the crystallites in the initial as-quenched state is small, but it sharply increases in the course of phase transitions when the alloy is heated. The microstrains are high and strongly anisotropic after slow cooling. Generally, phase transformations occur similarly in the powdered and bulk samples, but with a noticeable difference in details. The fulfilled analysis of the bulk and powdered samples allowed the real possibilities of the quantitative neutron diffraction analyses of phase transitions in ferromagnetic ordered alloys to be assessed.

FELIX: an algorithm for indexing multiple crystallites in X-ray free-electron laser snapshot diffraction images.

Abstract: A novel algorithm for indexing multiple crystals in snapshot X-ray diffraction images, especially suited for serial crystallography data, is presented. The algorithm, FELIX, utilizes a generalized parametrization of the Rodrigues–Frank space, in which all crystal systems can be represented without singularities. The new algorithm is shown to be capable of indexing more than ten crystals per image in simulations of cubic, tetragonal and monoclinic crystal diffraction patterns. It is also used to index an experimental serial crystallography dataset from lysozyme microcrystals. The increased number of indexed crystals is shown to result in a better signal-to-noise ratio, and fewer images are needed to achieve the same data quality as when indexing one crystal per image. The relative orientations between the multiple crystals indexed in an image show a slight tendency of the lysozme microcrystals to adhere on (\overline 110) facets.

Reconstructing detailed line profiles of lamellar gratings from GISAXS patterns with a Maxwell solver

Abstract: Laterally periodic nanostructures have been investigated with grazing-incidence small-angle X-ray scattering (GISAXS) by using the diffraction patterns to reconstruct the surface shape. To model visible light scattering, rigorous calculations of the near and far field by numerical solution of Maxwell's equations with a finite-element method are well established. The application of this technique to X-rays is still challenging, owing to the discrepancy between the incident wavelength and the finite-element size. This drawback vanishes for GISAXS because of the small angles of incidence, the conical scattering geometry and the periodicity of the surface structures, which allows a rigorous computation of the diffraction efficiencies with sufficient numerical precision. To develop metrology tools based on GISAXS, lamellar gratings with line widths down to 55 nm were produced by state-of-the-art electron-beam lithography and then etched into silicon. The high surface sensitivity of GISAXS in conjunction with a Maxwell solver allows the detailed reconstruction of the grating line shape for thick non-homogeneous substrates as well. The reconstructed geometric line-shape models are statistically validated by applying a Markov chain Monte Carlo sampling technique which reveals that GISAXS is able to reconstruct critical parameters like the widths of the lines with sub-nanometre uncertainty.

Precision and accuracy of stress measurement with a portable X-ray machine using an area detector

Abstract: The use of portable X-ray stress analyzers, which utilize an area detector along with the newly adopted `cosα' or full-ring fitting method, has recently attracted increasing interest. In laboratory conditions, these measurements are fast, convenient and precise because they employ a single-exposure technique that does not require sample rotation. In addition, the effects of grain size and orientation can be evaluated from the Debye ring recorded on the area detector prior to data analysis. The accuracy of the measured stress, however, has been questioned because in most cases just a single reflection is analyzed and the sample-to-detector distances are relatively short. This article presents a comprehensive analysis of the uncertainty associated with a state-of-the-art commercial portable X-ray device. Annealed ferrite reference powders were used to quantify the instrument precision, and the accuracy of the stress measurement was tested by in situ tensile loading on 1018 carbon steel and 6061 aluminium alloy bar samples. The results show that the precision and accuracy are sensitive to the instrument (or sample) tilt angle (ψ0) as well as to the selected hkl reflection of the sample. The instrument, sample and data analysis methods all affect the overall uncertainty, and each contribution is described for this specific portable X-ray system. Finally, on the basis of the conclusions reached, desirable measurement/analysis protocols for accurate stress assessments are also presented.

Quantification of supplementary cementitious content in blended Portland cement using an iterative Rietveld–PONKCS technique

Abstract: An iterative Rietveld–PONKCS (partial or no known crystal structure) technique has been developed for precise and accurate determination of the weight percentages of predominantly amorphous supplementary cementitious materials (SCMs) contained in Portland cement–SCM blends. This technique involves the iterative refinement of the SCM amorphous phase (SCMAP) content, with the separation of the refinement of the SCMAP shape parameters from background refinement. The technique also includes an internal and external standard refinement of both the calibration SCM and the cement–SCM blend. This approach enables the separation of the contributions of the SCMs and the cement to the amorphous content of the cement–SCM blend. The technique has been successfully applied to binary systems of cement–slag and cement–fly ash, and ternary blends of cement–fly ash–slag, over a wide range of cement replacement levels. In the ternary systems, the proposed technique was successfully able to separate the individual amorphous contributions of slag and fly ash to the total amorphous content of the system. The approach was also implemented on a pair of commercially available binary blended cements containing 30% slag and 30% fly ash, respectively.

New synchrotron powder diffraction facility for long-duration experiments

Abstract: A new synchrotron X-ray powder diffraction instrument has been built and commissioned for long-duration experiments on beamline I11 at Diamond Light Source. The concept is unique, with design features to house multiple experiments running in parallel, in particular with specific stages for sample environments to study slow kinetic systems or processes. The instrument benefits from a high-brightness X-ray beam and a large area detector. Diffraction data from the commissioning work have shown that the objectives and criteria are met. Supported by two case studies, the results from months of measurements have demonstrated the viability of this large-scale instrument, which is the world's first dedicated facility for long-term studies (weeks to years) using synchrotron radiation.

Debye–Waller coefficient of heavily deformed nanocrystalline iron

Abstract: 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.

An insight into the synthesis, crystal structure, geometrical modelling of crystal morphology, Hirshfeld surface analysis and characterization of N-(4-methylbenzyl)benzamide single crystals

Abstract: A versatile approach for the synthesis of N-(4-methyl­benzyl)­benzamide, C15H15NO, using CuI as catalyst has been reported. Single crystals of the synthesized compound were grown using the slow evaporation solution technique. The crystal structure of the N-(4-methyl­benzyl)­benzamide crystals has been determined by single-crystal X-ray diffraction. The compound crystallizes in an orthorhombic lattice, noncentrosymmetric space group Pna21. The crystal structure is stabilized by intermolecular N—H⋯O hydrogen bonds and weak C—H⋯π interactions to form layers parallel to the a axis. A user-friendly approach based on centre of mass propagation vector theory was used to predict the crystal morphology. The framework developed here utilizes the concept of intermolecular bond strength to discern the crystal morphology. Fourier transform IR, NMR and high-resolution mass spectrometry analytical techniques were used for the identification of functional groups and confirmation of the structure of the title compound. All of the intermolecular interactions present in the crystal structure, including the C—H⋯π, C—H⋯O and N—H⋯O interactions, were investigated and confirmed by molecular Hirshfeld surface analysis. From linear optical spectroscopy, the transmittance, optical band gap and UV cutoff wavelength were determined. The photoluminescence emission spectrum was recorded for a grown crystal. Dielectric measurements were performed at room temperature for various frequencies. The mechanical strength of the (001) plane of the title compound was measured using the Vickers micro-hardness technique. A piezo-coefficient of 15 pC N−1 was found along the (001) plane of the title crystals. The thermal stability and melting point were also investigated. In addition, density functional theory simulations were used to calculate the optimized molecular geometry and the UV–vis spectrum, and to determine the highest occupied molecular orbital/lowest unoccupied molecular orbital energy gap. The results show that N-(4-methyl­benzyl)­benzamide is a potential candidate for multifunctional optical and piezoelectric crystals.