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The pyRS (Python residual stress) analysis software was designed to address the data reduction and analysis needs of the High Intensity Diffractometer for Residual Stress Analysis (HIDRA) user community. pyRS implements frameworks for the calibration and reduction of measured 2D data into intensity versus scattering vector magnitude and subsequent single-peak-fitting analysis to facilitate texture and residual strain/stress analysis. pyRS components are accessible as standalone user interfaces for peak-fitting and stress/strain analysis or as Python scripts. The scripting interface facilitates automated data reduction and peak-fitting analysis using an autoreduction protocol. Details of the implemented functionality are discussed.

A user-friendly Python-based program has been developed to analyze diffuse scattering from single crystals with the reverse Monte Carlo method. The approach allows for refinement of correlated disorder from atomistic supercells with magnetic or structural (occupational and/or displacive) disorder., A user-friendly program has been developed to analyze diffuse scattering from single crystals with the reverse Monte Carlo method. The approach allows for refinement of correlated disorder from atomistic supercells with magnetic or structural (occupational and/or displacive) disorder. The program is written in Python and optimized for performance and efficiency. Refinements of two user cases obtained with legacy neutron-scattering data demonstrate the effectiveness of the approach and the developed program. It is shown with bixbyite, a naturally occurring magnetic mineral, that the calculated three-dimensional spin-pair correlations are resolved with finer real-space resolution compared with the pair distribution function calculated directly from the reciprocal-space pattern. With the triangular lattice Ba3Co2O6(CO3)0.7, refinements of occupational and displacive disorder are combined to extract the one-dimensional intra-chain correlations of carbonate molecules that move toward neighboring vacant sites to accommodate strain induced by electrostatic interactions. The program is packaged with a graphical user interface and extensible to serve the needs of single-crystal diffractometer instruments that collect diffuse-scattering data.

Laboratory X-ray diffractometers play a crucial role in X-ray crystallography and materials science. Such instruments still vastly outnumber synchrotron facilities and are responsible for most of the X-ray characterization of materials around the world. The efforts to enhance the design and performance of in-house X-ray diffraction instruments benefit a broad research community. Here, the realization of a custom-built multipurpose four-circle diffractometer in the laboratory for X-ray crystallography of functional materials at Tel Aviv University, Israel, is reported. The instrument is equipped with a microfocus Cu-based X-ray source, collimating X-ray optics, four-bounce monochromator, four-circle goniometer, large (PILATUS3 R 1M) pixel area detector, analyser crystal and scintillating counter. It is suitable for a broad range of tasks in X-ray crystallography/structure analysis and materials science. All the relevant X-ray beam parameters (total flux, flux density, beam divergence, monochromaticity) are reported and several applications such as determination of the crystal orientation matrix and high-resolution reciprocal-space mapping are demonstrated. The diffractometer is suitable for measuring X-ray diffraction in situ under an external electric field, as demonstrated by the measurement of electric-field-dependent rocking curves of a quartz single crystal. The diffractometer can be used as an independent research instrument, but also as a training platform and for preparation for synchrotron experiments.

Strategies for efficient and reliable texture measurements have been explored using the Nanoscale Ordered Materials Diffractometer (NOMAD) at the Spallation Neutron Source located at Oak Ridge National Laboratory (ORNL). To test these strategies, the texture of an Al alloy was also investigated using another neutron diffraction instrument, a constant-wavelength neutron diffractometer (NRSF2) located at the High Flux Isotope Reactor, also at ORNL. Reasonable agreement was found across the two experimental methods, but differences in overall texture strength and the symmetry of some components were noted, depending on the data reduction and analysis method selected. On the basis of these results, potential improvements are identified which would enhance the texture measurement capability on NOMAD.

A new sample stage for characterizing radioactive materials by X-ray powder diffraction was developed at the ATALANTE facility (CEA Marcoule, France) using a conventional (non-nuclearized) Bruker D8 goniometer mounted in Bragg–Brentano geometry. The setup consists of a removable, fully hermetic sample stage, with a 200 µm-thick beryllium window, that can be plugged onto a glove-box, allowing the sample to be introduced in an hermetic medium that also encapsulates the glove-box atmosphere throughout the analysis process. The whole setup is thus hermetically unplugged from the glove-box and positioned on the centre of the goniometer. No preliminary decontamination and/or decontainment of the sample is necessary. The device was developed to avoid an expensive and time-consuming nuclearization of the diffractometer while also keeping it easily accessible for maintenance. Ultimately, keeping the diffractometer out of a glove-box also limits the volume of the final nuclear wastes, and thus the removable sample stage is the only `active' part. X-ray diffraction results of two NIST standards LaB6 and α-Al2O3 as well as five actinide dioxides ThO2, UO2, NpO2, PuO2 and AmO2 are presented to show the efficiency of the setup.

This work demonstrates a sample environment suitable for studying solid–gas interactions by temperature control through thermal contact with a sample in a glass capillary, for temperature and pressure conditions of 0–100 bar (1 bar = 100 kPa) and −30 to 200°C., A sample cell for powder X-ray diffraction studies with in situ applied pressure and control of temperature is demonstrated. The cell is based on a previously reported design and consists of a glass or quartz capillary glued into a Swagelok weld gland; this configuration can hold up to 100 bar (1 bar = 100 kPa). The cell is placed in contact with a copper plate for control of temperature between −30 and 200°C. This is achieved by Peltier elements, heat cartridges and a refrigerated circulating bath. This work mainly focuses on the temperature control system. Commissioning tests were performed in a custom-made small/wide-angle X-ray diffractometer at the Norwegian University of Science and Technology. The system is easily portable to synchrotron facilities.

A sapphire single-crystal gas-pressure cell without external support allowing unobstructed optical access by neutrons has been developed and optimized for elasticin situneutron powder diffraction using hydrogen (deuterium) gas at the high-intensity two-axis diffractometer D20 at the Institut Laue-Langevin (Grenoble, France). Given a proper orientation of the single-crystal sample holder with respect to the detector, parasitic reflections from the sample holder can be avoided and the background can be kept low. Hydrogen (deuterium) gas pressures of up to 16.0 MPa at 298 K and 8.0 MPa at 655 K were tested successfully for a wall thickness of 3 mm. Heating was achieved by a two-sided laser heating system. The typical time resolution ofin situinvestigations of the reaction pathway of hydrogen (deuterium) uptake or release is on the order of 1 min. Detailed descriptions of all parts of the sapphire single-crystal gas-pressure cell are given, including materials information, technical drawings and instructions for use.

A feasibility study is carried out of an autoclave chamber for in situ X-ray diffraction experiments under hydrothermal conditions. Quartz dissolution and tobermorite formation are monitored on conventional laboratory X-ray diffractometers., This note describes an autoclave chamber developed and constructed by Anton Paar and its application for in situ experiments under hydrothermal conditions. Reactions of crystalline phases can be studied by successive in situ measurements on a conventional laboratory X-ray diffractometer with Bragg–Brentano geometry at temperatures

A simple statistical analysis which yields the precision, resolution, accuracy and trueness of diffraction-based lattice strain measurements is discussed. The procedure consists of measuring the thermal expansion induced in each component of an ideal non-reacting two-component crystalline powder sample in situ. One component, with a high coefficient of thermal expansion (CTE), serves as an internal thermometer. The quantities of interest are obtained by determining the smallest statistically significant thermal lattice strain which can be detected through diffraction analysis in the second, low-CTE, component in response to controlled temperature changes. This procedure also provides a robust check of the alignment of the diffraction system and is able to reveal the presence of systematic errors. The application of this technique to a time-of-flight engineering diffractometer/strain scanner is presented.

Herein, the successful use of a focused ion beam/scanning electron microscope to prepare microsamples of radioactive single crystals for X-ray diffraction analysis is reported. This technique was used to extract and analyze crystalline Pu-containing particles as small as 28 µm3from Hanford soil taken from the 216-Z-9 waste crib, which were then crystallographically characterized using single-crystal X-ray diffraction to confirm the cubic structure of PuO2. As a systematic proof of concept, the technique was first tested using UO2crystals milled into cubic shapes with approximate volumes of 4620, 1331, 125, 8 and 1 µm3, in order to empirically determine the crystal size limits for characterization by a laboratory-based diffractometer with a sealed tube Mo or Ag anode X-ray source and a charge-coupled device detector.

The IBARAKI biological crystal diffractometer (iBIX) was used in single-crystal time-of-flight neutron diffraction experiments on manganese catalase from Thermus thermophilus. The unit-cell dimensions were 133 × 133 × 133 Å, which is close to the designed maximum limitation of iBIX (135 × 135 × 135 Å). The optimum integration box sizes were set and the degree of integration box overlap was calculated for each Laue spot. Using the overlap ratio as the criterion, the selection of the diffraction intensity data was performed to give a minimum R p.i.m.. Subsequently, diffraction intensity data from Laue spots with overlap ratios ≤0.1 were selected and a complete reflection data set with d min = 2.35 Å was obtained. Joint X-ray and neutron structure refinements were also successfully performed. It was difficult to determine the structures and protonation states of all the oxygen atoms in the manganese cluster owing to the disordered structure. No hydrogen atom was observed on the ordered μ-bridging oxygen atom O1003. Instead, this oxygen atom probably forms a hydrogen bond with Thr39. In addition, the refinements clearly showed the protonation states of the amino acid residues and hydrogen bonds, as observed in Tyr192, Glu167 and Glu280. This first neutron crystal structure of manganese catalase shows that iBIX can provide acceptable diffraction data for neutron single-crystal analyses of at least 2.4 Å resolution within the original targeted unit-cell dimensions of 135 × 135 × 135 Å.

The high-resolution powder diffraction beamline at ESRF (ID22), built with a dual-undulator source on the 6 GeV storage ring, combines a wide continuous range of incident energy (6–80 keV) with high brightness, offering the possibility to carry out high-flux high-resolution powder diffraction measurements. In routine operation, a bank of nine scintillation detectors is scanned vertically to measure the diffracted intensity versus 2θ, each detector being preceded by an Si 111 analyser crystal. Although the current detector system has operated successfully for the past 20 years, recent developments in detector technology could be exploited to improve the overall performance. With this in mind, as a test, a two-dimensional Pilatus3 X CdTe 300 K-W pixel detector has been mounted on the arm of the diffractometer, replacing the nine scintillator detectors. At each nominal 2θ value, a two-dimensional image is recorded showing nine distinct regions corresponding to the diffraction signals passing via each of the analyser crystals. This arrangement offers new flexibility in terms of data handling and processing, with the possibility to optimize both peak shape and statistics, to remove parasitic effects, and to gain spatial resolution information. Combining the high efficiency of a hybrid photon-counting area detector with the high angular resolution given by analyser crystals is an effective approach to improving the overall performance of high-resolution powder diffraction.

EwaldSphere is a Microsoft Windows computer program that superimposes the Ewald sphere construction onto a small-molecule single-crystal X-ray diffractometer. The main objective of the software is to facilitate teaching of the Ewald sphere construction by depicting our classical description of the X-ray diffraction process as a three-dimensional model that can be explored interactively. Several features of the program are also useful for introducing students to the operation of a diffractometer. EwaldSphere creates a virtual reciprocal lattice based on user-defined unit-cell parameters. The Ewald sphere construction is then rendered visible, and the user can explore the effects of changing various diffractometer parameters (e.g. X-ray wavelength and intensity, goniometer angles, and detector distance) on the resulting diffraction pattern as captured by a virtual area detector. Additional digital resources are provided, including a simple but comprehensive program manual, a PowerPoint presentation that introduces the essential concepts, and an Excel file to facilitate calculation of lattice dhk spacings (required for the presentation). The program and accompanying resources are provided free of charge, and there are no restrictions on their use.

A procedure for a fast X-ray-diffraction-based crystal size distribution analysis, named FXD-CSD, is presented. The method enables the user, with minimal sample preparation, to determine the crystal size distribution (CSD) of crystalline powders or polycrystalline materials, derivedviaan intensity scaling procedure from the diffraction intensities of single Bragg spots measured in spotty diffraction patterns with a two-dimensional detector. The method can be implemented on any single-crystal laboratory diffractometer and any synchrotron-based instrument with a fast-readout two-dimensional detector and a precise sample scanning axis. The intensity scaling is achievedviathe measurement of areferencesample with known CSD under identical conditions; the only other prerequisite is that the structure (factors) of bothsampleandreferencematerial must be known. The data analysis is done with a software package written in Python. A detailed account is given of each step of the procedure, including the measurement strategy and the demands on the spottiness of the diffraction rings, the data reduction and the intensity corrections needed, and the data evaluation and the requirements for the reference material. Using commercial laboratory X-ray equipment, several corundum crystal size fractions with precisely known CSD were measured and analysed to verify the accuracy and precision of the FXD-CSD method; a comparison of known and deduced CSDs shows good agreement both in mean size and in the shape of the size distribution. For the used material and diffractometer setup, the crystal size application range is one to several tens of micrometres; this range is highly material and X-ray source dependent and can easily be extended on synchrotron sources to cover the range from below 0.5 µm to over 100 µm. FXD-CSD has the potential to become a generally applicable method for CSD determination in the field of materials science and pharmaceutics, including development and quality management, as well as in various areas of fundamental research in physics, chemistry, chemical engineering, crystallography, the geological sciences and bio-crystallization. It can be used also underin situconditions for studying crystal coarsening phenomena, and delivers precise and accurate CSDs, permitting experimental tests of various theories developed to predict their evolution.

Results of measurements of independent piezoelectric moduli d 11 and d 14 in Ca3NbGa3Si2O14, La3Ga5.5Ta0.5O14 and La3Ga5SiO14, promising single crystals of the calcium gallogermanate structural type, are presented. The moduli were measured with a triple-axis X-ray diffractometer under an external electric field which causes changes in the interplanar distances due to the reverse piezoelectric effect. The results of the X-ray diffractometry measurements agree fairly well (within less than 10%) with the results obtained by different methods.

The division of neutron detector panel regions has improved the precision of complex texture evaluation and appropriate sample rotation enhances the texture reliability in a limited neutron beam time. The TAKUMI instrument has achieved satisfactory texture precision for a limestone standard sample. The compressive rolling direction–transverse direction in-plane stress field was quantitatively measured in martensite layers of a martensite–austenite multilayered steel, and this stress field was found to originate from the martensite transformation strain and the linear contraction misfit between austenite layers and newly transformed martensite layers., Neutron diffraction texture measurements provide bulk averaged textures with excellent grain orientation statistics, even for large-grained materials, owing to the probed volume being of the order of 1 cm3. Furthermore, crystallographic parameters and other valuable microstructure information such as phase fraction, coherent crystallite size, root-mean-square microstrain, macroscopic or intergranular strain and stress, etc. can be derived from neutron diffractograms. A procedure for combined high stereographic resolution texture and residual stress evaluation was established on the pulsed-neutron-source-based engineering materials diffractometer TAKUMI at the Materials and Life Science Experimental Facility of the Japan Proton Accelerator Research Center, through division of the neutron detector panel regions. Pole figure evaluation of a limestone standard sample with a well known texture suggested that the precision obtained for texture measurement is comparable to that of the established neutron beamlines utilized for texture measurement, such as the HIPPO diffractometer at the Los Alamos Neutron Science Center (New Mexico, USA) and the D20 angle-dispersive neutron diffractometer at the Institut Laue–Langevin (Grenoble, France). A high-strength martensite–austenite multilayered steel was employed for further verification of the reliability of simultaneous Rietveld analysis of multiphase textures and macro stress tensors. By using a texture-weighted geometric mean micromechanical (BulkPathGEO) model, a macro stress tensor analysis with a plane stress assumption showed a rolling direction–transverse direction (RD–TD) in-plane compressive stress (about −330 MPa) in the martensite layers and an RD–TD in-plane tensile stress (about 320 MPa) in the austenite layers. The phase stress partitioning was ascribed mainly to the additive effect of the volume expansion during martensite transformation and the linear contraction misfit between austenite layers and newly transformed martensite layers during the water quenching process.

The Spallation Neutron Source at Oak Ridge National Laboratory, USA, ushered in a new era of neutron scattering experiments through the use of event-based data. Tagging each neutron event allows pump–probe experiments, measurements with a parameter asynchronous to the source, measurements with continuously varying parameters and novel ways of testing instrument components. This contribution will focus on a few examples. A pulsed magnet has been used to study diffraction under extreme fields. Continuous ramping of temperature is becoming standard on the POWGEN diffractometer. Battery degradation and phase transformations under heat and stress are often studied on the VULCAN diffractometer. Supercooled Al2O3 was studied on NOMAD. A study of a metallic glass through its glass transition was performed on the ARCS spectrometer, and the effect of source variation on chopper stability was studied for the SEQUOIA spectrometer. Besides a summary of these examples, an overview is provided of the hardware and software advances to enable these and many other event-based measurements.

This article reports the development and characterization of a laboratory-based high-resolution X-ray powder diffractometer equipped with a 5.5 T magnet and closed-cycle helium cryostat that is primarily designed for the investigation of magneto-structural phase transitions. Unique features of the diffractometer include the position-sensitive detector, allowing the collection of an entire diffraction pattern at once, and the high energy resolution with Mo Kα1radiation. The ability to utilize a lower energy resolution but higher photon flux by switching to an X-ray mirror monochromator makes it a versatile setup for a variety of compounds. In this contribution, details of the design and performance of the instrument are presented along with its specifications.

The polarized single-crystal diffractometer POLI is the first neutron scattering instrument routinely using 3He spin filters both to produce and to analyse neutron polarization. The instrument, with a non-magnetic goniometer, was designed to perform two types of polarized neutron diffraction experiment: spherical neutron polarimetry, also known as full three-dimensional polarization analysis in zero magnetic field, and classical polarized neutron diffraction, also called the flipping-ratio (FR) method, in high applied magnetic fields. Reported here is the implementation of the FR setup for short-wavelength neutrons on POLI using a new high-T c superconducting magnet with a maximal field of 2.2 T. The complete setup consists of a 3He polarizer, a nutator, a Mezei-type flipper, guide fields and dedicated pole pieces, together with the magnet. Each component, as well as the whole setup, was numerically simulated, optimized, built and finally successfully tested under real experimental conditions on POLI. The measured polarized neutron spin transport efficiency is about 99% at different wavelengths, e.g. as short as 0.7 Å, and up to the maximal available field of the magnet. No further depolarization of the 3He cells due to stray fields of the magnet occurs. The additional use of the available 3He analyser allows uniaxial polarization analysis experiments in fields up to 1.2 T. The results of the first experiment on the field-dependent distribution of the trigonal antiferromagnetic domains in haematite (α-Fe2O3) are presented and compared with the literature data.

The double-crystal ultra-small-angle neutron scattering (USANS) diffractometer KOOKABURRA at ANSTO was made available for user experiments in 2014. KOOKABURRA allows the characterization of microstructures covering length scales in the range of 0.1–10 µm. Use of the first- and second-order reflections coming off a doubly curved highly oriented mosaic pyrolytic graphite premonochromator at a fixed Bragg angle, in conjunction with two interchangeable pairs of Si(111) and Si(311) quintuple-reflection channel-cut crystals, permits operation of the instrument at two individual wavelengths, 4.74 and 2.37 Å. This unique feature among reactor-based USANS instruments allows optimal accommodation of a broad range of samples, both weakly and strongly scattering, in one sample setup. The versatility and capabilities of KOOKABURRA have already resulted in a number of research papers, clearly demonstrating that this instrument has a major impact in the field of large-scale structure determination.

The classical dynamical theory of X-ray diffraction is expanded to the special case of transversely restricted wavefronts of the incident and reflected waves. This approach allows one to simulate the two-dimensional coherently scattered intensity distribution centred around a particular reciprocal lattice vector in the so-called triple-crystal diffraction scheme. The effect of the diffractometer's instrumental function on X-ray diffraction data was studied.

A `2D + λ' mode using two detector angles and wavelength is added to the modes of operation of a six-circle diffractometer, i.e. `4S + 2D' diffractometer [You (1999). J. Appl. Cryst. 32, 614–623]. In synchrotron sources, the X-ray energy, and hence the wavelength, can be a degree of freedom for angle calculations. For diffractometers with two detector circles, therefore, the variable X-ray energy can be the third degree of freedom, sufficient for accessing reciprocal space without rotating the sample. This mode is useful for limited sample rotations or X-ray beams focused smaller than the diffractometer circle of confusion.

This study demonstrates a new preparation method for single-crystal X-ray diffraction samples using a focused ion beam. The results of the structure determination and electron density maps with differently prepared samples are discussed, to evaluate this new method., High-quality single-crystal X-ray diffraction measurements are a prerequisite for obtaining precise and reliable structure data and electron densities. The single crystal should therefore fulfill several conditions, of which a regular defined shape is of particularly high importance for compounds consisting of heavy elements with high X-ray absorption coefficients. The absorption of X-rays passing through a 50 µm-thick LiNbO3 crystal can reduce the transmission of Mo Kα radiation by several tens of percent, which makes an absorption correction of the reflection intensities necessary. In order to reduce ambiguities concerning the shape of a crystal, used for the necessary absorption correction, a method for preparation of regularly shaped single crystals out of large samples is presented and evaluated. This method utilizes a focused ion beam to cut crystals with defined size and shape reproducibly and carefully without splintering. For evaluation, a single-crystal X-ray diffraction study using a laboratory diffractometer is presented, comparing differently prepared LiNbO3 crystals originating from the same macroscopic crystal plate. Results of the data reduction, structure refinement and electron density reconstruction indicate qualitatively similar values for all prepared crystals. Thus, the different preparation techniques have a smaller impact than expected. However, the atomic coordinates, electron densities and atomic charges are supposed to be more reliable since the focused-ion-beam-prepared crystal exhibits the smallest extinction influences. This preparation technique is especially recommended for susceptible samples, for cases where a minimal invasive preparation procedure is needed, and for the preparation of crystals from specific areas, complex material architectures and materials that cannot be prepared with common methods (breaking or grinding).

A facile usage of a MYTHEN 1K detector with a Huber 5021 six-circle diffractometer is described in detail. A mechanical support has been custom designed for the first time to combine the MYTHEN 1K detector with a point detector, which can be used as a reference point for each individual pixel of the MYTHEN 1K during measurements. The MYTHEN 1K is mounted on the arm of the 2θ circle of the Huber diffractometer with an intrinsic angular resolution of ∼0.0038°, and its pitch angle can be automatically adjusted with an accuracy of 0.0072°. Standard procedures are discussed for its calibration. Programs have been written in theSPECenvironment for simultaneous data conversion, integration and acquisition. The X-ray powder diffraction patterns of standard samples were measured in the Debye–Scherrer geometry and matched well with those of references. The angular shift due to sample-to-center displacement in the `flat-plate transmission' geometry, which is frequently employed inoperandoexperiments, has been successfully investigated and can be efficiently corrected. Oneoperandoexperiment using the MYTHEN 1K is presented. This work provides a straightforward procedure to use the MYTHEN 1K detector properly in Debye–Scherrer geometry, and could facilitate its application at other synchrotron facilities.

A method is given for converting slit-smeared azimuthally asymmetric data collected on a double-crystal diffractometer for concatenation with the usual pinhole-geometry small-angle neuton scattering data., Small-angle neutron scattering (SANS) measurements from thin sections of rock samples such as shales demand as great a scattering vector range as possible because the pores cover a wide range of sizes. The limitation of the scattering vector range for pinhole SANS requires slit-smeared ultra-SANS (USANS) measurements that need to be converted to pinhole geometry. The desmearing algorithm is only successful for azimuthally symmetric data. Scattering from samples cut parallel to the plane of bedding is symmetric, exhibiting circular contours on a two-dimensional detector. Samples cut perpendicular to the bedding show elliptically dependent contours with the long axis corresponding to the normal to the bedding plane. A method is given for converting such asymmetric data collected on a double-crystal diffractometer for concatenation with the usual pinhole-geometry SANS data. The aspect ratio from the SANS data is used to modify the slit-smeared USANS data to produce quasi-symmetric contours. Rotation of the sample about the incident beam may result in symmetric data but cannot extract the same information as obtained from pinhole geometry.

Epitaxy of semiconductors is a process of tremendous importance in applied science and in the optoelectronics industry. The control of defects introduced during epitaxial growth is a key point in manufacturing devices of high efficiency and durability. In this work, it is demonstrated how useful hybrid reflections are for the study of epitaxial structures with anisotropic strain gradients due to patterned substrates. High accuracy in detecting and distinguishing elastic and plastic relaxations is one of the greatest advantages of measuring this type of reflection, as well as the fact that the method can be exploited in a symmetric reflection geometry on a commercial high-resolution diffractometer.

Microcrystals of lysozyme (5–10 µm) suspended in an ultraviolet-light-curable resin were aligned three dimensionally under a non-uniformly rotating magnetic field, and then the resin was consolidated by photopolymerization to obtain a composite in which microcrystals were three-dimensionally aligned. The obtained composite (MOMA: magnetically oriented microcrystal array) was analysed using a synchrotron X-ray source. A resolution of 1.8 Å was obtained, which is in marked contrast to the resolution of 3 Å previously reported for these composites, obtained by using an in-house X-ray diffractometer. These results show that a combination of MOMAs with conventional synchrotron beamlines may have valuable potential for crystal analyses of protein crystals that do not grow to larger sizes.

The multireflection grazing-incidence X-ray diffraction (MGIXD) method is commonly used to determine a stress gradient in thin surface layers (about 1–20 µm for metals). In this article, the development of MGIXD to enable the determination not only of stresses but also of thec/aratio and thea0strain-free lattice parameter in hexagonal polycrystalline materials is presented and tested. The new procedure was applied for the results of measurements performed using a laboratory X-ray diffractometer and synchrotron radiation. The evolution of stresses and lattice parameters with depth was determined for Ti and Ti-alloy samples subjected to different mechanical surface treatments. A very good agreement of the results obtained using three different wavelengths of synchrotron radiation as well as classical X-rays (CuKα radiation) was found.

A serious limitation of the all-in-vacuum diffractometer reported by Straasø, Dippel, Becker & Als-Nielsen [J. Synchrotron Rad.(2014),21, 119–126] has so far been the inability to cool samples to near-cryogenic temperatures during measurement. The problem is solved by placing the sample in a jet of helium gas cooled by liquid nitrogen. The resulting temperature change is quantified by determining the change in unit-cell parameter and atomic displacement parameter of copper. The cooling proved successful, with a resulting temperature of ∼95 (3) K. The measured powder X-ray diffraction data are of superb quality and high resolution [up to sinθ/λ = 2.2 Å−1], permitting an extensive modelling of the thermal displacement. The anharmonic displacement of copper was modelled by a Gram–Charlier expansion of the temperature factor. As expected, the corresponding probability distribution function shows an increased probability away from neighbouring atoms and a decreased probability towards them.

SENJU, a time-of-flight Laue-type single-crystal neutron diffractometer, was developed at the Materials and Life Science Experimental Facility of the Japan Accelerator Research Complex (J-PARC). Molecular structure analysis of a sub-millimetre taurine crystal and magnetic structure analysis of an MnF2 crystal were performed to evaluate its performance., SENJU is a new single-crystal time-of-flight neutron diffractometer installed at BL18 at the Materials and Life Science Experimental Facility of the Japan Accelerator Research Complex (J-PARC). The diffractometer was designed for precise crystal and magnetic structure analyses under multiple extreme sample environments such as low temperature, high pressure and high magnetic field, and for diffraction measurements of small single crystals down to 0.1 mm3 in volume. SENJU comprises three choppers, an elliptical shape straight supermirror guide, a vacuum sample chamber and 37 scintillator area detectors. The moderator-to-sample distance is 34.8 m, and the sample-to-detector distance is 800 mm. The wavelength of incident neutrons is 0.4–4.4 Å (first frame). Because short-wavelength neutrons are available and the large solid angle around the sample position is covered by the area detectors, a large reciprocal space can be simultaneously measured. Furthermore, the vacuum sample chamber and collimator have been designed to produce a very low background level. Thus, the measurement of a small single crystal is possible. As sample environment devices, a newly developed cryostat with a two-axis (ω and φ axes) goniometer and some extreme environment devices, e.g. a vertical-field magnet, high-temperature furnace and high-pressure cell, are available. The structure analysis of a sub-millimetre size (0.1 mm3) single organic crystal, taurine, and a magnetic structure analysis of the antiferromagnetic phase of MnF2 have been performed. These results demonstrate that SENJU can be a powerful tool to promote materials science research.

Using a double-disc chopper with a variable slit opening in concert with a velocity selector and the time-of-flight data acquisition mode, controlled variation of the wavelength spread Δλ/λ between 2 and 20% has become routinely possible at the KWS-2 SANS diffractometer of the Jülich Centre for Neutron Science at the Heinz Maier-Leibnitz Center., Following demand from the user community regarding the possibility of improving the experimental resolution, the dedicated high-intensity/extended Q-range SANS diffractometer KWS-2 of the Jülich Centre for Neutron Science at the Heinz Maier-Leibnitz Center in Garching was equipped with a double-disc chopper with a variable opening slit window and time-of-flight (TOF) data acquisition option. The chopper used in concert with a dedicated high-intensity velocity selector enables the tuning at will of the wavelength resolution Δλ/λ within a broad range, from 20% (standard) down to 2%, in a convenient and safe manner following pre-planned or spontaneous decisions during the experiment. The new working mode is described in detail, and its efficiency is demonstrated on several standard samples with known properties and on a completely new crystallizable copolymer system, which were investigated using both the conventional (static) and TOF modes.

The structure of graphene obtained by chemical exfoliation of graphiteviathe oxidation/reduction procedure has been determined using wide-angle scattering of neutrons and X-rays combined with computer simulations based on classical molecular dynamics (MD). A comparison of results obtained from wide-angle neutron scattering (WANS) with the D4 neutron diffractometer dedicated for liquids and amorphous materials (Institute Laue–Langevin in Grenoble) and from wide-angle X-ray scattering (WAXS) with the laboratory Rigaku-Denki D/MAX RAPID II diffractometer has shown that both techniques provide data of a good quality that can be used to derive precise and valuable structural information about graphene. To obtain detailed structural information, the paracrystal formalism has been used along with MD simulations. The MD simulations were performed at 300 K with second-generation reactive empirical bond order potential for atoms lying in the same layer and the Lennard–Jones potential for interlayer interactions. The proposed models consist of three-layered systems, 36 Å in diameter, in which mono-vacancy, di-vacancy and Stone–Thrower–Wales types of defects are introduced. The reported results show that the WANS and WAXS methods together with the MD simulations contribute to a detailed description of the graphene materials, including the presence of topological defects, which is important as their structure at the atomic scale dramatically affects their electrical and mechanical properties.

Orientations of single crystals are usually determined by diffraction experiments. Indexing of a diffraction pattern from one crystal leads to the determination of its `orientation matrix', which defines the orientation of its crystallographic axes relative to a set of reference axes associated with the diffractometer. Crystal orientations can also be described in terms of Euler angles, especially from electron backscattered diffraction measurements. OrientXplot is a Windows program that reads all common types of orientation matrices, as well as orientation data such as Euler angles. The program calculates and displays the relative orientations of pairs of crystals, such as twins or inclusion crystals trapped inside host crystals. OrientXplot can manipulate (under user control) the orientation matrices to allow for ambiguities in indexing that arise from crystal symmetries. Orientation data can be displayed on a stereogram or output in numerical form for plotting in external programs.

The Macromolecular Neutron Diffractometer (MaNDi) is located on beamline 11B of the Spallation Neutron Source at Oak Ridge National Laboratory. The instrument is a neutron time-of-flight wavelength-resolved Laue diffractometer optimized to collect diffraction data from single crystals. The instrument has been designed to provide flexibility in several instrumental parameters, such as beam divergence and wavelength bandwidth, to allow data collection from a range of macromolecular systems.

Modeling of the X-ray diffractometer instrumental function for a given optics configuration is important both for planning experiments and for the analysis of measured data. A fast and universal method for instrumental function simulation, suitable for fully automated computer realization and describing both coplanar and noncoplanar measurement geometries for any combination of X-ray optical elements, is proposed. The method can be identified as semi-analytical backward ray tracing and is based on the calculation of a detected signal as an integral of X-ray intensities for all the rays reaching the detector. The high speed of calculation is provided by the expressions for analytical integration over the spatial coordinates that describe the detection point. Consideration of the three-dimensional propagation of rays without restriction to the diffraction plane provides the applicability of the method for noncoplanar geometry and the accuracy for characterization of the signal from a two-dimensional detector. The correctness of the simulation algorithm is checked in the following two ways: by verifying the consistency of the calculated data with the patterns expected for certain simple limiting cases and by comparing measured reciprocal-space maps with the corresponding maps simulated by the proposed method for the same diffractometer configurations. Both kinds of tests demonstrate the agreement of the simulated instrumental function shape with the measured data.

The occurrence of the basis-forbidden Si 200 and Si 222 reflections in specular X-ray diffraction ω–2Θ scans is investigated in detail as a function of the in-plane sample orientation Φ. This is done for two different diffractometer types with low and high angular divergence perpendicular to the diffraction plane. It is shown that the reflections appear for well defined conditions as a result of multiple diffraction, and not only do the obtained peaks vary in intensity but additional features like shoulders or even subpeaks may occur within a 2Θ range of about ±2.5°. This has important consequences for the detection and verification of layer peaks in the corresponding angular range.

The problem of calculating the inverse pole figure (IPF) is analyzed from the perspective of the application of time-of flight neutron diffraction toin situmonitoring of the thermomechanical behavior of engineering materials. On the basis of a quasi-Monte Carlo (QMC) method, a consistent set of grain orientations is generated and used to compute the weighting factors for IPF normalization. The weighting factors are instrument dependent and were calculated for the engineering materials diffractometer VULCAN (Spallation Neutron Source, Oak Ridge National Laboratory). The QMC method is applied to face-centered cubic structures and can be easily extended to other crystallographic symmetries. Examples include 316LN stainless steelin situloaded in tension at room temperature and an Al–2%Mg alloy, substantially deformed by cold rolling andin situannealed up to 653 K.

State-of-the-art neutron time-of-flight diffractometers at modern neutron sources allow sample throughput at rates of much less than one hour per sample. Automated sample changes with a high degree of reliability and flexibility are essential to assure safe operation and efficient use of available neutron flux. At the High-Pressure Preferred Orientation (HIPPO) diffractometer, a previous sample changer measured over 2300 texture and 400 powder samples at ambient conditions to study the properties of crystalline materials at the Lujan neutron scattering facility at the Los Alamos Neutron Science Center. Experience gained during operation of the sample changer for over a decade showed room for improvement and led to a new design using current industrial robot technology. Here, the new HIPPO versatile six-axis robotic sample changer for neutron powder diffraction experiments including texture measurements is presented.

A methodology is presented to characterize residual stress gradients using the sin2ψ technique at constant penetration depths without the use of sample χ tilting. The experiments were performed using a laboratory five-axis X-ray diffractometer equipped with an in-plane arm by scanning several reflections in order to enlarge the penetration depth range. The proposed approach, demonstrated on a blasted 11.5 µm-thick TiN coating on a WC–Co substrate, opens the possibility to perform a complex stress gradient characterization in laboratory conditions where the sample χ tilting can deteriorate the sample properties or experimental conditions, like duringin situhigh-temperature studies.

The calibration of high-energy X-ray diffraction setups using an area detector and a rotation axis is discussed. The characterization of the tilt and spatial distortions of an area detector was discussed in part one of this series [Borbély, Renversade, Kenesei & Wright (2014).J. Appl. Cryst.47, 1042–1053]. Part II links the detector frame to the laboratory frame comprising an additional rotation axis and introduces a general diffractometer equation accounting for all sources of misalignment. Additionally, an independent high-accuracy method for the evaluation of the crystallographic orientation and cell parameters of the undeformed reference crystal is presented. Setup misalignments are mainly described in terms of a residual strain tensor, considered as a quality label of the diffractometer. The method is exemplified using data sets acquired at beamlines ID11 (European Synchrotron Radiation Facility) and 1-ID (Advanced Photon Source) on Al and W single crystals, respectively. The results show that the residual strain tensor is mainly determined by the detector spatial distortion, and values as small as 1–2 × 10−4can be practically achieved.

The application of Rietveld texture analysis (RTA) to time-of-flight (TOF) neutron diffraction data allows complex materials with many diffraction peaks to be investigated, for example, rocks composed of different minerals. At the recently upgraded SKAT texture diffractometer at the JINR in Dubna (Russia), which provides three alternative multidetector systems, resolution and accessible range of latticedspacings can be adapted to sample requirements. In order to infer the optimum experimental setup and the reliability of texture estimates from complicated TOF patterns, the influence of counting statistics and various spectral resolutions on texture deconvolution was investigated. Comparing the results obtained at different resolutions and from different sections of thedpatterns indicates that the textures of a four-phase sample can be determined, but using a section at smalldspacings with a larger number of peak overlaps leads to smoother textures. A complex seven-phase sample shows orientation differences in addition to the smoothing effect. Weak textures and textures of the minor rock constituents are inaccurate owing to multiple peak overlaps. Consequently, good resolution is essential for RTA on such samples. Grid thinning tests confirmed that no more than 150 diffraction spectra are needed to characterize the texture of a monomineralic sample, and approximately 350 spectra are sufficient for a four-phase sample. The irregular grid point arrangement caused by the SKAT geometry has no negative consequences.

Some characteristics are reported of a triple-crystal diffractometer with a (+, −, +) setting of Si(220) using mirage diffraction. The advantages of this diffractometer are that its setup is easy, its structure is simple, the divergence angle from the second crystal is small and the energy resolution of the third crystal is very high., Some characteristics are reported of a triple-crystal diffractometer with a (+, −, +) setting of Si(220) using mirage diffraction. The first crystal is flat, while the second and third crystals are bent. Basically, the first crystal is used as a collimator, the second as a monochromator and the third as the sample. The third crystal also works as an analyzer. The advantages of this diffractometer are that its setup is easy, its structure is simple, the divergence angle from the second crystal is small and the energy resolution of the third crystal is high, of the order of sub-meV.

A noncoplanar measurement geometry, achieved by using a diffractometer equipped with a detector arm possessing two degrees of freedom, is a promising technique for the analysis of residual stress gradients in polycrystalline objects and for anisotropic microstructure investigations. The instrumental function for a parallel beam and a set of two orthogonal receiving Soller slits is considered in detail, and the explicit analytical expressions in terms of a convolution of functions are derived. A comparison of the calculated results with the measured profiles from a NIST SRM 660b LaB6 powder standard sample shows a good agreement.

As-grown and chemically reduced Rh-doped (1500 p.p.m.) KnbO3 single crystals grown by the Czochralski method have been characterized. Reduction of the grown crystals at different levels was carried out under a mixture of CO and CO2 gases as the crystals were grown with excess oxygen. The effect of reduction and poling on crystalline perfection was studied by high-resolution X-ray diffraction (HRXRD) using a multi-crystal X-ray diffractometer developed in-house. The diffraction curves of the as-grown, electrically poled, moderately reduced and heavily reduced single-crystal specimens show remarkable differences. The studies by HRXRD reveal that poling has some influence on the improvement of crystalline perfection, while chemical reduction has a great influence on crystalline perfection; at moderate reduction the crystal becomes nearly perfect, but when the reduction is very heavy the crystal quality decreases slightly, although it is still better than for unreduced samples. Asymmetry of the diffraction curves with respect to the peak position reveals that the as-grown specimens contain a high concentration of both vacancies and self-interstitials. After poling, the concentration of self-interstitial defects is lowered to some extent. When the specimen is moderately chemically reduced, the scattered intensity on both sides of the peak is greatly reduced, showing that the concentrations of both vacancies and interstitials are reduced to a great extent owing to chemical reduction. This clearly indicates that, as a result of the chemical reduction of oxygen in the crystal, crystalline perfection is enhanced significantly. However, under heavy chemical reduction, the number of vacancy defects is increased to a significant extent. Raman scattering, dielectric and photoluminescence studies also show interesting features, with excellent correlation with the degree of crystalline perfection influenced by the processes of reduction and poling.

The use of cryocooling in neutron diffraction has been hampered by several technical challenges, such as the need for specialized equipment and techniques. This article reports the recent development and deployment of equipment and strategies that allow routine neutron data collection on cryocooled crystals using off-the-shelf components. This system has several advantages compared to a closed displex cooling system, such as fast cooling coupled with easier crystal mounting and centering. The ability to routinely collect cryogenic neutron data for analysis will significantly broaden the range of scientific questions that can be examined by neutron protein crystallography. Cryogenic neutron data collection for macromolecules has recently become available at the new Biological Diffractometer BIODIFF at the FRM II and the Macromolecular Diffractometer (MaNDi) at the Spallation Neutron Source, Oak Ridge National Laboratory. To evaluate the benefits of a cryocooled neutron structure, a full neutron data set was collected on the BIODIFF instrument on a Toho-1 β-lactamase structure at 100 K.

A new powder diffractometer operating in transmission mode is described. It can work as a rapid very compact instrument or as a high-resolution instrument, and the sample preparation is simplified., A new powder diffractometer operating in transmission mode is described. It can work as a rapid very compact instrument or as a high-resolution instrument, and the sample preparation is simplified. The incident beam optics create pure Cu Kα1 radiation, giving rise to peak widths of ∼0.1° in 2θ in compact form with a sample-to-detector minimum radius of 55 mm, reducing to peak widths of

Pure thin tin films, electroplated on copper substrates, were investigated byin situX-ray diffraction analysis during room-temperature aging, using a laboratory diffractometer equipped with a two-dimensional detector. Diffraction spots of single Sn grains in the Sn film could be observed and traced over time by using the diffraction method adopted. For the as-deposited specimens, striking changes of the Sn reflection spots, concerning their position and intensity, as well as sudden appearances and disappearances of additional diffraction spots, were observed. This could be ascribed to local microstructural changes in the films such as grain rotation, grain growth and grain dissolution. In contrast to the as-deposited specimens, so-called post-baked specimens (i.e.annealed at 423 K for 1 h after layer deposition) exhibited a stable microstructure. The results obtained are discussed with respect to their relevance for the Sn whisker-growth phenomenon.

Theoretical models of the variations of the peak positions of X-ray rocking curves as a function of the azimuthal angle of a single-crystal wafer have been proposed. These models completely describe the variations of the peak positions both when the surface normal of a wafer is parallel and when it is not parallel to the rotation axis of the goniometer used. Based on the models, an accurate measurement method for the surface orientation of a single-crystal wafer with a small surface miscut of

A diffractometer setup is presented, based on a laser-driven plasma X-ray source for reciprocal-space mapping with femtosecond temporal resolution. In order to map out the reciprocal space, an X-ray optic with a convergent beam is used with an X-ray area detector to detect symmetrically and asymmetrically diffracted X-ray photons simultaneously. The setup is particularly suited for measuring thin films or imperfect bulk samples with broad rocking curves. For quasi-perfect crystalline samples with insignificant in-plane Bragg peak broadening, the measured reciprocal-space maps can be corrected for the known resolution function of the diffractometer in order to achieve high-resolution rocking curves with improved data quality. In this case, the resolution of the diffractometer is not limited by the convergence of the incoming X-ray beam but is solely determined by its energy bandwidth.

Several different approaches have traditionally been used for detection of X-ray powder diffraction patterns, including area detectors, point detectors and position-sensitive detectors. Each has advantages. This paper discusses use of a low-cost CCD detector attached to a diffractometer arm, where line-by-line readout of the CCD is coupled to continuous motion of the arm. When this type of detector is used and where X-ray optics are employed to focus the source image onto the detector plane both high-resolution and rapid measurements can be performed, with data collection over a complete 2θ range. This is particularly advantageous for synchrotron applications but valuable also for Guinier diffractometer laboratory instruments. Peak resolutions are shown to be moderately better than what can be obtained with a position-sensitive detector and significantly better than with an area detector. Many samples have intrinsically broadened peak shapes for which little improvement in data quality could be obtained with an analyzer-crystal detector. With comparable numbers of modules, these CCD data collection speeds can be close to those with position-sensitive detectors, but without the low-angle asymmetry seen in the latter.