A curved image‐plate detector system for high‐resolution synchrotron X‐ray diffraction

The developed curved image plate (CIP) is a one‐dimensional detector which simultaneously records high‐resolution X‐ray diffraction (XRD) patterns over a 38.7° 2θ range. In addition, an on‐site reader enables rapid extraction, transfer and storage of X‐ray intensity information in ≤30 s, and further qualifies this detector to study kinetic processes in materials science. The CIP detector can detect and store X‐ray intensity information linearly proportional to the incident photon flux over a dynamical range of about five orders of magnitude. The linearity and uniformity of the CIP detector response is not compromised in the unsaturated regions of the image plate, regardless of saturation in another region. The speed of XRD data acquisition together with excellent resolution afforded by the CIP detector is unique and opens up wide possibilities in materials research accessible through X‐ray diffraction. This article presents details of the basic features, operation and performance of the CIP detector along with some examples of applications, including high‐temperature XRD.     

High‐resolution spectroscopy on an X‐ray absorption beamline

A bent‐crystal spectrometer based on the Rowland circle geometry has been installed and tested on the BM30b/FAME beamline at the European Synchrotron Radiation Facility to improve its performances. The energy resolution of the spectrometer allows different kinds of measurements to be performed, including X‐ray absorption spectroscopy, resonant inelastic X‐ray scattering and X‐ray Raman scattering experiments. The simplicity of the experimental device makes it easily implemented on a classical X‐ray absorption beamline. This improvement in the fluorescence detection is of particular importance when the probed element is embedded in a complex and/or heavy matrix, for example in environmental sciences.     

Focusing synchrotron radiation using a polycapillary half‐focusing X‐ray lens for imaging

An imaging system based on a polycapillary half‐focusing X‐ray lens (PHFXRL) and synchrotron radiation source has been designed. The focal spot size and the gain in power density of the PHFXRL were 22 µm (FWHM) and 4648, respectively, at 14.0 keV. The spatial resolution of this new imaging system was better than 5 µm when an X‐ray charge coupled device with a pixel size of 10.9 × 10.9 µm was used. A fossil of an ancient biological specimen was imaged using this system.     

Feasibility of in‐line instruments for high‐resolution inelastic X‐ray scattering

Inelastic X‐ray scattering instruments in operation at third‐generation synchrotron radiation facilities are based on backreflections from perfect silicon crystals. This concept reaches back to the very beginnings of high‐energy‐resolution X‐ray spectroscopy and has several advantages but also some inherent drawbacks. In this paper an alternate path is investigated using a different concept, the `M⁴ instrument'. It consists of a combination of two in‐line high‐resolution monochromators, focusing mirrors and collimating mirrors. Design choices and performance estimates in comparison with existing conventional inelastic X‐ray scattering instruments are presented.     

Confocal full‐field X‐ray microscope for novel three‐dimensional X‐ray imaging

A confocal full‐field X‐ray microscope has been developed for use as a novel three‐dimensional X‐ray imaging method. The system consists of an X‐ray illuminating `sheet‐beam' whose beam shape is micrified only in one dimension, and an X‐ray full‐field microscope whose optical axis is normal to the illuminating sheet beam. An arbitral cross‐sectional region of the object is irradiated by the sheet‐beam, and secondary X‐ray emission such as fluorescent X‐rays from this region is imaged simultaneously using the full‐field microscope. This system enables a virtual sliced image of a specimen to be obtained as a two‐dimensional magnified image, and three‐dimensional observation is available only by a linear translation of the object along the optical axis of the full‐field microscope. A feasibility test has been carried out at beamline 37XU of SPring‐8. Observation of the three‐dimensional distribution of metallic inclusions in an artificial diamond was performed.     

X‐ray fluorescent CT imaging of cerebral uptake of stable‐iodine perfusion agent iodoamphetamine analog IMP in mice

Using X‐ray fluorescent computed tomography (XFCT), the in vivo and ex vivo cerebral distribution of a stable‐iodine‐labeled cerebral perfusion agent, iodoamphetamine analog (¹²⁷I‐IMP), has been recorded in the brains of mice. In vivo cerebral perfusion in the cortex, hippocampus and thalamus was depicted at 0.5 mm in‐plane spatial resolution. Ex vivo XFCT images at 0.25 mm in‐plane spatial resolution allowed the visualisation of the detailed structures of these regions. The quality of the XFCT image of the hippocampus was comparable with the ¹²⁵I‐IMP autoradiogram. These results highlight the sensitivity of XFCT and its considerable potential to evaluate cerebral perfusion in small animals without using radioactive agents.     

The contribution of synchrotron X‐ray computed microtomography to understanding volcanic processes

A series of computed microtomography experiments are reported which were performed by using a third‐generation synchrotron radiation source on volcanic rocks from various active hazardous volcanoes in Italy and other volcanic areas in the world. The applied technique allowed the internal structure of the investigated material to be accurately imaged at the micrometre scale and three‐dimensional views of the investigated samples to be produced as well as three‐dimensional quantitative measurements of textural features. The geometry of the vesicle (gas‐filled void) network in volcanic products of both basaltic and trachytic compositions were particularly focused on, as vesicle textures are directly linked to the dynamics of volcano degassing. This investigation provided novel insights into modes of gas exsolution, transport and loss in magmas that were not recognized in previous studies using solely conventional two‐dimensional imaging techniques. The results of this study are important to understanding the behaviour of volcanoes and can be combined with other geosciences disciplines to forecast their future activity.     

A multiplexed high‐resolution imaging spectrometer for resonant inelastic soft X‐ray scattering spectroscopy

The optical design of a two‐dimensional imaging soft X‐ray spectrometer is described. A monochromator will produce a dispersed spectrum in a narrow vertical illuminated stripe (～2 µm wide by ～2 mm tall) on a sample. The spectrometer will use inelastically scattered X‐rays to image the extended field on the sample in the incident photon energy direction (vertical), resolving the incident photon energy. At the same time it will image and disperse the scattered photons in the orthogonal (horizontal) direction, resolving the scattered photon energy. The principal challenge is to design a system that images from the flat‐field illumination of the sample to the flat field of the detector and to achieve sufficiently high spectral resolution. This spectrometer provides a completely parallel resonant inelastic X‐ray scattering measurement at high spectral resolution (～30000) over the energy bandwidth (～5 eV) of a soft X‐ray absorption resonance.     

Time‐resolved X‐ray PIV technique for diagnosing opaque biofluid flow with insufficient X‐ray fluxes

X‐ray imaging is used to visualize the biofluid flow phenomena in a nondestructive manner. A technique currently used for quantitative visualization is X‐ray particle image velocimetry (PIV). Although this technique provides a high spatial resolution (less than 10 µm), significant hemodynamic parameters are difficult to obtain under actual physiological conditions because of the limited temporal resolution of the technique, which in turn is due to the relatively long exposure time (～10 ms) involved in X‐ray imaging. This study combines an image intensifier with a high‐speed camera to reduce exposure time, thereby improving temporal resolution. The image intensifier amplifies light flux by emitting secondary electrons in the micro‐channel plate. The increased incident light flux greatly reduces the exposure time (below 200 µs). The proposed X‐ray PIV system was applied to high‐speed blood flows in a tube, and the velocity field information was successfully obtained. The time‐resolved X‐ray PIV system can be employed to investigate blood flows at beamlines with insufficient X‐ray fluxes under specific physiological conditions. This method facilitates understanding of the basic hemodynamic characteristics and pathological mechanism of cardiovascular diseases.     

In situ X‐ray diffraction study on the growth kinetics of NiO nanoparticles

The growth kinetics of NiO nanoparticles have been studied by in situ X‐ray diffraction using two detection systems (conventional and imaging plate). NiO nanoparticles were formed by thermal decomposition after heating of an amorphous compound formed by the coprecipitation method. It was found that the detection method using an imaging plate is more efficient than the conventional detection mode for observing changes in the crystallite growth of nanocrystalline materials. Studies have been carried out to investigate the effects of the heating rates on the particles growth. The results suggest that the growth process of the particles is accelerated when the samples are treated at low heating rates. The evolution of particles size and the diffusion coefficient obtained from X‐ray powder diffraction patterns are discussed in terms of the thermal conditions for the two types of detection.     

A miniature X‐ray emission spectrometer (miniXES) for high‐pressure studies in a diamond anvil cell

Core–shell X‐ray emission spectroscopy (XES) is a valuable complement to X‐ray absorption spectroscopy (XAS) techniques. However, XES in the hard X‐ray regime is much less frequently employed than XAS, often as a consequence of the relative scarcity of XES instrumentation having energy resolutions comparable with the relevant core‐hole lifetimes. To address this, a family of inexpensive and easily operated short‐working‐distance X‐ray emission spectrometers has been developed. The use of computer‐aided design and rapid prototype machining of plastics allows customization for various emission lines having energies from ～3 keV to ～10 keV. The specific instrument described here, based on a coarsely diced approximant of the Johansson optic, is intended to study volume collapse in Pr metal and compounds by observing the pressure dependence of the Pr Lα emission spectrum. The collection solid angle is ～50 msr, roughly equivalent to that of six traditional spherically bent crystal analyzers. The miniature X‐ray emission spectrometer (miniXES) methodology will help encourage the adoption and broad application of high‐resolution XES capabilities at hard X‐ray synchrotron facilities.     

Utilizing broadband X‐rays in a Bragg coherent X‐ray diffraction imaging experiment

A method is presented to simplify Bragg coherent X‐ray diffraction imaging studies of complex heterogeneous crystalline materials with a two‐stage screening/imaging process that utilizes polychromatic and monochromatic coherent X‐rays and is compatible with in situ sample environments. Coherent white‐beam diffraction is used to identify an individual crystal particle or grain that displays desired properties within a larger population. A three‐dimensional reciprocal‐space map suitable for diffraction imaging is then measured for the Bragg peak of interest using a monochromatic beam energy scan that requires no sample motion, thus simplifying in situ chamber design. This approach was demonstrated with Au nanoparticles and will enable, for example, individual grains in a polycrystalline material of specific orientation to be selected, then imaged in three dimensions while under load.     

High‐throughput synchrotron X‐ray diffraction for combinatorial phase mapping

Discovery of new materials drives the deployment of new technologies. Complex technological requirements demand precisely tailored material functionalities, and materials scientists are driven to search for these new materials in compositionally complex and often non‐equilibrium spaces containing three, four or more elements. The phase behavior of these high‐order composition spaces is mostly unknown and unexplored. High‐throughput methods can offer strategies for efficiently searching complex and multi‐dimensional material genomes for these much needed new materials and can also suggest a processing pathway for synthesizing them. However, high‐throughput structural characterization is still relatively under‐developed for rapid material discovery. Here, a synchrotron X‐ray diffraction and fluorescence experiment for rapid measurement of both X‐ray powder patterns and compositions for an array of samples in a material library is presented. The experiment is capable of measuring more than 5000 samples per day, as demonstrated by the acquisition of high‐quality powder patterns in a bismuth–vanadium–iron oxide composition library. A detailed discussion of the scattering geometry and its ability to be tailored for different material systems is provided, with specific attention given to the characterization of fiber textured thin films. The described prototype facility is capable of meeting the structural characterization needs for the first generation of high‐throughput material genomic searches.     

Multimodal hard X‐ray imaging of a mammography phantom at a compact synchrotron light source

The Compact Light Source is a miniature synchrotron producing X‐rays at the interaction point of a counter‐propagating laser pulse and electron bunch through the process of inverse Compton scattering. The small transverse size of the luminous region yields a highly coherent beam with an angular divergence of a few milliradians. The intrinsic monochromaticity and coherence of the produced X‐rays can be exploited in high‐sensitivity differential phase‐contrast imaging with a grating‐based interferometer. Here, the first multimodal X‐ray imaging experiments at the Compact Light Source at a clinically compatible X‐ray energy of 21 keV are reported. Dose‐compatible measurements of a mammography phantom clearly demonstrate an increase in contrast attainable through differential phase and dark‐field imaging over conventional attenuation‐based projections.     

The dedicated high‐resolution grazing‐incidence X‐ray scattering beamline 8‐ID‐E at the Advanced Photon Source

As an increasingly important structural‐characterization technique, grazing‐incidence X‐ray scattering (GIXS) has found wide applications for in situ and real‐time studies of nanostructures and nanocomposites at surfaces and interfaces. A dedicated beamline has been designed, constructed and optimized at beamline 8‐ID‐E at the Advanced Photon Source for high‐resolution and coherent GIXS experiments. The effectiveness and applicability of the beamline and the scattering techniques have been demonstrated by a host of experiments including reflectivity, grazing‐incidence static and kinetic scattering, and coherent surface X‐ray photon correlation spectroscopy. The applicable systems that can be studied at 8‐ID‐E include liquid surfaces and nanostructured thin films.     

High‐energy‐resolution diced spherical quartz analyzers for resonant inelastic X‐ray scattering

A novel diced spherical quartz analyzer for use in resonant inelastic X‐ray scattering (RIXS) is introduced, achieving an unprecedented energy resolution of 10.53 meV at the Ir L₃ absorption edge (11.215 keV). In this work the fabrication process and the characterization of the analyzer are presented, and an example of a RIXS spectrum of magnetic excitations in a Sr₃Ir₂O₇ sample is shown.     

A microfocus X‐ray fluorescence beamline at Indus‐2 synchrotron radiation facility

A microfocus X‐ray fluorescence spectroscopy beamline (BL‐16) at the Indian synchrotron radiation facility Indus‐2 has been constructed with an experimental emphasis on environmental, archaeological, biomedical and material science applications involving heavy metal speciation and their localization. The beamline offers a combination of different analytical probes, e.g. X‐ray fluorescence mapping, X‐ray microspectroscopy and total‐external‐reflection fluorescence characterization. The beamline is installed on a bending‐magnet source with a working X‐ray energy range of 4–20 keV, enabling it to excite K‐edges of all elements from S to Nb and L‐edges from Ag to U. The optics of the beamline comprises of a double‐crystal monochromator with Si(111) symmetric and asymmetric crystals and a pair of Kirkpatrick–Baez focusing mirrors. This paper describes the performance of the beamline and its capabilities with examples of measured results.     

An electrochemical cell with sapphire windows for operando synchrotron X‐ray powder diffraction and spectroscopy studies of high‐power and high‐voltage electrodes for metal‐ion batteries

A new multi‐purpose operando electrochemical cell was designed, constructed and tested on the Swiss–Norwegian Beamlines BM01 and BM31 at the European Synchrotron Radiation Facility. Single‐crystal sapphire X‐ray windows provide a good signal‐to‐noise ratio, excellent electrochemical contact because of the constant pressure between the electrodes, and perfect electrochemical stability at high potentials due to the inert and non‐conductive nature of sapphire. Examination of the phase transformations in the Li_1–xFe_0.5Mn_0.5PO₄ positive electrode (cathode) material at C/2 and 10C charge and discharge rates, and a study of the valence state of the Ni cations in the Li_1–xNi_0.5Mn_1.5O₄ cathode material for Li‐ion batteries, revealed the applicability of this novel cell design to diffraction and spectroscopic investigations of high‐power/high‐voltage electrodes for metal‐ion batteries.     

High‐resolution stress mapping of polycrystalline alumina compression using synchrotron X‐ray diffraction

The ability to achieve uniform stress in uniaxial compression tests of polycrystalline alumina is of significance for the calibration of piezospectroscopic coefficients as well as strength studies in ceramics. In this study high‐energy X‐rays were used to capture powder diffraction profiles over a half‐section of a polycrystalline alumina parallelepiped sample under an increasing uniaxial compressive load. The data were converted to strain and results were used for stress mapping of the sample. Stress maps from the study quantify the higher stresses at the sample–platen contact interface and reveal the evolution of the stress distribution in these specimens with load. For the geometry of the samples used, at the center section of the specimen the overall magnitudes of the compressive stresses were found to be 20% higher compared with the average expected theoretical stress based on the applied load and cross‐sectional area. The observed compressive stresses at the corners of the parallelepiped specimen were 62% higher and shear stresses were observed at the specimen interface to the load mechanism. The effects, seen at the interface, can lead to premature failure at these locations and can affect the accuracy of calibration of spectral peaks with stress as well as compression strength measurements. The results provide important information that can be used to establish guidelines on material and geometry considerations in developing compression tests on high‐strength ceramics.     

In situ observation of water distribution and behaviour in a polymer electrolyte fuel cell by synchrotron X‐ray imaging

In situ visualization of the distribution and behaviour of water in a polymer electrolyte fuel cell during power generation has been demonstrated using a synchrotron X‐ray imaging technique. Images were recorded using a CCD detector combined with a scintillator (Gd₂O₂S:Tb) and relay lens system, which were placed at 2.0 m or 2.5 m from the fuel cell. The images were measured continuously before and during power generation, and data on cell performance was recorded. The change of water distribution during power generation was obtained from X‐ray images normalized with the initial state of the fuel cell. Compared with other techniques for visualizing the water in fuel cells, this technique enables the water distribution and behaviour in the fuel cell to be visualized during power generation with high spatial resolution. In particular, the effects of the specifications of the gas diffusion layer on the cathode side of the fuel cell on the distribution of water were efficiently identified. This is a very powerful technique for investigating the mechanism of water flow within the fuel cell and the relationship between water behaviour and cell performance.