Incorporation of palladium into pyrite: Insights from X-ray absorption spectroscopy analysis and modelling.

Pyrite (FeS) often accommodates elevated concentrations of platinum-group elements in ores of magmatic and hydrothermal origin. In order to elucidate the role of pyrite in concentrating Pd, Pd-doped synthetic crystals were studied via X-ray absorption spectroscopy (XAS). Crystals were obtained by salt-flux method in the system saturated with respect to Pd at the temperature of 580 °C and sulphur fugacity of log f (S) = -0.

Mesoscale self-organization of polydisperse magnetic nanoparticles at the water surface.

In this study, we investigated the self-ordering process in Langmuir films of polydisperse iron oxide nanoparticles on a water surface, employing in situ x-ray scattering, surface pressure-area isotherm analysis, and Brewster angle microscopy. X-ray reflectometry confirmed the formation of a monolayer, while grazing incidence small-angle x-ray scattering revealed short-range lateral correlations with a characteristic length equal to the mean particle size. Remarkably, our findings indicated that at zero surface pressure, the particles organized into submicrometer clusters, merging upon compression to form a homogeneous layer.

Self-transformation of solid CaCO microspheres into core-shell and hollow hierarchical structures revealed by coherent X-ray diffraction imaging.

The self-transformation of solid microspheres into complex core-shell and hollow architectures cannot be explained by classical Ostwald ripening alone. Here, coherent X-ray diffraction imaging and 3D X-ray fluorescence were used to visualize in 3D the formation of hollow microparticles of calcium carbonate in the presence of polystyrene sulfonate (PSS). During the dissolution of the core made from 10-25 nm crystals, the shell developed a global spheroidal shape composed of an innermost layer of 30 nm particles containing high PSS content on which oriented vaterite crystals grew with their axis mainly oriented along the meridians.

X-ray diffraction imaging of the diamond anvils based on the microfocus x-ray source with a liquid anode.

This paper presents the results of using laboratory x-ray systems in the study of the crystal structure of anvil made from single-crystal diamond. The system is equipped with an Excillum MetalJet D2 + 70 kV high-brightness x-ray source with a liquid GaIn anode. The x-ray diffraction imaging (topography) technique with the use of a high-resolution x-ray Rigaku camera was applied to analyze crystal structure defects.

De novo determination of mosquitocidal Cry11Aa and Cry11Ba structures from naturally-occurring nanocrystals.

Cry11Aa and Cry11Ba are the two most potent toxins produced by mosquitocidal Bacillus thuringiensis subsp. israelensis and jegathesan, respectively. The toxins naturally crystallize within the host; however, the crystals are too small for structure determination at synchrotron sources.

X-ray reflectivity from curved surfaces as illustrated by a graphene layer on molten copper.

The X-ray reflectivity technique can provide out-of-plane electron-density profiles of surfaces, interfaces, and thin films, with atomic resolution accuracy. While current methodologies require high surface flatness, this becomes challenging for naturally curved surfaces, particularly for liquid metals, due to the very high surface tension. Here, the development of X-ray reflectivity measurements with beam sizes of a few tens of micrometres on highly curved liquid surfaces using a synchrotron diffractometer equipped with a double crystal beam deflector is presented.

Using diffraction losses of X-rays in a single crystal for determination of its lattice parameters as well as for monochromator calibration.

A way has been developed to measure the unit-cell parameters of a single crystal just from an energy scan with X-rays, even when the exact energy of the X-rays is not well defined due to an error in the pitch angle of the monochromator. The precision of this measurement reaches da/a ∼ 1 × 10. The method is based on the analysis of diffraction losses of the beam, transmitted through a single crystal (the so-called `glitch effect').

Coherent X-ray beam expander based on a multilens interferometer.

A coherent X-ray beam expander based on a multilens interferometer is proposed in this paper. The multilens interferometer allows efficient generation of a highly diverging coherent beam up to several milliradians in the hard X-ray energy range. The optical properties of the interferometer were experimentally demonstrated at the ESRF ID13 undulator beamline (Grenoble, France), using 12.

X-ray phase-sensitive imaging using a bilens interferometer based on refractive optics.

The phase-sensitive X-ray imaging technique based on the bilens interferometer is developed. The essence of the method consists of scanning a sample, which is set upstream of the bilens across the beam of one lens of the interferometer by recording changes in the interference pattern using a high-resolution image detector. The proposed approach allows acquiring the absolute value of a phase shift profile of the sample with a fairly high phase and spatial resolution.

Serial femtosecond crystallography on in vivo-grown crystals drives elucidation of mosquitocidal Cyt1Aa bioactivation cascade.

Cyt1Aa is the one of four crystalline protoxins produced by mosquitocidal bacterium Bacillus thuringiensis israelensis (Bti) that has been shown to delay the evolution of insect resistance in the field. Limiting our understanding of Bti efficacy and the path to improved toxicity and spectrum has been ignorance of how Cyt1Aa crystallizes in vivo and of its mechanism of toxicity. Here, we use serial femtosecond crystallography to determine the Cyt1Aa protoxin structure from sub-micron-sized crystals produced in Bti.

Diamond refractive micro-lenses for full-field X-ray imaging and microscopy produced with ion beam lithography.

We demonstrate that ion-beam lithography can be applied to the fabrication of rotationally parabolic refractive diamond X-ray micro-lenses that are of interest to the field of high-resolution X-ray focusing and microscopy. Three single half-lenses with curvature radii of 4.8 µm were produced and stacked to form a compound refractive lens, which provided diffraction-limited focusing of X-ray radiation at the P14 beamline of PETRA-III (DESY).

Impact of beryllium microstructure on the imaging and optical properties of X-ray refractive lenses.

Beryllium is one of the most transparent materials to hard X-ray radiation and, as a direct consequence, it is the main material for the fabrication of X-ray refractive optics and instrumentation for synchrotron radiation sources and free-electron laser facilities. However, it is known that almost all beryllium currently in use is polycrystalline material. In this paper, the influence of the microstructure of different beryllium grades on the optical properties of X-ray refractive lenses is studied.

Visualization of protein crystals by high-energy phase-contrast X-ray imaging.

For the extraction of the best possible X-ray diffraction data from macromolecular crystals, accurate positioning of the crystals with respect to the X-ray beam is crucial. In addition, information about the shape and internal defects of crystals allows the optimization of data-collection strategies. Here, it is demonstrated that the X-ray beam available on the macromolecular crystallography beamline P14 at the high-brilliance synchrotron-radiation source PETRA III at DESY, Hamburg, Germany can be used for high-energy phase-contrast microtomography of protein crystals mounted in an optically opaque lipidic cubic phase matrix.

X-ray reflecto-interferometer based on compound refractive lenses.

An X-ray amplitude-splitting interferometer based on compound refractive lenses, which operates in the reflection mode, is proposed and realized. The idea of a reflecto-interferometer is to use a very simplified experimental setup where a focused X-ray beam reflected from parallel flat surfaces creates an interference pattern in a wide angular range. The functional capabilities of the interferometer were experimentally tested at the European Synchrotron Radiation Facility (ESRF) ID06 beamline in the X-ray energy range from 10 keV to 15 keV.

CRL-based ultra-compact transfocator for X-ray focusing and microscopy.

A new ultra-compact transfocator (UCTF) based on X-ray compound refractive lenses (CRLs) is presented. The device can be used to change the number of one- and two-dimensional focusing CRLs by moving the individual parabolic lenses one-by-one independently, thus providing permanent energy and focal-length tunability for scanning and full-field X-ray microscopy applications. The small overall size and light weight of the device allow it to be integrated in any synchrotron beamline, while even simplifying the experimental layout.

Optical performance and radiation stability of polymer X-ray refractive nano-lenses.

Full-field X-ray imaging and microscopy with polymer compound refractive nano-lenses is demonstrated. Experiments were carried out at beamline ID13 at the European Synchrotron and yielded a resolution of 100 nm. The lenses were demonstrated to be functioning even after an absorbed dose of ∼10 Gy.

Investigation of `glitches' in the energy spectrum induced by single-crystal diamond compound X-ray refractive lenses.

Single-crystal diamond stands out among all the candidate materials that could be exploited to fabricate compound refractive lenses (CRLs) owing to its extremely stable properties. Among all related experimental features, beam divergence, χ-angles relative to the incoming beam in Eulerian geometry and different positions of the X-ray beam relative to the lens geometry may influence the transmission energy spectrum of CRLs. In addition, the orientation of the single-crystal diamond sample may also affect the glitches significantly.

Zernike phase contrast in high-energy x-ray transmission microscopy based on refractive optics.

The current work represents the first implementation of Zernike phase contrast for compound refractive lens based x-ray microscopy, and also the first successful Zernike phase contrast experiment at photon energies above 12 keV. Phase contrast was achieved by fitting a compound refractive lens with a circular phase plate. The resolution is demonstrated to be sub-micron, and can be improved using already existing technology.

Polymer X-ray refractive nano-lenses fabricated by additive technology.

The present work demonstrates the potential applicability of additive manufacturing to X-Ray refractive nano-lenses. A compound refractive lens with a radius of 5 µm was produced by the two-photon polymerization induced lithography. It was successfully tested at the X-ray microfocus laboratory source and a focal spot of 5 μm was measured.

Protective radiolucent aluminium oxide coatings for beryllium X-ray optics.

Beryllium, being one of the most transparent materials to X-ray radiation, has become the material of choice for X-ray optics instrumentation at synchrotron radiation sources and free-electron laser facilities. However, there are concerns due to its high toxicity and, consequently, there is a need for special safety regulations. The authors propose to apply protective coatings in order to seal off beryllium from the ambient atmosphere, thus preventing degradation processes providing additional protection for users and prolonging the service time of the optical elements.

Linear parabolic single-crystal diamond refractive lenses for synchrotron X-ray sources.

Linear parabolic diamond refractive lenses are presented, designed to withstand high thermal and radiation loads coming from upgraded accelerator X-ray sources. Lenses were manufactured by picosecond laser treatment of a high-quality single-crystal synthetic diamond. Twelve lenses with radius of curvature at parabola apex R = 200 µm, geometrical aperture A = 900 µm and length L = 1.

30-Lens interferometer for high-energy X-rays.

A novel high-energy multi-lens interferometer consisting of 30 arrays of planar compound refractive lenses is reported. Under coherent illumination each lens array creates a diffraction-limited secondary source. Overlapping such coherent beams produces an interference pattern demonstrating strong longitudinal functional dependence.

Terapascal static pressure generation with ultrahigh yield strength nanodiamond.

Studies of materials' properties at high and ultrahigh pressures lead to discoveries of unique physical and chemical phenomena and a deeper understanding of matter. In high-pressure research, an achievable static pressure limit is imposed by the strength of available strong materials and design of high-pressure devices. Using a high-pressure and high-temperature technique, we synthesized optically transparent microballs of bulk nanocrystalline diamond, which were found to have an exceptional yield strength (~460 GPa at a confining pressure of ~70 GPa) due to the unique microstructure of bulk nanocrystalline diamond.

Lens coupled tunable Young's double pinhole system for hard X-ray spatial coherence characterization.

We have implemented a modified Young's double slit experiment using pinholes with tunable separation distance coupled with compound refractive lens for hard X-ray spatial coherence characterization. Varying distance between the apertures provides a high sensitivity to the determination of spatial coherence across a wide range of experimental parameters. The use of refractive lenses as a Fourier transformer ensures far field registration conditions and allows the realization of a very compact experimental setup in comparison with the classical Young technique and its derivatives.

Substantial Difference in Ordering of 10, 15, and 20 nm Iron Oxide Nanoparticles on a Water Surface: In Situ Characterization by the Grazing Incidence X-ray Scattering.

In the present study, for the first time, a unique combination of in situ grazing incidence small-angle X-ray scattering and X-ray reflectivity, accompanied by the pressure-area isotherm analysis, Brewster angle microscopy, and ex situ scanning electron microscopy, was applied for investigation of two-dimensional superlattices of magnetic nanoparticles as they form on a water surface in a Langmuir trough. Iron oxide particles of different sizes stabilized with a single layer of oleic acid were used. It is demonstrated that monodisperse 10 nm particles on a water surface reproducibly form identical highly ordered monolayers in a wide range of experimental conditions, while monodisperse 20 nm particles always form compact three-dimensional clusters and never the monolayers.