copy The role of carboxylate ligand orbitals in the breathing dynamics of a metal-organic framework by resonant X-ray emission spectroscopy By journals.iucr.org Published On :: 2024-02-16 Metal-organic frameworks (MOFs) exhibit structural flexibility induced by temperature and guest adsorption, as demonstrated in the structural breathing transition in certain MOFs between narrow-pore and large-pore phases. Soft modes were suggested to entropically drive such pore breathing through enhanced vibrational dynamics at high temperatures. In this work, oxygen K-edge resonant X-ray emission spectroscopy of the MIL-53(Al) MOF was performed to selectively probe the electronic perturbation accompanying pore breathing dynamics at the ligand carboxylate site for metal–ligand interaction. It was observed that the temperature-induced vibrational dynamics involves switching occupancy between antisymmetric and symmetric configurations of the carboxylate oxygen lone pair orbitals, through which electron density around carboxylate oxygen sites is redistributed and metal–ligand interactions are tuned. In turn, water adsorption involves an additional perturbation of π orbitals not observed in the structural change solely induced by temperature. Full Article text
copy High-pressure X-ray photon correlation spectroscopy at fourth-generation synchrotron sources By journals.iucr.org Published On :: 2024-04-10 A new experimental setup combining X-ray photon correlation spectroscopy (XPCS) in the hard X-ray regime and a high-pressure sample environment has been developed to monitor the pressure dependence of the internal motion of complex systems down to the atomic scale in the multi-gigapascal range, from room temperature to 600 K. The high flux of coherent high-energy X-rays at fourth-generation synchrotron sources solves the problems caused by the absorption of diamond anvil cells used to generate high pressure, enabling the measurement of the intermediate scattering function over six orders of magnitude in time, from 10−3 s to 103 s. The constraints posed by the high-pressure generation such as the preservation of X-ray coherence, as well as the sample, pressure and temperature stability, are discussed, and the feasibility of high-pressure XPCS is demonstrated through results obtained on metallic glasses. Full Article text
copy A sub-100 nm thickness flat jet for extreme ultraviolet to soft X-ray absorption spectroscopy By journals.iucr.org Published On :: 2024-04-09 Experimental characterization of the structural, electronic and dynamic properties of dilute systems in aqueous solvents, such as nanoparticles, molecules and proteins, are nowadays an open challenge. X-ray absorption spectroscopy (XAS) is probably one of the most established approaches to this aim as it is element-specific. However, typical dilute systems of interest are often composed of light elements that require extreme-ultraviolet to soft X-ray photons. In this spectral regime, water and other solvents are rather opaque, thus demanding radical reduction of the solvent volume and removal of the liquid to minimize background absorption. Here, we present an experimental endstation designed to operate a liquid flat jet of sub-micrometre thickness in a vacuum environment compatible with extreme ultraviolet/soft XAS measurements in transmission geometry. The apparatus developed can be easily connected to synchrotron and free-electron-laser user-facility beamlines dedicated to XAS experiments. The conditions for stable generation and control of the liquid flat jet are analyzed and discussed. Preliminary soft XAS measurements on some test solutions are shown. Full Article text
copy PINK: a tender X-ray beamline for X-ray emission spectroscopy By journals.iucr.org Published On :: 2024-04-25 A high-flux beamline optimized for non-resonant X-ray emission spectroscopy (XES) in the tender X-ray energy range has been constructed at the BESSY II synchrotron source. The beamline utilizes a cryogenically cooled undulator that provides X-rays over the energy range 2.1 keV to 9.5 keV. This energy range provides access to XES [and in the future X-ray absorption spectroscopy (XAS)] studies of transition metals ranging from Ti to Cu (Kα, Kβ lines) and Zr to Ag (Lα, Lβ), as well as light elements including P, S, Cl, K and Ca (Kα, Kβ). The beamline can be operated in two modes. In PINK mode, a multilayer monochromator (E/ΔE ≃ 30–80) provides a high photon flux (1014 photons s−1 at 6 keV and 300 mA ring current), allowing non-resonant XES measurements of dilute substances. This mode is currently available for general user operation. X-ray absorption near-edge structure and resonant XAS techniques will be available after the second stage of the PINK commissioning, when a high monochromatic mode (E/ΔE ≃ 10000–40000) will be facilitated by a double-crystal monochromator. At present, the beamline incorporates two von Hamos spectrometers, enabling time-resolved XES experiments with time scales down to 0.1 s and the possibility of two-color XES experiments. This paper describes the optical scheme of the PINK beamline and the endstation. The design of the two von Hamos dispersive spectrometers and sample environment are discussed here in detail. To illustrate, XES spectra of phosphorus complexes, KCl, TiO2 and Co3O4 measured using the PINK setup are presented. Full Article text
copy Synchrotron infrared nanospectroscopy in fourth-generation storage rings By journals.iucr.org Published On :: 2024-04-17 Fourth-generation synchrotron storage rings represent a significant milestone in synchrotron technology, offering outstandingly bright and tightly focused X-ray beams for a wide range of scientific applications. However, due to their inherently tight magnetic lattices, these storage rings have posed critical challenges for accessing lower-energy radiation, such as infrared (IR) and THz. Here the first-ever IR beamline to be installed and to operate at a fourth-generation synchrotron storage ring is introduced. This work encompasses several notable advancements, including a thorough examination of the new IR source at Sirius, a detailed description of the radiation extraction scheme, and the successful validation of our optical concept through both measurements and simulations. This optimal optical setup has enabled us to achieve an exceptionally wide frequency range for our nanospectroscopy experiments. Through the utilization of synchrotron IR nanospectroscopy on biological and hard matter samples, the practicality and effectiveness of this beamline has been successfully demonstrated. The advantages of fourth-generation synchrotron IR sources, which can now operate with unparalleled stability as a result of the stringent requirements for producing low-emittance X-rays, are emphasized. Full Article text
copy Development of dual-beamline photoelectron momentum microscopy for valence orbital analysis By journals.iucr.org Published On :: 2024-04-15 The soft X-ray photoelectron momentum microscopy (PMM) experimental station at the UVSOR Synchrotron Facility has been recently upgraded by additionally guiding vacuum ultraviolet (VUV) light in a normal-incidence configuration. PMM offers a very powerful tool for comprehensive electronic structure analyses in real and momentum spaces. In this work, a VUV beam with variable polarization in the normal-incidence geometry was obtained at the same sample position as the soft X-ray beam from BL6U by branching the VUV beamline BL7U. The valence electronic structure of the Au(111) surface was measured using horizontal and vertical linearly polarized (s-polarized) light excitations from BL7U in addition to horizontal linearly polarized (p-polarized) light excitations from BL6U. Such highly symmetric photoemission geometry with normal incidence offers direct access to atomic orbital information via photon polarization-dependent transition-matrix-element analysis. Full Article text
copy A new experimental setup for combined fast differential scanning calorimetry and X-ray photon correlation spectroscopy By journals.iucr.org Published On :: 2024-04-24 Synchrotron-radiation-based techniques are a powerful tool for the investigation of materials. In particular, the availability of highly brilliant sources has opened the possibility to develop techniques sensitive to dynamics at the atomic scale such as X-ray photon correlation spectroscopy (XPCS). XPCS is particularly relevant in the study of glasses, which have been often investigated at the macroscopic scale by, for example, differential scanning calorimetry. Here, we show how to adapt a Flash calorimeter to combine XPCS and calorimetric scans. This setup paves the way to novel experiments requiring dynamical and thermodynamic information, ranging from the study of the crystallization kinetics to the study of the glass transition in systems that can be vitrified thanks to the high cooling rates reachable with an ultrafast calorimeter. Full Article text
copy Operando double-edge high-resolution X-ray absorption spectroscopy study of BiVO4 photoanodes By journals.iucr.org Published On :: 2024-04-15 High energy resolution fluorescence detected X-ray absorption spectroscopy is a powerful method for probing the electronic structure of functional materials. The X-ray penetration depth and photon-in/photon-out nature of the method allow operando experiments to be performed, in particular in electrochemical cells. Here, operando high-resolution X-ray absorption measurements of a BiVO4 photoanode are reported, simultaneously probing the local electronic states of both cations. Small but significant variations of the spectral lineshapes induced by the applied potential were observed and an explanation in terms of the occupation of electronic states at or near the band edges is proposed. Full Article text
copy Infrared spectroscopy across scales in length and time at BESSY II By journals.iucr.org Published On :: 2024-04-23 The infrared beamline at BESSY II storage ring was upgraded recently to extend the capabilities of infrared microscopy. The endstations available at the beamline are now facilitating improved characterization of molecules and materials at different length scales and time resolutions. Here, the current outline of the beamline is reported and an overview of the endstations available is given. In particular, the first results obtained by using a new microscope for nano-spectroscopy that was implemented are presented. The capabilities of the scattering-type near-field optical microscope (s-SNOM) are demonstrated by investigating cellulose microfibrils, representing nanoscopic objects of a hierarchical structure. It is shown that the s-SNOM coupled to the beamline allows imaging to be performed with a spatial resolution of less than 30 nm and infrared spectra to be collected from an effective volume of less than 30 nm × 30 nm × 12 nm. Potential steps for further optimization of the beamline performance are discussed. Full Article text
copy Asymmetric electrostatic dodecapole: compact bandpass filter with low aberrations for momentum microscopy By journals.iucr.org Published On :: 2024-06-20 Imaging energy filters in photoelectron microscopes and momentum microscopes use spherical fields with deflection angles of 90°, 180° and even 2 × 180°. These instruments are optimized for high energy resolution, and exhibit image aberrations when operated in high transmission mode at medium energy resolution. Here, a new approach is presented for bandpass-filtered imaging in real or reciprocal space using an electrostatic dodecapole with an asymmetric electrode array. In addition to energy-dispersive beam deflection, this multipole allows aberration correction up to the third order. Here, its use is described as a bandpass prefilter in a time-of-flight momentum microscope at the hard X-ray beamline P22 of PETRA III. The entire instrument is housed in a straight vacuum tube because the deflection angle is only 4° and the beam displacement in the filter is only ∼8 mm. The multipole is framed by transfer lenses in the entrance and exit branches. Two sets of 16 different-sized entrance and exit apertures on piezomotor-driven mounts allow selection of the desired bandpass. For pass energies between 100 and 1400 eV and slit widths between 0.5 and 4 mm, the transmitted kinetic energy intervals are between 10 eV and a few hundred electronvolts (full width at half-maximum). The filter eliminates all higher or lower energy signals outside the selected bandpass, significantly improving the signal-to-background ratio in the time-of-flight analyzer. Full Article text
copy Roentgenoscopy of laser-induced projectile impact testing By journals.iucr.org Published On :: 2024-06-06 Laser-induced projectile impact testing (LIPIT) based on synchrotron imaging is proposed and validated. This emerging high-velocity, high-strain microscale dynamic loading technique offers a unique perspective on the strain and energy dissipation behavior of materials subjected to high-speed microscale single-particle impacts. When combined with synchrotron radiation imaging techniques, LIPIT allows for in situ observation of particle infiltration. Two validation experiments were carried out, demonstrating the potential of LIPIT in the roentgenoscopy of the dynamic properties of various materials. With a spatial resolution of 10 µm and a temporal resolution of 33.4 µs, the system was successfully realized at the Beijing Synchrotron Radiation Facility 3W1 beamline. This innovative approach opens up new avenues for studying the dynamic properties of materials in situ. Full Article text
copy L3-edge X-ray spectroscopy of rhodium and palladium compounds By journals.iucr.org Published On :: 2024-06-26 L3-edge high-energy-resolution fluorescence-detection X-ray absorption near-edge structure (XANES) spectra for palladium and rhodium compounds are presented, with focus on their electronic structures. The data are compared with transmission XANES spectra recorded at the K-edge. A correlation between the absorption edge energy and the metal ion oxidation state is not observed. Despite the different filling of the 4d orbitals and different local coordination, the Rh and Pd compounds show remarkably similar spectral shapes. Calculation of the density of states and of the L3-XANES data reproduce the experimental results. Full Article text
copy A versatile sample-delivery system for X-ray photoelectron spectroscopy of in-flight aerosols and free nanoparticles at MAX IV Laboratory By journals.iucr.org Published On :: 2024-08-07 Aerosol science is of utmost importance for both climate and public health research, and in recent years X-ray techniques have proven effective tools for aerosol-particle characterization. To date, such methods have often involved the study of particles collected onto a substrate, but a high photon flux may cause radiation damage to such deposited particles and volatile components can potentially react with the surrounding environment after sampling. These and many other factors make studies on collected aerosol particles challenging. Therefore, a new aerosol sample-delivery system dedicated to X-ray photoelectron spectroscopy studies of aerosol particles and gas molecules in-flight has been developed at the MAX IV Laboratory. The aerosol particles are brought from atmospheric pressure to vacuum in a continuous flow, ensuring that the sample is constantly renewed, thus avoiding radiation damage, and allowing measurements on the true unsupported aerosol. At the same time, available gas molecules can be used for energy calibration and to study gas-particle partitioning. The design features of the aerosol sample-delivery system and important information on the operation procedures are described in detail here. Furthermore, to demonstrate the experimental range of the aerosol sample-delivery system, results from aerosol particles of different shape, size and composition are presented, including inorganic atmospheric aerosols, secondary organic aerosols and engineered nanoparticles. Full Article text
copy Web-CONEXS: an inroad to theoretical X-ray absorption spectroscopy By journals.iucr.org Published On :: 2024-08-01 Accurate analysis of the rich information contained within X-ray spectra usually calls for detailed electronic structure theory simulations. However, density functional theory (DFT), time-dependent DFT and many-body perturbation theory calculations increasingly require the use of advanced codes running on high-performance computing (HPC) facilities. Consequently, many researchers who would like to augment their experimental work with such simulations are hampered by the compounding of nontrivial knowledge requirements, specialist training and significant time investment. To this end, we present Web-CONEXS, an intuitive graphical web application for democratizing electronic structure theory simulations. Web-CONEXS generates and submits simulation workflows for theoretical X-ray absorption and X-ray emission spectroscopy to a remote computing cluster. In the present form, Web-CONEXS interfaces with three software packages: ORCA, FDMNES and Quantum ESPRESSO, and an extensive materials database courtesy of the Materials Project API. These software packages have been selected to model diverse materials and properties. Web-CONEXS has been conceived with the novice user in mind; job submission is limited to a subset of simulation parameters. This ensures that much of the simulation complexity is lifted and preliminary theoretical results are generated faster. Web-CONEXS can be leveraged to support beam time proposals and serve as a platform for preliminary analysis of experimental data. Full Article text
copy In situ characterization of stresses, deformation and fracture of thin films using transmission X-ray nanodiffraction microscopy. Corrigendum By journals.iucr.org Published On :: 2024-08-06 Errors in variable subscripts, equations and Fig. 8 in Section 3.2 of the article by Lotze et al. [(2024). J. Synchrotron Rad. 31, 42–52] are corrected. Full Article text
copy Demonstration of full polarization control of soft X-ray pulses with Apple X undulators at SwissFEL using recoil ion momentum spectroscopy By journals.iucr.org Published On :: 2024-08-09 The ability to freely control the polarization of X-rays enables measurement techniques relying on circular or linear dichroism, which have become indispensable tools for characterizing the properties of chiral molecules or magnetic structures. Therefore, the demand for polarization control in X-ray free-electron lasers is increasing to enable polarization-sensitive dynamical studies on ultrafast time scales. The soft X-ray branch Athos of SwissFEL was designed with the aim of providing freely adjustable and arbitrary polarization by building its undulator solely from modules of the novel Apple X type. In this paper, the magnetic model of the linear inclined and circular Apple X polarization schemes are studied. The polarization is characterized by measuring the angular electron emission distributions of helium for various polarizations using cold target recoil ion momentum spectroscopy. The generation of fully linear polarized light of arbitrary angle, as well as elliptical polarizations of varying degree, are demonstrated. Full Article text
copy Development of a flat jet delivery system for soft X-ray spectroscopy at MAX IV By journals.iucr.org Published On :: 2024-08-22 One of the most challenging aspects of X-ray research is the delivery of liquid sample flows into the soft X-ray beam. Currently, cylindrical microjets are the most commonly used sample injection systems for soft X-ray liquid spectroscopy. However, they suffer from several drawbacks, such as complicated geometry due to their curved surface. In this study, we propose a novel 3D-printed nozzle design by introducing microscopic flat sheet jets that provide micrometre-thick liquid sheets with high stability, intending to make this technology more widely available to users. Our research is a collaboration between the EuXFEL and MAX IV research facilities. This collaboration aims to develop and refine a 3D-printed flat sheet nozzle design and a versatile jetting platform that is compatible with multiple endstations and measurement techniques. Our flat sheet jet platform improves the stability of the jet and increases its surface area, enabling more precise scanning and differential measurements in X-ray absorption, scattering, and imaging applications. Here, we demonstrate the performance of this new arrangement for a flat sheet jet setup with X-ray photoelectron spectroscopy, photoelectron angular distribution, and soft X-ray absorption spectroscopy experiments performed at the photoemission endstation of the FlexPES beamline at MAX IV Laboratory in Lund, Sweden. Full Article text
copy The soft X-ray spectromicroscopy beamline BL08U1A upgrade at SSRF By journals.iucr.org Published On :: 2024-08-22 Beamline BL08U1A is a soft X-ray spectromicroscopy beamline at Shanghai Synchrotron Radiation Facility (SSRF) that exhibits the capabilities of high spatial resolution (30 nm) and high energy resolving power (over 104). As a first-generation beamline of SSRF, owing to its continuous operation over the last ten years, an urgent upgrade of the equipment including the monochromator was deemed necessary. The upgrade work included the overall construction of the monochromator and replacement of the mirrors upstream and downstream of the monochromator. Based on its original skeleton, two elliptically cylinder mirrors were designed to focus the beam horizontally, which can increase the flux density by about three times on the exit slits. Meanwhile, the application of variable-line-space gratings in the monochromator demonstrates the dual functions of dispersing and focusing on the exit slits which can decrease abberations dramatically. After the upgrade of the main components of the beamline, the energy range is 180–2000 eV, the energy resolving power reaches 16333 @ 244 eV and 12730 @ 401 eV, and the photon flux measured in the experimental station is over 2.45 × 109 photons s−1 (E/ΔE = 6440 @ 244 eV). Full Article text
copy The TR-icOS setup at the ESRF: time-resolved microsecond UV–Vis absorption spectroscopy on protein crystals By journals.iucr.org Published On :: 2024-01-01 The technique of time-resolved macromolecular crystallography (TR-MX) has recently been rejuvenated at synchrotrons, resulting in the design of dedicated beamlines. Using pump–probe schemes, this should make the mechanistic study of photoactive proteins and other suitable systems possible with time resolutions down to microseconds. In order to identify relevant time delays, time-resolved spectroscopic experiments directly performed on protein crystals are often desirable. To this end, an instrument has been built at the icOS Lab (in crystallo Optical Spectroscopy Laboratory) at the European Synchrotron Radiation Facility using reflective focusing objectives with a tuneable nanosecond laser as a pump and a microsecond xenon flash lamp as a probe, called the TR-icOS (time-resolved icOS) setup. Using this instrument, pump–probe spectra can rapidly be recorded from single crystals with time delays ranging from a few microseconds to seconds and beyond. This can be repeated at various laser pulse energies to track the potential presence of artefacts arising from two-photon absorption, which amounts to a power titration of a photoreaction. This approach has been applied to monitor the rise and decay of the M state in the photocycle of crystallized bacteriorhodopsin and showed that the photocycle is increasingly altered with laser pulses of peak fluence greater than 100 mJ cm−2, providing experimental laser and delay parameters for a successful TR-MX experiment. Full Article text
copy Validation of electron-microscopy maps using solution small-angle X-ray scattering By journals.iucr.org Published On :: 2024-06-27 The determination of the atomic resolution structure of biomacromolecules is essential for understanding details of their function. Traditionally, such a structure determination has been performed with crystallographic or nuclear resonance methods, but during the last decade, cryogenic transmission electron microscopy (cryo-TEM) has become an equally important tool. As the blotting and flash-freezing of the samples can induce conformational changes, external validation tools are required to ensure that the vitrified samples are representative of the solution. Although many validation tools have already been developed, most of them rely on fully resolved atomic models, which prevents early screening of the cryo-TEM maps. Here, a novel and automated method for performing such a validation utilizing small-angle X-ray scattering measurements, publicly available through the new software package AUSAXS, is introduced and implemented. The method has been tested on both simulated and experimental data, where it was shown to work remarkably well as a validation tool. The method provides a dummy atomic model derived from the EM map which best represents the solution structure. Full Article text
copy Scanning WAXS microscopy of regenerated cellulose fibers at mesoscopic resolution By journals.iucr.org Published On :: 2024-06-11 In this work, regenerated cellulose textile fibers, Ioncell-F, dry-wet spun with different draw ratios, have been investigated by scanning wide-angle X-ray scattering (WAXS) using a mesoscopic X-ray beam. The fibers were found to be homogeneous on the 500 nm length scale. Analysis of the azimuthal angular dependence of a crystalline Bragg spot intensity revealed a radial dependence of the degree of orientation of crystallites that was found to increase with the distance from the center of the fiber. We attribute this to radial velocity gradients during the extrusion of the spin dope and the early stage of drawing. On the other hand, the fiber crystallinity was found to be essentially homogeneous over the fiber cross section. Full Article text
copy Structure of Aquifex aeolicus lumazine synthase by cryo-electron microscopy to 1.42 Å resolution By journals.iucr.org Published On :: 2024-07-04 Single-particle cryo-electron microscopy (cryo-EM) has become an essential structural determination technique with recent hardware developments making it possible to reach atomic resolution, at which individual atoms, including hydrogen atoms, can be resolved. In this study, we used the enzyme involved in the penultimate step of riboflavin biosynthesis as a test specimen to benchmark a recently installed microscope and determine if other protein complexes could reach a resolution of 1.5 Å or better, which so far has only been achieved for the iron carrier ferritin. Using state-of-the-art microscope and detector hardware as well as the latest software techniques to overcome microscope and sample limitations, a 1.42 Å map of Aquifex aeolicus lumazine synthase (AaLS) was obtained from a 48 h microscope session. In addition to water molecules and ligands involved in the function of AaLS, we can observe positive density for ∼50% of the hydrogen atoms. A small improvement in the resolution was achieved by Ewald sphere correction which was expected to limit the resolution to ∼1.5 Å for a molecule of this diameter. Our study confirms that other protein complexes can be solved to near-atomic resolution. Future improvements in specimen preparation and protein complex stabilization may allow more flexible macromolecules to reach this level of resolution and should become a priority of study in the field. Full Article text
copy Roodmus: a toolkit for benchmarking heterogeneous electron cryo-microscopy reconstructions By journals.iucr.org Published On :: 2024-10-15 Conformational heterogeneity of biological macromolecules is a challenge in single-particle averaging (SPA). Current standard practice is to employ classification and filtering methods that may allow a discrete number of conformational states to be reconstructed. However, the conformation space accessible to these molecules is continuous and, therefore, explored incompletely by a small number of discrete classes. Recently developed heterogeneous reconstruction algorithms (HRAs) to analyse continuous heterogeneity rely on machine-learning methods that employ low-dimensional latent space representations. The non-linear nature of many of these methods poses a challenge to their validation and interpretation and to identifying functionally relevant conformational trajectories. These methods would benefit from in-depth benchmarking using high-quality synthetic data and concomitant ground truth information. We present a framework for the simulation and subsequent analysis with respect to the ground truth of cryo-EM micrographs containing particles whose conformational heterogeneity is sourced from molecular dynamics simulations. These synthetic data can be processed as if they were experimental data, allowing aspects of standard SPA workflows as well as heterogeneous reconstruction methods to be compared with known ground truth using available utilities. The simulation and analysis of several such datasets are demonstrated and an initial investigation into HRAs is presented. Full Article text
copy Simulations of dislocation contrast in dark-field X-ray microscopy By journals.iucr.org Published On :: 2024-03-21 Dark-field X-ray microscopy (DFXM) is a full-field imaging technique that non-destructively maps the structure and local strain inside deeply embedded crystalline elements in three dimensions. In DFXM, an objective lens is placed along the diffracted beam to generate a magnified projection image of the local diffracted volume. This work explores contrast methods and optimizes the DFXM setup specifically for the case of mapping dislocations. Forward projections of detector images are generated using two complementary simulation tools based on geometrical optics and wavefront propagation, respectively. Weak and strong beam contrast and the mapping of strain components are studied. The feasibility of observing dislocations in a wall is elucidated as a function of the distance between neighbouring dislocations and the spatial resolution. Dislocation studies should be feasible with energy band widths of 10−2, of relevance for fourth-generation synchrotron and X-ray free-electron laser sources. Full Article text
copy Low-dose electron microscopy imaging for beam-sensitive metal–organic frameworks By journals.iucr.org Published On :: 2024-09-05 Metal–organic frameworks (MOFs) have garnered significant attention in recent years owing to their exceptional properties. Understanding the intricate relationship between the structure of a material and its properties is crucial for guiding the synthesis and application of these materials. (Scanning) Transmission electron microscopy (S)TEM imaging stands out as a powerful tool for structural characterization at the nanoscale, capable of detailing both periodic and aperiodic local structures. However, the high electron-beam sensitivity of MOFs presents substantial challenges in their structural characterization using (S)TEM. This paper summarizes the latest advancements in low-dose high-resolution (S)TEM imaging technology and its application in MOF material characterization. It covers aspects such as framework structure, defects, and surface and interface analysis, along with the distribution of guest molecules within MOFs. This review also discusses emerging technologies like electron ptychography and outlines several prospective research directions in this field. Full Article text
copy The AUREX cell: a versatile operando electrochemical cell for studying catalytic materials using X-ray diffraction, total scattering and X-ray absorption spectroscopy under working conditions By journals.iucr.org Published On :: 2024-09-20 Understanding the structure–property relationship in electrocatalysts under working conditions is crucial for the rational design of novel and improved catalytic materials. This paper presents the Aarhus University reactor for electrochemical studies using X-rays (AUREX) operando electrocatalytic flow cell, designed as an easy-to-use versatile setup with a minimal background contribution and a uniform flow field to limit concentration polarization and handle gas formation. The cell has been employed to measure operando total scattering, diffraction and absorption spectroscopy as well as simultaneous combinations thereof on a commercial silver electrocatalyst for proof of concept. This combination of operando techniques allows for monitoring of the short-, medium- and long-range structure under working conditions, including an applied potential, liquid electrolyte and local reaction environment. The structural transformations of the Ag electrocatalyst are monitored with non-negative matrix factorization, linear combination analysis, the Pearson correlation coefficient matrix, and refinements in both real and reciprocal space. Upon application of an oxidative potential in an Ar-saturated aqueous 0.1 M KHCO3/K2CO3 electrolyte, the face-centered cubic (f.c.c.) Ag gradually transforms first to a trigonal Ag2CO3 phase, followed by the formation of a monoclinic Ag2CO3 phase. A reducing potential immediately reverts the structure to the Ag (f.c.c.) phase. Following the electrochemical-reaction-induced phase transitions is of fundamental interest and necessary for understanding and improving the stability of electrocatalysts, and the operando cell proves a versatile setup for probing this. In addition, it is demonstrated that, when studying electrochemical reactions, a high energy or short exposure time is needed to circumvent beam-induced effects. Full Article text
copy Deconstructing 3D growth rates from transmission microscopy images of facetted crystals as captured in situ within supersaturated aqueous solutions By journals.iucr.org Published On :: 2024-09-25 Here, a morphologically based approach is used for the in situ characterization of 3D growth rates of facetted crystals from the solution phase. Crystal images of single crystals of the β-form of l-glutamic acid are captured in situ during their growth at a relative supersaturation of 1.05 using transmission optical microscopy. The crystal growth rates estimated for both the {101} capping and {021} prismatic faces through image processing are consistent with those determined using reflection light mode [Jiang, Ma, Hazlehurst, Ilett, Jackson, Hogg & Roberts (2024). Cryst. Growth Des. 24, 3277–3288]. The growth rate in the {010} face is, for the first time, estimated from the shadow widths of the {021} prismatic faces and found to be typically about half that of the {021} prismatic faces. Analysis of the 3D shape during growth reveals that the initial needle-like crystal morphology develops during the growth process to become more tabular, associated with the Zingg factor evolving from 2.9 to 1.7 (>1). The change in relative solution supersaturation during the growth process is estimated from calculations of the crystal volume, offering an alternative approach to determine this dynamically from visual observations. Full Article text
copy Five-analyzer Johann spectrometer for hard X-ray photon-in/photon-out spectroscopy at the Inner Shell Spectroscopy beamline at NSLS-II: design, alignment and data acquisition By journals.iucr.org Published On :: 2024-10-30 Here, a recently commissioned five-analyzer Johann spectrometer at the Inner Shell Spectroscopy beamline (8-ID) at the National Synchrotron Light Source II (NSLS-II) is presented. Designed for hard X-ray photon-in/photon-out spectroscopy, the spectrometer achieves a resolution in the 0.5–2 eV range, depending on the element and/or emission line, providing detailed insights into the local electronic and geometric structure of materials. It serves a diverse user community, including fields such as physical, chemical, biological, environmental and materials sciences. This article details the mechanical design, alignment procedures and data-acquisition scheme of the spectrometer, with a particular focus on the continuous asynchronous data-acquisition approach that significantly enhances experimental efficiency. Full Article text
copy Correlative X-ray micro-nanotomography with scanning electron microscopy at the Advanced Light Source By journals.iucr.org Published On :: 2024-10-29 Geological samples are inherently multi-scale. Understanding their bulk physical and chemical properties requires characterization down to the nano-scale. A powerful technique to study the three-dimensional microstructure is X-ray tomography, but it lacks information about the chemistry of samples. To develop a methodology for measuring the multi-scale 3D microstructure of geological samples, correlative X-ray micro- and nanotomography were performed on two rocks followed by scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS) analysis. The study was performed in five steps: (i) micro X-ray tomography was performed on rock sample cores, (ii) samples for nanotomography were prepared using laser milling, (iii) nanotomography was performed on the milled sub-samples, (iv) samples were mounted and polished for SEM analysis and (v) SEM imaging and compositional mapping was performed on micro and nanotomography samples for complimentary information. Correlative study performed on samples of serpentine and basalt revealed multiscale 3D structures involving both solid mineral phases and pore networks. Significant differences in the volume fraction of pores and mineral phases were also observed dependent on the imaging spatial resolution employed. This highlights the necessity for the application of such a multiscale approach for the characterization of complex aggregates such as rocks. Information acquired from the chemical mapping of different phases was also helpful in segmentation of phases that did not exhibit significant contrast in X-ray imaging. Adoption of the protocol used in this study can be broadly applied to 3D imaging studies being performed at the Advanced Light Source and other user facilities. Full Article text
copy Development of hard X-ray photoelectron spectroscopy in liquid cells using optimized microfabricated silicon nitride membranes By journals.iucr.org Published On :: 2024-10-15 We present first hard X-ray photoelectron spectroscopy (HAXPES) results of aqueous salt solutions and dispersions of gold nanoparticles in liquid cells equipped with specially designed microfabricated thin silicon nitride membranes, with thickness in the 15–25 nm range, mounted in a high-vacuum-compatible environment. The experiments have been performed at the HAXPES endstation of the GALAXIES beamline at the SOLEIL synchrotron radiation facility. The low-stress membranes are fabricated from 100 mm silicon wafers using standard lithography techniques. Platinum alignment marks are added to the chips hosting the membranes to facilitate the positioning of the X-ray beam on the membrane by detecting the corresponding photoemission lines. Two types of liquid cells have been used, a static one built on an Omicron-type sample holder with the liquid confined in the cell container, and a circulating liquid cell, in which the liquid can flow in order to mitigate the effects due to beam damage. We demonstrate that the membranes are mechanically robust and able to withstand 1 bar pressure difference between the liquid inside the cell and vacuum, and the intense synchrotron radiation beam during data acquisition. This opens up new opportunities for spectroscopic studies of liquids. Full Article text
copy Foreword to the special virtual issue on X-ray spectroscopy to understand functional materials: instrumentation, applications, data analysis By journals.iucr.org Published On :: 2024-10-21 Full Article text
copy Internet Archive's digital book lending violates copyrights, US judge rules By cio.economictimes.indiatimes.com Published On :: Mon, 27 Mar 2023 07:48:00 +0530 The ruling by U.S. District Judge John Koeltl in Manhattan on Friday came in a closely watched lawsuit that tested the ability of Internet Archive to lend out the works of writers and publishers protected by U.S. copyright laws. Full Article
copy IISc scientists use AI, Raman spectroscopy to detect bacterial pathogen By cio.economictimes.indiatimes.com Published On :: Thu, 29 Dec 2022 08:53:05 +0530 In a new study, Siva Umapathy and Deepak Kumar Saini’s teams have demonstrated another application for this combination: Quickly identifying bacterial pathogens in different types of clinical samples. Full Article
copy Antique Bank Found in Louisiana Flea Market Discovered to Be Never Before Seen Copy of Famous Leonardo Da Vinci Painting - Salvator Mundi By www.24-7pressrelease.com Published On :: Sun, 31 Mar 2024 08:00:00 GMT A mechanical antique metal bank purchased at this year's Ponchatoula, LA's annual Antique day sheds new questions on the origins and story of the world's most expensive work of art, the "Salvator Mundi" painting presumed to be by Leonardo Da Vinci. Full Article
copy 2015 Copy Service Fee Schedule By ww3.workcompcentral.com Published On :: Mon, 15 Jun 2015 16:26:13 -0700 Learn the fundamentals of the new 2015 Copy Service Fee Schedule. Understand how things are defined, what services are bundled, and when services are not payable. This class is important… Full Article
copy Integrated and enhanced datasets on food security and household coping strategies in the G5 Sahel Countries (2018-2023) Copy By africa.ifpri.info Published On :: Tue, 12 Nov 2024 12:54:39 +0000 The objective of this analysis is to gain more insight into the coping behavior of households in Mali when facing covariate shocks and stressors of different kinds Source: IFPRI Africa Regional Office (AFR) Full Article Africa Burkina Faso Chad households Mauritania; New Publication News Publications Sahel climate food security Mali Niger violence
copy Combining X-ray Fluorescence, Infrared Spectroscopy and Software Algorithms for Positive Material and Contaminant Identification By www.qualitymag.com Published On :: Wed, 11 Sep 2024 00:00:00 -0400 FTIR is the primary method for material and contaminant identification but lacks sensitivity to metallic components. X-ray fluorescence (XRF) can fill this gap and improve identification accuracy. Full Article
copy Seeing Further with Digital Microscopy in U.S. Manufacturing By www.qualitymag.com Published On :: Sat, 17 Aug 2024 00:00:00 -0400 In manufacturing, microscopes and magnified viewing systems are crucial for inspecting products. Digital microscopes offer enhanced capabilities and AI-assisted inspections, revolutionizing the way manufacturers view and interact with macro and microscopic details. Full Article
copy Taking Industrial Metrology to the Next Level: Dimensional Measurements with 3D X-ray Microscopy By www.qualitymag.com Published On :: Mon, 23 Sep 2024 00:00:00 -0400 The push for smaller, more complex device components has spiked the need for precise, non-damaging metrology, with 3D X-ray microscopy (XRM) leading the way. This technology offers high-resolution measurements critical for quality control in the electronics and manufacturing industries. Full Article
copy Dukascopy Bank Celebrates 20 Years of Innovation and Stability in Trading and Banking By www.forexlive.com Published On :: Thu, 07 Nov 2024 09:43:16 GMT Since its founding in 2004, Dukascopy has grown into a trusted, innovative leader in the fintech and online trading space, providing clients with advanced tools and a stable platform for smart financial decisions.Over the past 20 years, Dukascopy has reached major milestones that reflect its core values of stability, innovation, and putting clients first. From its proprietary JForex platform to the popular MT4 and MT5, Dukascopy offers a variety of trading platforms along with modern neo-banking services for both individuals, businesses, and institutions. The bank has also led the way in technology upgrades with White Label and banking-as-a-platform solutions.As Dr.Andre Duka, Dukascopy’s founder, says, "Innovation has always been at the heart of what we do. We aim to continue delivering these high standards into the future. Thank you, our clients, for choosing us for these 20 years."Currently, Dukascopy (https://dukascopy.click/agw) proudly serves over 400,000 clients across both trading and banking services. This commitment to delivering cutting-edge solutions, backed by Swiss-grade stability, has allowed the company to maintain long-term relationships with clients, many of whom have been trading and banking with Dukascopy for decades.As the company looks toward the future, Dukascopy remains focused on empowering traders and banking clients, expecting significant growth of its client base across all segments, from trading to neo-banking, corporate to white-label services. This article was written by FL Contributors at www.forexlive.com. Full Article Education
copy News outlets lose copyright lawsuit against OpenAI By www.siliconrepublic.com Published On :: Fri, 08 Nov 2024 09:08:48 +0000 The judge ruled in favour of OpenAI stating that the outlets were unable to prove 'concrete injury'. Read more: News outlets lose copyright lawsuit against OpenAI Full Article Machines legal OpenAI US
copy AI could transform visual effects in film — but the emerging field is mired in copyright issues By thenextweb.com Published On :: Sun, 03 Nov 2024 07:32:07 +0000 While many people in the creative industries are worrying that AI is about to steal their jobs, Oscar-winning film director James Cameron is embracing the technology. Cameron is famous for making the Avatar and Terminator movies, as well as Titanic. Now he has joined the board of Stability.AI, a leading player in the world of Generative AI. In Cameron’s Terminator films, Skynet is an artificial general intelligence that has become self-aware and is determined to destroy the humans who are trying to deactivate it. Forty years after the first of those movies, its director appears to be changing sides and…This story continues at The Next Web Full Article Deep tech Future of work
copy Spectroscopy of polymer nanocomposites By search.lib.uiowa.edu Published On :: Location: Engineering Library- QC463.P5S64 2016 Full Article
copy Nirvana Sued for Copyright Infringement Over 'Dante's Inferno' Illustration By www.aceshowbiz.com Published On :: Wed, 05 May 2021 22:30:02 +0000 The legendary band fronted by the late Kurt Cobain has been slapped with a copyright infringement by C.W. Scott-Giles' family over 'Dante's Inferno' illustration. Full Article music Nirvana Dante's Inferno
copy Meghan Markle Wins Additional Copyright Claim Against U.K. Tabloid Over Letter to Her Father By www.aceshowbiz.com Published On :: Thu, 06 May 2021 02:17:04 +0000 In other news, the Duchess of Sussex is accused of plagiarizing British author Corrinne Averiss and Gabriel Alborozo's 2018 book titled 'The Boy on the Bench' for her yet-to-be released children's book 'The Bench'. Full Article celebrity Meghan Markle
copy Nirvana Sued for Copyright Infringement Over 'Dante's Inferno' Illustration By www.aceshowbiz.com Published On :: Wed, 05 May 2021 22:30:02 +0000 The legendary band fronted by the late Kurt Cobain has been slapped with a copyright infringement by C.W. Scott-Giles' family over 'Dante's Inferno' illustration. Full Article music Nirvana Dante's Inferno
copy Meghan Markle Wins Additional Copyright Claim Against U.K. Tabloid Over Letter to Her Father By www.aceshowbiz.com Published On :: Thu, 06 May 2021 02:17:04 +0000 In other news, the Duchess of Sussex is accused of plagiarizing British author Corrinne Averiss and Gabriel Alborozo's 2018 book titled 'The Boy on the Bench' for her yet-to-be released children's book 'The Bench'. Full Article celebrity Meghan Markle
copy The Birmingham Salon Debate: Have we got copyright wrong? By thebirminghampress.com Published On :: Fri, 31 Aug 2012 08:55:15 +0000 So what do we make of the current copyright regime? Join in the debate at The Ropewalk, 15-20 St. Paul’s Square, Birmingham Full Article Birmingham The Debate Uncategorized What's on Law media
copy 383: ‘A Photocopy of a Fax’, With Jason Snell By daringfireball.net Published On :: Tue, 29 Aug 2023 22:36:45 EDT Jason Snell, come on down. You’re the next contestent on The Talk Show. Special topics: John Warnock and Adobe, Disney and Apple, the iMac’s 25th anniversary, and more. Full Article
copy SteelFox and Rhadamanthys Malware Use Copyright Scams, Driver Exploits to Target Victims By thehackernews.com Published On :: Thu, 07 Nov 2024 15:12:00 +0530 An ongoing phishing campaign is employing copyright infringement-related themes to trick victims into downloading a newer version of the Rhadamanthys information stealer since July 2024. Cybersecurity firm Check Point is tracking the large-scale campaign under the name CopyRh(ight)adamantys. Targeted regions include the United States, Europe, East Asia, and South America. "The campaign Full Article