Journal of Synchrotron Radiation最新文献

Modern inelastic X-ray spectrometers employ curved, bent and diced analyzers to capture sufficiently large solid angles of radially emitted scattered radiation emanating from the sample. Fabricating these intricate analyzers, especially when a high energy resolution of a few millielectronvolts is required, is very time-consuming, expensive and often a hit-or-miss affair. A novel fabrication technique is introduced, utilizing a concave-spherical, microporous aluminium base to hold an assembly of a thin glass substrate with a diced crystal wafer bonded to it. Under uniform vacuum forces, the glass substrate is drawn into the aluminium base, achieving the desired bending radius, while dicing of the diffracting crystal layer prevents bending strain from being imposed on the individual crystal pixels. This technique eliminates the need for permanently bonding the crystal assembly to the concave lens, offering the opportunity for correcting figure errors, avoiding long-term degradation of the permanent bond, and making both lens and crystal reusable. Process and material costs are thus substantially decreased. Two analyzers, Si(844) and Ge(337) with intrinsic resolutions of 14.6 meV and 36.5 meV, respectively, were produced in this fashion and characterized in resonant inelastic X-ray scattering (RIXS) measurements. The achieved overall energy resolutions for both analyzers were 29.4 meV for Si(844) and 56.6 meV for Ge(337). Although the RIXS technique is veru sensitive to analyzer imperfections, the analyzers were found to be equal, if not superior, in quality to their traditional, permanently bonded counterparts.

A set of electron time-of-flight spectrometers for high-resolution angle-resolved spectroscopy was developed for the Small Quantum Systems (SQS) instrument at the SASE3 soft X-ray branch of the European XFEL. The resolving power of this spectrometer design is demonstrated to exceed 10 000 (E/ΔE), using the well known Ne 1s^-13p resonant Auger spectrum measured at a photon energy of 867.11 eV at a third-generation synchrotron radiation source. At the European XFEL, a width of ∼0.5 eV full width at half-maximum for a kinetic energy of 800 eV was demonstrated. It is expected that this linewidth can be reached over a broad range of kinetic energies. An array of these spectrometers, with different angular orientations, is tailored for the Atomic-like Quantum Systems endstation for high-resolution angle-resolved spectroscopy of gaseous samples.

Complex dynamic tomographic experiments at brilliant X-ray light sources require real-time feedback on the sample changes with respect to environmental conditions, selecting representative regions of interest for high-resolution scanning, and on-demand data saving mechanisms for storing only relevant projections acquired by fast area detectors and reducing data volumes. Here the implementation details of a 3D real-time imaging monitoring instrument, with zooming to a volume of interest with easy-to-use visualization via ImageJ, a tool familiar to most beamline users, is presented. The instrument relies on optimized data flow between the detector and processing machines and is implemented on commodity computers. The instrument has been developed at beamline 2-BM of the Advanced Photon Source, where the automatic lens changing mechanism for zooming is implemented with an Optique Peter microscope. Performance tests demonstrate the ability to process more than 3 GB of projection data per second and generate real-time 3D zooming with different magnification. These new capabilities are essential for new APS Upgrade instruments such as the projection microscope under development at beamline 32-ID. The efficacy of the proposed instrument was demonstrated during an in situ tomographic experiment on ice and gas hydrate formation in porous samples.

X-ray nano-tomography with phase contrast (nanoCT) using synchrotron radiation is a powerful tool to non-destructively investigate 3D material properties at the nanoscale. In large bone lesions, such as severe bone fractures, bone cancer or other diseases, bone grafts substituting the lost bone might be necessary. Such grafts can be of biological origin or be composed of a synthetic bone substitute. The long-term functioning of artificial bone substitutes depends on many factors. Synchrotron nanoCT imaging has great potential to contribute to further the understanding of integration of implants into bone tissue by imaging the spatial interaction between bone tissue and implant, and by accessing the interface between implant material and bone tissue. With this aim, a methodology for evaluating the image quality is presented for in-line phase contrast nanoCT images of bone scaffold samples. A PMMA-embedded tricalcium phosphate scaffold was used with both a closed and an open porosity structure and bone ingrowths as a representative system of three known materials. Parameters such as spatial resolution and signal-to-noise ratio were extracted and used to explore and quantitatively compare the effects of implementation choices in the imaging setup, such as camera technology and imaging energy, on the resulting image quality. Increasing the X-ray energy from 17.5 keV to 29.6 keV leads to a notable improvement in image quality regardless of the camera technology used, with the two tested camera setups performing at a comparable level when the recorded intensity was kept constant.

An in situ synchrotron experimental study of phase formation dynamics in clad mechanocomposites of Ti-Al systems during high-temperature synthesis was performed. Cladding of the obtained mechanocomposites was carried out with an SiO₂ target, with a deposition time of 40 min. The high-temperature synthesis was performed using the thermal explosion method based on a microwave induction heater in the in situ mode on an experimental setup adapted to synchrotron radiation time-resolved diffractometry. The influence of the cladding on the macrokinetic parameters of synthesis in situ was investigated experimentally. It was found that for an ignition temperature T_ig = 650 ± 10°C, the maximum synthesis temperatures were in the range T_max = 1380-1465°C. The characteristic heating speed was 525 K min^-1. The sequence and temperature-time interval of phase formation are determined. The formation of the TiAl, TiAl₃ and Ti₃Al compounds begins at T = 661°C. At T_max = 1465.6°C, the synthesis product is multiphase, the structures of the formed TiAl₃ (content about 70%) and TiAl (content about 25%) have a nonequilibrium state. At the stage of system annealing with T = 1384.9°C, the reaction of the components occurs with the formation of almost monophase TiAl (content of more than 90%); Ti occupies the rest.

X-ray free-electron lasers (XFELs) deliver pulses of coherent X-rays on the femtosecond time scale, with potentially high repetition rates. While XFELs provide high peak intensities, both the intensity and the centroid of the beam fluctuate strongly on a pulse-to-pulse basis, motivating high-rate beam diagnostics that operate over a large dynamic range. The fast drift velocity, low X-ray absorption and high radiation tolerance properties of chemical vapour deposition diamonds make these crystals a promising candidate material for developing a fast (multi-GHz) pass-through diagnostic for the next generation of XFELs. A new approach to the design of a diamond sensor signal path is presented, along with associated characterization studies performed in the XPP endstation of the LINAC Coherent Light Source (LCLS) at SLAC. Qualitative charge collection profiles (collected charge versus time) are presented and compared with those from a commercially available detector. Quantitative results on the charge collection efficiency and signal collection times are presented over a range of approximately four orders of magnitude in the generated electron-hole plasma density.

A novel experimental setup dedicated to the study of liquid and amorphous materials, on the white beam station of the PSICHÉ beamline at SOLEIL, is described. The Beer-Lambert absorption method has been developed using a broad-spectrum (white) incident beam for in situ density measurements at extreme conditions of pressure and temperature. This technique has been combined with other existing X-ray techniques (radiographic imaging, tomography and combined angle energy dispersive X-ray diffraction). Such a multi-technical approach offers new possibilities for the characterization of liquid and amorphous materials at high pressure and high temperature. The strength of this approach is illustrated by density measurements of liquid gallium at pressures up to 4 GPa, combining the three independent X-ray techniques (the Beer-Lambert absorption method, tomography and X-ray diffraction).

A simple spectrometer using diffraction from diamond microcrystals has been developed to diagnose single-shot spectra of X-ray free-electron laser (XFEL) pulses. The large grain size and uniform lattice constant of the adopted crystals enable characterizing the XFEL spectrum at a resolution of a few eV from the peak shape of the powder diffraction profile. This single-shot spectrometer has been installed at beamline 3 of SACLA and is used for daily machine tuning.

Resonant inelastic X-ray scattering in the XUV-regime has been implemented at BESSY II, pushing for a few-meV bandwidth in inelastic X-ray scattering at transition metal M-edges, rare earth N-edges and the K-edges of light elements up to carbon with full polarization control. The new dedicated low-energy beamline UE112-PGM1 has been designed to provide 1 µm vertical and 20 µm horizontal beam dimensions that serve together with sub-micrometre solid-state sample positioning as the source point for a high-resolution plane grating spectrometer and a high-transmission Rowland spectrometer for rapid overview spectra. The design and commissioning results of the beamline and high-resolution spectrometer are presented. Helium autoionization spectra demonstrate a resolving power of the beamline better than 10 000 at 64 eV with a 300 lines mm^-1 grating while the measured resolving power of the spectrometer in the relevant energy range is 3000 to 6000.

Serial crystallography of membrane proteins often employs high-viscosity injectors (HVIs) to deliver micrometre-sized crystals to the X-ray beam. Typically, the carrier medium is a lipidic cubic phase (LCP) media, which can also be used to nucleate and grow the crystals. However, despite the fact that the LCP is widely used with HVIs, the potential impact of the injection process on the LCP structure has not been reported and hence is not yet well understood. The self-assembled structure of the LCP can be affected by pressure, dehydration and temperature changes, all of which occur during continuous flow injection. These changes to the LCP structure may in turn impact the results of X-ray diffraction measurements from membrane protein crystals. To investigate the influence of HVIs on the structure of the LCP we conducted a study of the phase changes in monoolein/water and monoolein/buffer mixtures during continuous flow injection, at both atmospheric pressure and under vacuum. The reservoir pressure in the HVI was tracked to determine if there is any correlation with the phase behaviour of the LCP. The results indicated that, even though the reservoir pressure underwent (at times) significant variation, this did not appear to correlate with observed phase changes in the sample stream or correspond to shifts in the LCP lattice parameter. During vacuum injection, there was a three-way coexistence of the gyroid cubic phase, diamond cubic phase and lamellar phase. During injection at atmospheric pressure, the coexistence of a cubic phase and lamellar phase in the monoolein/water mixtures was also observed. The degree to which the lamellar phase is formed was found to be strongly dependent on the co-flowing gas conditions used to stabilize the LCP stream. A combination of laboratory-based optical polarization microscopy and simulation studies was used to investigate these observations.