2016-04-02Having accurate and comprehensive photon diagnostics for the X-ray pulses delivered by free-electron laser (FEL) facilities is of utmost importance. Along with various parameters of the photon beam (such as photon energy, beam intensity, etc.), the pulse length measurements are particularly useful both for the machine operators to measure the beam parameters and monitor the stability of the machine performance, and for the users carrying out pump–probe experiments at such facilities to better understand their measurement results. One of the most promising pulse length measurement techniques used for photon diagnostics is the THz streak camera which is capable of simultaneously measuring the lengths of the photon pulses and their arrival times with respect to the pump laser. This work presents simulations of a THz streak camera performance. The simulation procedure utilizes FEL pulses with two different photon energies in hard and soft X-ray regions, respectively. It recreates the energy spectra of the photoelectrons produced by the photon pulses and streaks them by a single-cycle THz pulse. Following the pulse-retrieval procedure of the THz streak camera, the lengths were calculated from the streaked spectra. To validate the pulse length calculation procedure, the precision and the accuracy of the method were estimated for streaking configuration corresponding to previously performed experiments. The obtained results show that for the discussed setup the method is capable of measuring FEL pulses with about a femtosecond accuracy and precision.
2016-04-02The design and the first experiments are described of a versatile cryogenic insert used for its electrical transport capabilities. The insert is designed for the cryomagnet installed on the DEIMOS beamline at the SOLEIL synchrotron dedicated to magnetic characterizations through X-ray absorption spectroscopy (XAS) measurements. This development was spurred by the multifunctional properties of novel materials such as multiferroics, in which, for example, the magnetic and electrical orders are intertwined and may be probed using XAS. The insert thus enables XAS to in situ probe this interplay. The implementation of redundant wiring and careful shielding also enables studies on operating electronic devices. Measurements on magnetic tunnel junctions illustrate the potential of the equipment toward XAS studies of in operando electronic devices.
2016-04-19Hard X-ray Fabry–Perot resonators (FPRs) made from sapphire crystals were constructed and characterized. The FPRs consisted of two crystal plates, part of a monolithic crystal structure of Al2O3, acting as a pair of mirrors, for the backward reflection (0 0 0 30) of hard X-rays at 14.3147 keV. The dimensional accuracy during manufacturing and the defect density in the crystal in relation to the resonance efficiency of sapphire FPRs were analyzed from a theoretical standpoint based on X-ray cavity resonance and measurements using scanning electron microscopic and X-ray topographic techniques for crystal defects. Well defined resonance spectra of sapphire FPRs were successfully obtained, and were comparable with the theoretical predictions.
2016-04-20An open-source database containing metrology data for X-ray mirrors is presented. It makes available metrology data (mirror heights and slopes profiles) that can be used with simulation tools for calculating the effects of optical surface errors in the performances of an optical instrument, such as a synchrotron beamline. A typical case is the degradation of the intensity profile at the focal position in a beamline due to mirror surface errors. This database for metrology (DABAM) aims to provide to the users of simulation tools the data of real mirrors. The data included in the database are described in this paper, with details of how the mirror parameters are stored. An accompanying software is provided to allow simple access and processing of these data, calculate the most usual statistical parameters, and also include the option of creating input files for most used simulation codes. Some optics simulations are presented and discussed to illustrate the real use of the profiles from the database.
2016-04-19Small-angle scattering X-ray photon correlation spectroscopy (XPCS) studies were performed using a novel photon-counting pixel array detector with dual counters for each pixel. Each counter can be read out independently from the other to ensure there is no readout dead-time between the neighboring frames. A maximum frame rate of 11.8 kHz was achieved. Results on test samples show good agreement with simple diffusion. The potential of extending the time resolution of XPCS beyond the limit set by the detector frame rate using dual counters is also discussed.
2016-03-24The short pulse duration, small effective source size and high flux of synchrotron radiation is ideally suited for probing a wide range of transient deformation processes in materials under extreme conditions. In this paper, the challenges of high-resolution time-resolved indirect X-ray detection are reviewed in the context of dynamic synchrotron experiments. In particular, the discussion is targeted at two-dimensional integrating detector methods, such as those focused on dynamic radiography and diffraction experiments. The response of a scintillator to periodic synchrotron X-ray excitation is modelled and validated against experimental data collected at the Diamond Light Source (DLS) and European Synchrotron Radiation Facility (ESRF). An upper bound on the dynamic range accessible in a time-resolved experiment for a given bunch separation is calculated for a range of scintillators. New bunch structures are suggested for DLS and ESRF using the highest-performing commercially available crystal LYSO:Ce, allowing time-resolved experiments with an interframe time of 189 ns and a maximum dynamic range of 98 (6.6 bits).
2016-04-20When studying electro-mechanical materials, observing the structural changes during the actuation process is necessary for gaining a complete picture of the structure–property relationship as certain mechanisms may be meta-stable during actuation. In situ diffraction methods offer a powerful and direct means of quantifying the structural contributions to the macroscopic strain of these materials. Here, a sample cell is demonstrated capable of measuring the structural variations of electro-mechanical materials under applied electric potentials up to 10 kV. The cell is designed for use with X-ray scattering techniques in reflection geometry, while simultaneously collecting macroscopic strain data using a linear displacement sensor. The results show that the macroscopic strain measured using the cell can be directly correlated with the microscopic response of the material obtained from diffraction data. The capabilities of the cell have been successfully demonstrated at the Powder Diffraction beamline of the Australian Synchrotron and the potential implementation of this cell with laboratory X-ray diffraction instrumentation is also discussed.
2016-04-14The slicing facility FemtoSpeX at BESSY II offers unique opportunities to study photo-induced dynamics on femtosecond time scales by means of X-ray magnetic circular dichroism, resonant and non-resonant X-ray diffraction, and X-ray absorption spectroscopy experiments in the soft X-ray regime. Besides femtosecond X-ray pulses, slicing sources inherently also produce a so-called `halo' background with a different time structure, polarization and pointing. Here a detailed experimental characterization of the halo radiation is presented, and a method is demonstrated for its correct and unambiguous removal from femtosecond time-resolved data using a special laser triggering scheme as well as analytical models. Examples are given for time-resolved measurements with corresponding halo correction, and errors of the relevant physical quantities caused by either neglecting or by applying a simplified model to describe this background are estimated.
2016-03-30Dynamic compression experiments are performed on single-crystal Si under split Hopkinson pressure bar loading, together with simultaneous high-speed (250–350 ns resolution) synchrotron X-ray Laue diffraction and phase-contrast imaging. A methodology is presented which determines crystal rotation parameters, i.e. instantaneous rotation axes and angles, from two unindexed Laue diffraction spots. Two-dimensional translation is obtained from dynamic imaging by a single camera. High-speed motion of crystals, including translation and rotation, can be tracked in real time via simultaneous imaging and diffraction.
2016-04-01Silver nanoparticles were synthesized with a chemical reduction method in the presence of polyvinylpyrrolidone as stabilizing agent. The thermal stability behavior of the silver nanoparticles was studied in the temperature range from 25 to 700°C. Thermal gravimetric analysis was used to measure the weight loss of the silver nanoparticles. Scanning electron microscopy and high-resolution transmission electron microscopy were used to observe the morphology and the change in shape of the silver nanoparticles. In situ temperature-dependent small-angle X-ray scattering was used to detect the increase in particle size with temperature. In situ temperature-dependent X-ray diffraction was used to characterize the increase in nanocrystal size and the thermal expansion coefficient. The results demonstrate that sequential slow and fast Ostward ripening are the main methods of nanoparticle growth at lower temperatures (<500°C), whereas successive random and directional coalescences are the main methods of nanoparticle growth at higher temperatures (>500°C). A four-stage model can be used to describe the whole sintering process. The thermal expansion coefficient (2.8 × 10−5 K−1) of silver nanoparticles is about 30% larger than that of bulk silver. To our knowledge, the temperature-driven directional coalescence of silver nanocrystals is reported for the first time. Two possible mechanisms of directional coalescence have been proposed. This study is of importance not only in terms of its fundamental academic interest but also in terms of the thermal stability of silver nanoparticles.
2016-04-20Dynamical scattering effects are observed in grazing-incidence X-ray diffraction experiments using an organic thin film of 2,2′:6′,2′′-ternaphthalene grown on oxidized silicon as substrate. Here, a splitting of all Bragg peaks in the out-of-plane direction (z-direction) has been observed, the magnitude of which depends both on the incidence angle of the primary beam and the out-of-plane angle of the scattered beam. The incident angle was varied between 0.09° and 0.25° for synchrotron radiation of 10.5 keV. This study reveals comparable intensities of the split peaks with a maximum for incidence angles close to the critical angle of total external reflection of the substrate. This observation is rationalized by two different scattering pathways resulting in diffraction peaks at different positions at the detector. In order to minimize the splitting, the data suggest either using incident angles well below the critical angle of total reflection or angles well above, which sufficiently attenuates the contributions from the second scattering path. This study highlights that the refraction of X-rays in (organic) thin films has to be corrected accordingly to allow for the determination of peak positions with sufficient accuracy. Based thereon, a reliable determination of the lattice constants becomes feasible, which is required for crystallographic structure solutions from thin films.
2016-04-01An angle-resolved linearly polarized hard X-ray photoemission spectroscopy (HAXPES) system has been developed to study the ground-state symmetry of strongly correlated materials. The linear polarization of the incoming X-ray beam is switched by a transmission-type phase retarder composed of two diamond (100) crystals. The best value of the degree of linear polarization was found to be −0.96, containing a vertical polarization component of 98%. A newly developed low-temperature two-axis manipulator enables easy polar and azimuthal rotations to select the detection direction of photoelectrons. The lowest temperature achieved was 9 K, offering the chance to access the ground state even for strongly correlated electron systems in cubic symmetry. A co-axial sample monitoring system with long-working-distance microscope enables the same region on the sample surface to be measured before and after rotation. Combining this sample monitoring system with a micro-focused X-ray beam by means of an ellipsoidal Kirkpatrick–Baez mirror (25 µm × 25 µm FWHM), polarized valence-band HAXPES has been performed on NiO for voltage application as resistive random access memory to demonstrate the micro-positioning technique and polarization switching.
2016-04-14The design and operation of a low-volume spectroelectrochemical cell for X-ray absorption spectroscopy (XAS) of solutions at room temperature is described. Fluorescence XAS measurements are obtained from samples contained in the void space of a 50 µL reticulated vitreous carbon (sponge) working electrode. Both rapid electrosynthesis and control of the effects of photoreduction are achieved by control over the flow properties of the solution through the working electrode, where a good balance between the rate of consumption of sample and the minimization of decomposition was obtained by pulsing the flow of the solution by 1–2 µL with duty cycle of ∼3 s while maintaining a small net flow rate (26–100 µL h−1). The performance of the cell in terms of control of the redox state of the sample and minimization of the effects of photoreduction was demonstrated by XAS measurements of aqueous solutions of the photosensitive FeIII species, [Fe(C2O4)3]3−, together with that of the electrogenerated [Fe(C2O4)3]4− product. The current response from the cell during the collection of XAS spectra provides an independent measure of the stability of the sample of the measurement. The suitability of the approach for the study of small volumes of mM concentrations of protein samples was demonstrated by the measurement of the oxidized and electrochemically reduced forms of cytochrome c.
2016-04-19A simple scheme to quickly switch the polarity of circular radiation is proposed, which is based on spectrum splitting of undulator radiation. In this scheme, two helical undulators with opposite helicities are placed tandem in one straight section, both of which are divided into several segments. The optical phases between segments are tuned so that light waves from one of the two undulators are out of phase, while those from the other are in phase. Then the radiation spectrum of the former is split and the intensity at the fundamental photon energy vanishes. As a consequence, the monochromated photon beam at the fundamental energy is circularly polarized with the helicity specified by the in-phase undulator, which can be quickly flipped by tuning the optical phase. Numerical calculations carried out to demonstrate the feasibility of the proposed scheme show that a relatively high degree of circular polarization is expected if the angular acceptance of the beamline is not too large.
2016-03-24Obtaining structural information of uranyl species at an atomic/molecular scale is a critical step to control and predict their physical and chemical properties. To obtain such information, experimental and theoretical L3-edge X-ray absorption near-edge structure (XANES) spectra of uranium were studied systematically for uranyl complexes. It was demonstrated that the bond lengths (R) in the uranyl species and relative energy positions (ΔE) of the XANES were determined as follows: ΔE1 = 168.3/R(U—Oax)2 − 38.5 (for the axial plane) and ΔE2 = 428.4/R(U—Oeq)2 − 37.1 (for the equatorial plane). These formulae could be used to directly extract the distances between the uranium absorber and oxygen ligand atoms in the axial and equatorial planes of uranyl ions based on the U L3-edge XANES experimental data. In addition, the relative weights were estimated for each configuration derived from the water molecule and nitrate ligand based on the obtained average equatorial coordination bond lengths in a series of uranyl nitrate complexes with progressively varied nitrate concentrations. Results obtained from XANES analysis were identical to that from extended X-ray absorption fine-structure (EXAFS) analysis. XANES analysis is applicable to ubiquitous uranyl–ligand complexes, such as the uranyl–carbonate complex. Most importantly, the XANES research method could be extended to low-concentration uranyl systems, as indicated by the results of the uranyl–amidoximate complex (∼40 p.p.m. uranium). Quantitative XANES analysis, a reliable and straightforward method, provides a simplified approach applied to the structural chemistry of actinides.
2016-04-14A new concept that comprises both time- and lateral-resolved X-ray absorption fine-structure information simultaneously in a single shot is presented. This uncomplicated set-up was tested at the BAMline at BESSY-II (Berlin, Germany). The primary broadband beam was generated by a double multilayer monochromator. The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by either an energy-sensitive area detector, the so-called color X-ray camera, or by an area-sensitive detector based on a CCD camera, in θ–2θ geometry. The first tests were performed with thin metal foils and some iron oxide mixtures. A time resolution of lower than 1 s together with a spatial resolution in one dimension of at least 50 µm is achieved.
2016-03-23Dental burs are used extensively in dentistry to mechanically prepare tooth structures for restorations (fillings), yet little has been reported on the bur debris left behind in the teeth, and whether it poses potential health risks to patients. Here it is aimed to image dental bur debris under dental fillings, and allude to the potential health hazards that can be caused by this debris when left in direct contact with the biological surroundings, specifically when the debris is made of a non-biocompatible material. Non-destructive micro-computed tomography using the BioMedical Imaging & Therapy facility 05ID-2 beamline at the Canadian Light Source was pursued at 50 keV and at a pixel size of 4 µm to image dental bur fragments under a composite resin dental filling. The bur's cutting edges that produced the fragment were also chemically analyzed. The technique revealed dental bur fragments of different sizes in different locations on the floor of the prepared surface of the teeth and under the filling, which places them in direct contact with the dentinal tubules and the dentinal fluid circulating within them. Dispersive X-ray spectroscopy elemental analysis of the dental bur edges revealed that the fragments are made of tungsten carbide–cobalt, which is bio-incompatible.
2016-04-12A new multi-platform freeware has been developed for the processing and reconstruction of scanning multi-technique X-ray imaging and tomography datasets. The software platform aims to treat different scanning imaging techniques: X-ray fluorescence, phase, absorption and dark field and any of their combinations, thus providing an easy-to-use data processing tool for the X-ray imaging user community. A dedicated data input stream copes with the input and management of large datasets (several hundred GB) collected during a typical multi-technique fast scan at the Nanoscopium beamline and even on a standard PC. To the authors' knowledge, this is the first software tool that aims at treating all of the modalities of scanning multi-technique imaging and tomography experiments.
2016-04-12The hydraulic efficiency of a leaf depends on its vascular structure as this is responsible for transport activities. To investigate the effect of exclusion of UVAB and UVB radiation from the solar spectrum on the micro-structure of leaves of soybean (Glycine max, variety JS-335), a field experiment was conducted using synchrotron-based phase contrast imaging (PCI). Plants were grown in specially designed UV exclusion chambers, and wrapped with filters that excluded UVB (280–315 nm) or UVAB (280–400 nm), or transmitted all the ambient solar UV (280–400 nm) radiation (filter control). Qualitative observation of high-resolution X-ray PCI images obtained at 10 keV has shown the differences in major and minor vein structures of the leaves. The mid-rib width of the middle leaflet of third trifoliate leaves, for all treatments, were obtained using quantitative image analysis. The width of the mid-rib of the middle leaflet of third trifoliate leaves of UVB excluded plants was found to be more compared to leaves of filter control plants, which are exposed to ambient UV. The mid-rib or the main conducting vein transports water and sugars to the whole plant; therefore, mid-rib enhancement by the exclusion of solar UV radiation possibly implies enhancement in the leaf area which in turn causes an increased rate of photosynthesis.
2016-04-14Synchrotron radiation inline phase-contrast imaging combined with computed tomography (SR-inline-PCI-CT) offers great potential for non-invasive characterization and three-dimensional visualization of fine features in weakly absorbing materials and tissues. For cartilage tissue engineering, the biomaterials and any associated cartilage extracellular matrix (ECM) that is secreted over time are difficult to image using conventional absorption-based imaging techniques. For example, three-dimensional printed polycaprolactone (PCL)/alginate/cell hybrid constructs have low, but different, refractive indices and thicknesses. This paper presents a study on the optimization and utilization of inline-PCI-CT for visualizing the components of three-dimensional printed PCL/alginate/cell hybrid constructs for cartilage tissue engineering. First, histological analysis using Alcian blue staining and immunofluorescent staining assessed the secretion of sulfated glycosaminoglycan (GAGs) and collagen type II (Col2) in the cell-laden hybrid constructs over time. Second, optimization of inline PCI-CT was performed by investigating three sample-to-detector distances (SDD): 0.25, 1 and 3 m. Then, the optimal SDD was utilized to visualize structural changes in the constructs over a 42-day culture period. The results showed that there was progressive secretion of cartilage-specific ECM by ATDC5 cells in the hybrid constructs over time. An SDD of 3 m provided edge-enhancement fringes that enabled simultaneous visualization of all components of hybrid constructs in aqueous solution. Structural changes that might reflect formation of ECM also were evident in SR-inline-PCI-CT images. Summarily, SR-inline-PCI-CT images captured at the optimized SDD enables visualization of the different components in hybrid cartilage constructs over a 42-day culture period.
2016-04-16Amyloid beta accumulation into insoluble plaques (Aβp) is known to play a significant role in the pathological process in Alzheimer's disease (AD). The presence of Aβp is also one of the neuropathological hallmarks for the disease. AD final diagnosis is generally acknowledged after the evaluation of Aβp deposition in the brain. Insoluble Aβp accumulation may also concur to cause AD as postulated in the so-called amyloid hypothesis. Therefore, the visualization, evaluation and quantification of Aβp are nowadays the keys for a better understanding of the disease, which may point to a possible cure for AD in the near future. Synchrotron-based X-ray phase contrast (XPC) has been demonstrated as the only imaging method that can retrieve the Aβp signal with high spatial resolution (up to 10 µm), high sensitivity and three-dimensional information at the same time. Although at the moment XPC is suitable for ex vivo samples only, it may develop into an alternative to positron emission tomography and magnetic resonance imaging in Aβp imaging. In this contribution the possibility of using synchrotron-based X-ray phase propagation computed tomography to visualize and measure Aβp on mouse brains is presented. A careful setup optimization for this application leads to a significant improvement of spatial resolution (∼1 µm), data acquisition speed (five times faster), X-ray dose (five times lower) and setup complexity, without a substantial loss in sensitivity when compared with the classic implementation of grating-based X-ray interferometry.
2016-03-23An automatic sample changer chamber for total reflection X-ray fluorescence (TXRF) and X-ray absorption near-edge structure (XANES) analysis in TXRF geometry was successfully set up at the BAMline at BESSY II. TXRF and TXRF-XANES are valuable tools for elemental determination and speciation, especially where sample amounts are limited (<1 mg) and concentrations are low (ng ml−1 to µg ml−1). TXRF requires a well defined geometry regarding the reflecting surface of a sample carrier and the synchrotron beam. The newly installed chamber allows for reliable sample positioning, remote sample changing and evacuation of the fluorescence beam path. The chamber was successfully used showing accurate determination of elemental amounts in the certified reference material NIST water 1640. Low limits of detection of less than 100 fg absolute (10 pg ml−1) for Ni were found. TXRF-XANES on different Re species was applied. An unknown species of Re was found to be Re in the +7 oxidation state.
2016-03-23The diffraction beamline BM01A at the European Synchrotron Radiation Facility (CRG Swiss–Norwegian beamlines) has been successfully operational for 20 years. Recently, a new multifunctional diffractometer based on the Dectris Pilatus 2M detector has been constructed, commissioned and offered to users. The diffractometer combines a fast and low-noise area detector, which can be tilted and moved horizontally and vertically, together with flexible goniometry for sample positioning and orientation. The diffractometer is controlled by a user-friendly and GUI-based software Pylatus which is also used to control various auxiliary equipment. The latter includes several heating and cooling devices, in situ cells and complimentary spectroscopic tools.
2016-04-14The implementation of a laser pump/X-ray probe scheme for performing picosecond-resolution X-ray diffraction at the 1W2B wiggler beamline at Beijing Synchrotron Radiation Facility is reported. With the hybrid fill pattern in top-up mode, a pixel array X-ray detector was optimized to gate out the signal from the singlet bunch with interval 85 ns from the bunch train. The singlet pulse intensity is ∼2.5 × 106 photons pulse−1 at 10 keV. The laser pulse is synchronized to this singlet bunch at a 1 kHz repetition rate. A polycapillary X-ray lens was used for secondary focusing to obtain a 72 µm (FWHM) X-ray spot. Transient photo-induced strain in BiFeO3 film was observed at a ∼150 ps time resolution for demonstration.
2016-04-16This paper gives a detailed description, including equations, of the Johann-type X-ray emission spectrometer which has been recently installed and tested at the Rossendorf beamline (ROBL) of the European Synchrotron Radiation Facility. The spectrometer consists of a single spherically bent crystal analyzer and an avalanche photodiode detector positioned on the vertical Rowland cycle of 1 m diameter. The hard X-ray emission spectrometer (∼3.5–25 keV) operates at atmospheric pressure and covers the Bragg angles of 65°–89°. The instrument has been tested at high and intermediate incident energies, i.e. at the Zr K-edge and at the Au L3-edge, in the second experimental hutch of ROBL. The spectrometer is dedicated for studying actinides in materials and environmental samples by high-energy-resolution X-ray absorption and X-ray emission spectroscopies.
2016-04-28The processing of tomographic synchrotron data requires advanced and efficient software to be able to produce accurate results in reasonable time. In this paper, the integration of two software toolboxes, TomoPy and the ASTRA toolbox, which, together, provide a powerful framework for processing tomographic data, is presented. The integration combines the advantages of both toolboxes, such as the user-friendliness and CPU-efficient methods of TomoPy and the flexibility and optimized GPU-based reconstruction methods of the ASTRA toolbox. It is shown that both toolboxes can be easily installed and used together, requiring only minor changes to existing TomoPy scripts. Furthermore, it is shown that the efficient GPU-based reconstruction methods of the ASTRA toolbox can significantly decrease the time needed to reconstruct large datasets, and that advanced reconstruction methods can improve reconstruction quality compared with TomoPy's standard reconstruction method.
2016-04-28A correction is made to a citation in the article by Antipov et al. (2016) [J. Synchrotron Rad. 23, 163–168].