Synchrotron Radiation Research Articles

Resonant photoemission studies on Fe-Ni alloys

This paper investigates the electronic structure of Fe1−xNix (x = 0.32, 0.36, 0.4, 0.5) alloys employing high resolution photoelectron spectroscopy using synchrotron radiation. The valence bands and the core levels have been recorded at various on-resonance and off-resonance photon energies of Fe and Ni. An anti-resonance dip observed in the valence bands taken at Fe 3p → 3d resonance lies closer to the Fermi level compared to that observed at Ni 3p → 3d resonance, indicating larger density of itinerant Fe 3d electrons. Whereas, Ni 3d states are comparatively less itinerant in these alloys. The hybridization effects increase with increase of Fe content in the alloy system. The intensity of Ni L3M4,5M4,5 Coster-Cronig Auger transition observed with 853 eV (Ni 2p → 3d resonance) photon energy, drops down drastically for the Invar alloy (Fe0.64Ni0.36) as compared to other Fe-Ni alloys due to the existence of Ni in more than one local chemical surroundings as expected for Invar alloy. The electron-electron interaction energy (Udd) of Ni 3d shell is found to decrease with the decrease of Ni concentration. The 3p and 3s core levels of Fe and Ni recorded at 707 eV (Fe 2p → 3d resonance) are overwhelmed by various intense resonant Auger features such as Fe L3M2,3M2,3, Fe L3M2,3M4,5 and Fe L3M1M4,5. The 1S state of Fe L3M2,3M2,3 is greatly enhanced in the Invar alloy as compared to other alloys. The microscopic compositional in-homogeneity present in Invar alloy plays a crucial role in the screening of holes in Ni sites but does not contribute in screening the holes in Fe sites.

Advanced mapping of inorganic treatments on porous carbonate stones by combined synchrotron radiation high lateral μXRPD and μXRF

Understanding the effects of consolidating inorganic mineral treatments on carbonate stones of cultural heritage, and on the nature and distribution of newly formed products within the matrix, poses a significant challenge in Heritage Science and Conservation Science. Existing analytical methods often fail to deliver spatial and compositional insights into the newly formed crystalline phases with the appropriate high lateral resolution. In this study, we explore the capabilities and limitations of synchrotron radiation (SR) micro-X-ray powder diffraction (μXRPD) mapping combined with micro-X-ray fluorescence (μXRF) to give insight into compounds formed following the application of ammonium oxalate (AmOx) and diammonium phosphate-based (DAP) solutions on porous carbonate stone. Ultimately, the integration of μXRPD mapping and μXRF analysis proved itself a powerful asset in providing precise qualitative and quantitative data on the newly formed phases, in the case of both calcium oxalates (CaOxs) and calcium phosphates (CaPs), and their complex stratigraphic distribution, thus opening a new route for applications to a more comprehensive study of inorganic treatments applied to carbonate substrates.

Evaluation of the X-ray/EUV Nanolithography Facility at AS through wavefront propagation simulations.

Synchrotron light sources can provide the required spatial coherence, stability and control to support the development of advanced lithography at the extreme ultraviolet and soft X-ray wavelengths that are relevant to current and future fabricating technologies. Here an evaluation of the optical performance of thesoft X-ray (SXR) beamline of the Australian Synchrotron (AS) and its suitability for developing interference lithography using radiation in the 91.8 eV (13.5 nm) to 300 eV (4.13 nm) range are presented. A comprehensive physical optics model of the APPLE-II undulator source and SXR beamline was constructed to simulate the properties of the illumination at the proposed location of a photomask, as a function of photon energy, collimation and monochromator parameters. The model is validated using a combination of experimental measurements of the photon intensity distribution of the undulator harmonics. It is shown that the undulator harmonics intensity ratio can be accurately measured using an imaging detector and controlled using beamline optics. Finally, the photomask geometric constraints and achievable performance for the limiting case of fully spatially coherent illumination are evaluated.

Severe perturbation and observation of forbidden transitions in asymmetrically deuterated methanol (CHD2OH) and atlas of very accurate torsional rotational spectrum obtained using Synchrotron radiation

High-resolution spectral studies have been continued for the doubly deuterated methanol species (CHD2OH) in the entire region from far infrared (FIR) to Infrared (IR). The spectrum has been obtained using a conventional Fourier transform spectrometer and the state-of-the-art Synchrotron radiation-based spectrometer with unprecedented resolution and very high signal-to-noise (S/N). During the investigation severe perturbation was encountered. The perturbation has been characterized as due to first and second-order Coriolis interaction. The interaction affected a wide range of states and caused the spectral study quite challenging. The perturbation caused a variety of mixing of states producing hybrid states. This hybridization resulted in producing a large number of transitions which should not be allowed by the dipole selection rules via the “intensity borrowing effect”. It was possible to identify a large number of such forbidden transitions that gain sufficient strength through the “Intensity borrowing” effect. The transitions connecting to these perturbed states have been analyzed using standard Coriolis interaction formulae. The possibility of “Fermi” interaction has been excluded as the interaction is highly dependent on the rotational quantum number J. In general, this kind of transition should be excluded from global analysis and should be treated in isolation. It is pertinent to note that some previously published works studied these states using un-substantiated assignments being perhaps unaware of the perturbation. Corrections have been suggested for the analysis and understanding of the properties of the energy levels which have subtle differences with the energy levels of normal asymmetric molecules. In all, available microwave (MW) millimeter wave (MMW) far infrared (FIR), and infrared (IR) assignments have been put together to prepare the most accurate and and complete atlas of about 12,000 spectral lines. This atlas (Appendix A) should be considered a work-in-progress supplement to this paper and supersedes all other lists known to date on this species can be had from one of us (IM) or via Researchgate.

MALDI-mass spectrometry imaging as a new technique for detecting non-heme iron in peripheral tissues via caudal vein injection of deferoxamine.

As one of the most common iron-chelating agents, deferoxamine (DFO) rapidly chelates iron in the body. Moreover, it does not compete for the iron characteristic of hemoglobin in the blood cells, which is common in the clinical treatment of iron poisoning. Iron is a trace element necessary to maintain organism normal life activities. Iron deficiency can lead to anemia, whereas iron overload can cause elevated levels of cellular oxidative stress and cell damage. As a consequence, detection of the iron content in tissues and blood is of great significance. The traditional techniques for detecting the iron content include inductively coupled plasma-mass spectrometry and atomic absorption spectrometry, which cannot be used for imaging purposes. Laser ablation-ICP-MS and synchrotron radiation micro-X-ray fluorescence can map the concentration and distribution of iron in tissues. However, these methods can only be used to measure the total iron levels in blood or tissues. In recent years, due to the deepening understanding of iron metabolism, diseases related to iron overload have attracted increasing attention. Therefore, we took advantage of the properties of DFO in terms of chelating iron and investigated different sampling times following DFO injection in the tail vein of mice. We used mass spectrometry imaging (MSI) technology to detect the DFO and ferrioxamine content in the blood and different tissues to indirectly characterize the non-heme iron content.

Interactions of CaO with Pure Mg and Mg-Ca alloys - an in situ synchrotron radiation diffraction study

Interactions of CaO with Pure Mg and Mg-Ca alloys - an in situ synchrotron radiation diffraction study

Preparation and measurement of an x-ray Laue-type monochromator based on a WSi2/Si multilayer

The Laue-type multilayer monochromator (LMM) is a promising optical element with a small size and high efficiency in a synchrotron radiation facility. By the dynamical diffraction theory, using DC magnetron sputtering technology, an LMM with a total thickness of 47 µm and a periodic thickness of 4.7 nm WSi2/Si multilayer at 26 keV is designed and fabricated. During the preparation, the total number of layers is up to 20000, and every 300th layer of Si is replaced by WSi2 as the marker, so the multilayer is divided into 67 areas. The cross section of the multilayer is measured by a scanning electron microscope (SEM), and the marker region thickness error is 0.28% (RMS). The diffraction test experiment of the LMM is carried out at the Shanghai synchrotron radiation facility (SSRF). The 1st-order peak angle is 5.05 mrad, and the efficiency is 75.0%, which is close to the theoretical calculation result of 5.1 mrad and 79.1%. The Darwin width of the LMM is 0.17 mrad which is equal to the theoretical calculation. Based on the Bragg’s diffraction equation, the energy resolution (ΔE/E) is 3.3%.

Upgrade of crystallography beamline BL19U1 at the Shanghai Synchrotron Radiation Facility

BL19U1, an energy-tunable protein complex crystallography beamline at the Shanghai Synchrotron Radiation Facility, has emerged as one of the most productive MX beamlines since opening to the public in July 2015. As of October 2023, it has contributed to over 2000 protein structures deposited in the Protein Data Bank (PDB), resulting in the publication of more than 1000 scientific papers. In response to increasing interest in structure-based drug design utilizing X-ray crystallography for fragment library screening, enhancements have been implemented in both hardware and data collection systems on the beamline to optimize efficiency. Hardware upgrades include the transition from MD2 to MD2S for the diffractometer, alongside the installation of a humidity controller featuring a rapid nozzle exchanger. This allows users to opt for either low-temperature or room-temperature data collection modes. The control system has been upgraded from Blu-Ice to MXCuBE3, which supports website-mode data collection, providing enhanced compatibility and easy expansion with new features. An automated data processing pipeline has also been developed to offer users real-time feedback on data quality.

Feature extraction and spatial imaging of synchrotron radiation X-ray diffraction patterns using unsupervised machine learning

Feature extraction and spatial imaging of synchrotron radiation X-ray diffraction patterns using unsupervised machine learning

Microanatomy of the human tunnel of Corti structures and cochlear partition-tonotopic variations and transcellular signaling.

Auditory sensitivity and frequency resolution depend on the optimal transfer of sound-induced vibrations from the basilar membrane (BM) to the inner hair cells (IHCs), the principal auditory receptors. There remains a paucity of information on how this is accomplished along the frequency range in the human cochlea. Most of the current knowledge is derived either from animal experiments or human tissue processed after death, offering limited structural preservation and optical resolution. In our study, we analyzed the cytoarchitecture of the human cochlear partition at different frequency locations using high-resolution microscopy of uniquely preserved normal human tissue. The results may have clinical implications and increase our understanding of how frequency-dependent acoustic vibrations are carried to human IHCs. A 1-micron-thick plastic-embedded section (mid-modiolar) from a normal human cochlea uniquely preserved at lateral skull base surgery was analyzed using light and transmission electron microscopy (LM, TEM). Frequency locations were estimated using synchrotron radiation phase-contrast imaging (SR-PCI). Archival human tissue prepared for scanning electron microscopy (SEM) and super-resolution structured illumination microscopy (SR-SIM) were also used and compared in this study. Microscopy demonstrated great variations in the dimension and architecture of the human cochlear partition along the frequency range. Pillar cell geometry was closely regulated and depended on the reticular lamina slope and tympanic lip angle. A type II collagen-expressing lamina extended medially from the tympanic lip under the inner sulcus, here named "accessory basilar membrane." It was linked to the tympanic lip and inner pillar foot, and it may contribute to the overall compliance of the cochlear partition. Based on the findings, we speculate on the remarkable microanatomic inflections and geometric relationships which relay different sound-induced vibrations to the IHCs, including their relevance for the evolution of human speech reception and electric stimulation with auditory implants. The inner pillar transcellular microtubule/actin system's role of directly converting vibration energy to the IHC cuticular plate and ciliary bundle is highlighted.

Nonstationary Laguerre–Gaussian states in a Magnetic Field

Abstract The Landau states of electrons with orbital angular momentum in magnetic fields are important in the quantum theories of metals and of synchrotron radiation at storage rings, in relativistic astrophysics of neutron stars, and in many other areas. In realistic scenarios, electrons are often born inside the field or injected from a field-free region, requiring nonstationary quantum states to account for boundary or initial conditions. This study presents nonstationary Laguerre–Gaussian (NSLG) states in a longitudinal magnetic field, characterizing vortex electrons after their transfer from vacuum to the field. Comparisons with Landau states and calculations of observables such as mean energy and root-mean-square (r.m.s.) radius show that the r.m.s. radius of the electron packet in the NSLG state oscillates in time around a significantly larger value than that of the Landau state. This quantum effect of oscillations is due to boundary conditions and can potentially be observed in various problems, particularly when using magnetic lenses of electron microscopes and linear accelerators. Analogies are drawn between a quantum wave packet and a classical beam of many particles in phase space, including the calculation of mean emittance of the NSLG state as a measure of its quantum nature.

Depth profiling of microwave nitrogen-terminated polycrystalline diamond surfaces by energy-dependent X-ray photoelectron spectroscopy

Nitrogen-terminated diamonds hold promise for stabilizing near-surface NV− centers, which is essential for reliable quantum sensing. Among various surface preparation methods, microwave (MW) nitrogen plasma, known for its minimal surface damage, appears as the most effective choice. In this investigation, we explore the nature of nitrogen bonding of polycrystalline diamond (PCD) surfaces exposed to MW nitrogen plasma using X-ray Photoelectron Spectroscopy (XPS) depth profiling and Near-Edge X-ray Absorption Fine Structure (NEXAFS) spectroscopy at the C K- and N K-edges. XPS depth profiling with atomic resolution, achieved by varying the probing photon energy using synchrotron radiation and supported by a physical model considering the associated inelastic mean free path, suggests a surface of almost fully saturated nitrogen in two main bonding configurations of similar contribution and a low coverage of ∼5 % of graphene-like islands residing atop the nitrogen-terminated diamond surface. The thermal stability of these surface groups is monitored by in situ annealing up to 700 °C. The depth profiles reveal that nitrogen atoms do not diffuse in the diamond crystal, resulting in excellent diamond crystallinity in the first atomic planes below the surface. C K-edge NEXAFS analysis reveals the position of unoccupied surface states within the diamond bandgap, opening new perspective on the stabilization of near-surface NV− centers.

Observation of Granulation Tissue of Tongue Using Synchrotron Radiation

Observation of Granulation Tissue of Tongue Using Synchrotron Radiation

Polarized QED cascades over pulsar polar caps

ABSTRACT The formation of e± plasmas within pulsar magnetospheres through quantum electrodynamics (QED) cascades in vacuum gaps is widely acknowledged. This paper aims to investigate the effect of photon polarization during the QED cascade occurring over the polar cap of a pulsar. We employ a Monte Carlo-based QED algorithm that accurately accounts for both spin and polarization effects during photon emission and pair production in both single-particle and particle-in-cell (PIC) simulations. Our findings reveal distinctive properties in the photon polarization of curvature radiation (CR) and synchrotron radiation (SR). CR photons exhibit high linear polarization parallel to the plane of the curved magnetic field lines, whereas SR photons, on average, demonstrate weak polarization. As the QED cascade progresses, SR photons gradually dominate over CR photons, thus reducing the average degree of photon polarization. Additionally, our study highlights an intriguing observation: the polarization of CR photons enhances e± pair production by approximately 5 per cent, in contrast to the inhibition observed in laser–plasma interactions. Our self-consistent QED-PIC simulations in the corotating frame reproduce the essential results obtained from single-particle simulations.

Radio emission from SN 1181 hosting a white dwarf merger product

Abstract The remnant of the historical supernova 1181 is claimed to be associated with a white dwarf merger remnant J005311. The supernova remnant (SNR) shock, and a termination shock expected to be formed by the intense wind of J005311, are potential sites for radio emission via synchrotron emission from shock-accelerated electrons. In this paper, we estimate the radio emission from these two shocks, and find the peak radio flux to be 0.1–10 mJy (at 0.01–1 GHz) in the outer SNR shock and 0.01–0.1 mJy (at 1–10 GHz) in the inner termination shock. We also search for radio emission from this source in the archival data of the Karl G. Jansky Very Large Array (VLA) Sky Survey at 3 GHz, the NRAO VLA Sky Survey at 1.4 GHz and the Canadian Galactic Plane Survey at 408 MHz, finding no significant detection. While targeted observations with higher sensitivity are desired, we particularly encourage those at higher frequency and angular resolution to probe the inner termination shock and its evolution.

Gamma-ray variability and multi-wavelength insights into the unprecedented outburst from 4C 31.03

The blazar 4C31.03 recently underwent a major γ-ray outburst at the beginning of 2023 after a prolonged quiescent phase. Fermi-LAT reported a daily average flux of 5×10−6 phs cm−2 s−1, which is about 60 times its average value. We investigated this extraordinary outbreak through temporal and multi-wavelength analysis. From the statistical analysis of the γ-ray lightcurves using Bayesian blocks, we identified 3 epochs of prominent flares. The fastest flux decay during this major outburst was observed within 5.5±0.7 hours. The highest energy of γ-ray photons found from the source during the active phase is ∼82GeV. Using the transparency of γ-rays against pair production and light crossing time argument, we could obtain the minimum jet Doppler factor as 17 corresponding to the flaring state. The broadband spectral energy distribution study performed using synchrotron, SSC and EC emission processes supports the external Compton scattering of IR photons as the likely mechanism for the γ-ray emission from the source. The results of this study support the scenario of the emission region in 4C31.03, being located beyond the Broad line region from the central blackhole. The long-term γ-ray flux distribution depicts a double log-normal variability, indicating that two distinct flux states are active in this energy band. The index distribution also reveals a two distinct variability pattern and hints that the γ-ray spectrum can be more precisely described by two photon indices.

Volume X-Ray Micro-Computed Tomography Analysis of the Early Cephalized Central Nervous System in a Marine Flatworm, Stylochoplana pusilla.

Platyhelminthes are a phylum of simple bilaterian invertebrates with prototypic body systems. Compared with non-bilaterians such as cnidarians, the bilaterians are likely to exhibit integrated free-moving behaviors, which require a concentrated nervous system "brain" rather than the distributed nervous system of radiatans. Marine flatworms have an early cephalized 'central' nervous system compared not only with non-bilaterians but also with parasitic flatworms or freshwater planarians. In this study, we used the marine flatworm Stylochoplana pusilla as an excellent model organism in Platyhelminthes because of the early cephalized central nervous system. Here, we investigated the three-dimensional structures of the flatworm central nervous system by the use of X-ray micro-computed tomography (micro-CT) in a synchrotron radiation facility. We found that the obtained tomographic images were sufficient to discriminate some characteristic structures of the nervous system, including nerve cords around the cephalic ganglion, mushroom body-like structures, and putative optic nerves forming an optic commissure-like structure. Through the micro-CT imaging, we could obtain undistorted serial section images, permitting us to visualize precise spatial relationships of neuronal subpopulations and nerve tracts. 3-D micro-CT is very effective in the volume analysis of the nervous system at the cellular level; the methodology is straightforward and could be applied to many other non-model organisms.

X-ray Synchrotron Radiation to Look at Pigments in Antiquities: Overview and Examples

The recent upgrading of synchrotron radiation (SR) sources has favored, in the last few years, the construction and design of beamlines optimized for the study of cultural heritage materials, which may require ad hoc setups, specific spatial resolutions, and detection limits. In the field of cultural heritage, integrated approaches combining different techniques are often required, even at large facilities, where some beamlines offer the possibility of performing different types of measurements at the same point of analysis, complementing preliminary information usually obtained by conventional laboratory and/or portable in situ methods. An overview of the last ten years of synchrotron applications for the study of pigments is given, with discussion of upstream and downstream challenges to methods and techniques. The possibilities offered by the synchrotron techniques are illustrated by a case study of a particular class of painted ceramics, as an example of different research questions that are solved by a combination of SR-based methods.

A comprehensive investigation of the interactions of human serum albumin with polymeric and hybrid nanoparticles.

Nanoparticles (NPs) engineered as drug delivery systems continue to make breakthroughs as they offer numerous advantages over free therapeutics. However, the poor understanding of the interplay between the NPs and biomolecules, especially blood proteins, obstructs NP translation to clinics. Nano-bio interactions determine the NPs' in vivo fate, efficacy and immunotoxicity, potentially altering protein function. To fulfill the growing need to investigate nano-bio interactions, this study provides a systematic understanding of two key aspects: (i) protein corona (PC) formation and (ii) NP-induced modifications on protein's structure and stability. A methodology was developed by combining orthogonal techniques to analyze both quantitative and qualitative aspects of nano-bio interactions, using human serum albumin (HSA) as a model protein. Protein quantification via liquid chromatography-mass spectrometry, and capillary zone electrophoresis (CZE) clarified adsorbed protein quantity and stability. CZE further unveiled qualitative insights into HSA forms (native, glycated HSA and cysteinylated), while synchrotron radiation circular dichroism enabled analyzing HSA's secondary structure and thermal stability. Comparative investigations of NP cores (organic vs. hybrid), and shells (with or without polyethylene glycol (PEG)) revealed pivotal factors influencing nano-bio interactions. Polymeric NPs based on poly(lactic-co-glycolic acid) (PLGA) and hybrid NPs based on metal-organic frameworks (nanoMOFs) presented distinct HSA adsorption profiles. PLGA NPs had protein-repelling properties while inducing structural modifications on HSA. In contrast, HSA exhibited a high affinity for nanoMOFs forming a PC altering thereby the protein structure. A shielding effect was gained through PEGylation for both types of NPs, avoiding the PC formation as well as the alteration of unbound HSA structure.

Third-Order Intrinsic Aberration Modification with Second-Order Accuracy Transfer of Pupil Coordinates and Extrinsic Aberration of Plane-Symmetric Optical System with a Two-Dimensional Field Light Source

A plane-symmetric optical system with a two-dimensional field light source, such as a soft X-ray and vacuum ultraviolet optical system, is widely used for synchrotron radiation source devices, microscopes and so on. Therefore, this paper studied third-order intrinsic aberration modification with second-order accuracy transfer of pupil coordinates and extrinsic aberration of these kinds of optical systems. First, we discuss the extrinsic aberration calculation method and derive the corresponding aberration expressions; in addition, we apply optical geometric relations and the polynomial fitting method to obtain a second-order accuracy transfer relationship expression of the pupil coordinates between adjacent optical surfaces and derived the modification calculation expressions of the intrinsic aberration caused by the above factor. Finally, the third-order intrinsic aberration modification with second-order accuracy transfer of pupil coordinates and extrinsic aberration expressions derived in this paper are applied to calculate ray spot diagrams of two soft X-ray and vacuum ultraviolet optical systems with meridional and sagittal field angle light sources, and these results are compared with those obtained from the ray-tracing software Shadow; this showed that the calculation accuracy of the aberration expressions is sufficient.