Search Results (44)

Magnetron sputtering offers a scalable route to magnetic topological insulators (MTIs) based on Cr-doped Sb₂Te₃. We combine a range of X-ray diffraction (XRD), reciprocal-space mapping (RSM), scanning transmission electron microscopy (STEM), scanning TEM-energy-dispersive X-ray spectroscopy (STEM-EDS), and X-ray absorption spectroscopy, and X-ray magnetic circular dichroism (XAS/XMCD) techniques to study the structure and magnetism of Cr-doped Sb₂Te₃ films. Symmetric $\theta$-2$\theta$ XRD and RSM establish a solubility window. Layered tetradymite order persists up to ∼10 at.-% Cr, while higher doping yields CrTe/Cr₂Te₃ secondary phases. STEM reveals nanocrystalline layered stacking at low Cr and loss of long-range layering at higher Cr concentrations, consistent with XRD/RSM. Magnetometry on a 6% film shows soft ferromagnetism at 5 K. XAS and XMCD at the Cr $L_{2,3}$ edges exhibits a depth dependence: total electron yield (TE; surface sensitive) shows both nominal Cr²⁺ and Cr³⁺, whereas fluorescence yield (FY; bulk sensitive) shows a much higher Cr²⁺ weight. Sum rules applied to TEY give $m_L=(0.20\pm 0.04)$${\mu }_{\mathrm{B}}$/Cr, and $m_S=(1.6\pm 0.2)$${\mu }_{\mathrm{B}}$/Cr, whereby we note that the applied maximum field (3 T) likely underestimates $m_S$. These results define a practical growth window and outline key parameters for MTI films. Full article

Recent measurements of the band properties of AlN and GaN by fluorescence yield absorption and soft X-ray emission spectroscopies revealed that their valence band (VB) is composed of two separate subbands. The upper VB subband of GaN is composed of gallium sp and nitrogen p orbitals; the lower subband consists of metal d and nitrogen s orbitals. These findings were confirmed by extensive ab initio simulations. These results are not consistent with the standard tetrahedrally coordinated semiconductors, which are bonded by sp³-hybridized orbitals of metal and nonmetal atoms. The new analysis techniques and ab initio simulations create a new picture, allowing the calculation of overlap integrals to determine the bond order in these crystals. According to these results, bonding occurs between resonant p-states of nitrogen and sp³-hybridized metal orbitals in tetrahedral nitrides, allowing tetrahedral symmetry to be maintained. A similar resonant bonding mechanism is observed in hexagonal BN, where the p orbitals of nitrogen create three resonant states necessary for maintaining the planar symmetry of the lattice. In addition, nonresonant $\pi$-type bonds in BN are created by the overlap of $p_z$ orbitals of boron and nitrogen. BN bonding differs from that in graphene, where carbon states are fully sp²-hybridized. Additionally, $\pi$-type bonds in graphene have no ionic contributions, which leads to the formation of Dirac states with linear dispersion close to the K point, closing the band gap. Full article

The interaction of fullerenes and their derivatives with environmental molecules such as oxygen or water was crucial for the rational design of low-dimensional materials and devices. In this paper, the near-edge X-ray absorption fine structure (NEXAFS), X-ray emission spectroscopy (XES) and X-ray photoelectron spectroscopy (XPS) shake-up satellites were employed to distinguish the oxides and hydrates of the fullerene C₆₀ and azafullerene C₅₉N families. The study includes various isomers, such as the open [5,6] and closed [6,6] isomers of C₆₀O, C₆₀H(OH), C₆₀-O-C₆₀, C₆₀H-O-C₆₀H, C₅₉N(OH) and C₅₉N-O-C₅₉N, based on density functional theory. These soft X-ray spectra offered comprehensive insights into the molecular orbitals of these azafullerene molecular groups. The oxygen K-edge NEXAFS, carbon and oxygen K-edge XPS shake-up satellite spectra provided valuable tools for distinguishing oxides or hydrates of fullerene C₆₀ and azafullerene C₅₉N. Our findings could significantly benefit the development of fullerene functional molecular materials and expand the application scope of soft X-ray spectroscopy as a molecular fingerprinting tool for the fullerene family. Full article

Nanomaterial-based humidity sensors hold great promise for water vapor detection because of their high sensitivity and fast response/recovery. However, the condensation of water in nanomaterial films remains unclear from a physicochemical perspective. Herein, the condensation of water vapor in silica nanoparticle films was physicochemically analyzed to bridge the abovementioned gap. The morphology of surface-adsorbed water molecules was characterized using infrared absorption spectroscopy and soft X-ray absorption spectroscopy, and the effect of RH on the amount of adsorbed water was observed using a quartz crystal microbalance. The adsorbed water was found to exist in liquid- and ice-like states, which contributed to high and low conductivity, respectively. The large change in film impedance above 80% RH was ascribed to the condensation of water between the nanoparticles. Moreover, RH alteration resulted in a colorimetric change in the film’s interference fringe. The obtained insights were used to construct a portable device with response and recovery times suitable for the real-time monitoring of water vapor. Thus, this study clarifies the structure of water adsorbed on nanomaterial surfaces and, hence, the action mechanism of the corresponding nanoparticle-based sensors, inspiring further research on the application of various nanomaterials to vapor sensing. Full article

An online automatic feedback system has been successfully installed and commissioned at the BL08U1A Soft X-ray Spectromicroscopy Beamline of Shanghai Synchrotron Radiation Facility, which can monitor the incident X-ray beam in real time by measuring the blade-edge signals of the exit slit and automatically adjust the elliptical cylindrical mirror parameters to achieve beam calibration and maintain the optimal X-ray flux of the sample. This work provides a comprehensive description of the hardware composition, system implementation, feedback logic, function and software design, system optimization and commission, as well as the online experimental results supported by the system. The experimental results demonstrated that the online automatic feedback system is capable of effectively maintaining the optimal X-ray beam flux for X-ray absorption spectroscopy experiments. Its success can provide valuable technique assistance for the design, construction and optimization of similar systems at various beamlines in synchrotron sources in the future. Full article

The aim of this project is to fabricate hydrogen-rich silicone doped with magnetic nanoparticles for use as a temperature change indicator in magnetic resonance imaging-guided (MRIg) thermal ablations. To avoid clustering, the particles of mixed MnZn ferrite were synthesized directly in a medical-grade silicone polymer solution. The particles were characterized by transmission electron microscopy, powder X-ray diffraction, soft X-ray absorption spectroscopy, vibrating sample magnetometry, temperature-dependent nuclear magnetic resonance relaxometry (20 °C to 60 °C, at 3.0 T), and magnetic resonance imaging (at 3.0 T). Synthesized nanoparticles were the size of 4.4 nm ± 2.1 nm and exhibited superparamagnetic behavior. Bulk silicone material showed a good shape stability within the study’s temperature range. Embedded nanoparticles did not influence spin–lattice relaxation, but they shorten the longer component of spin–spin nuclear relaxation times of silicone’s protons. However, these protons exhibited an extremely high r₂^* relaxivity (above 1200 L s⁻¹ mmol⁻¹) due to the presence of particles, with a moderate decrease in the magnetization with temperature. With an increased temperature decrease of r₂^*, this ferro–silicone can be potentially used as a temperature indicator in high-temperature MRIg ablations (40 °C to 60 °C). Full article

Scanning transmission X-ray microscopy (STXM) provides the imaging of biological specimens allowing the parallel collection of localized spectroscopic information by X-ray fluorescence (XRF) and/or X-ray Absorption Near Edge Spectroscopy (XANES). The complex metabolic mechanisms which can take place in biological systems can be explored by these techniques by tracing even small quantities of the chemical elements involved in the metabolic pathways. Here, we present a review of the most recent publications in the synchrotrons’ scenario where soft X-ray spectro-microscopy has been employed in life science as well as in environmental research. Full article

Cotton fiber is favored by people because of its good moisture absorption, heat preservation, soft feel, comfortable wearing and other excellent performance. In recent years, due to the destruction of the ozone layer, the intensity of ultraviolet radiation at ground level has increased. Cotton fiber will degrade under long time ultraviolet irradiation, which limits the outdoor application of cotton fiber. In this study, titanium dioxide (TiO₂) particles were prepared on the surface of cotton fibers with the help of supercritical carbon dioxide (SCCO₂) to improve the UV resistance of cotton fibers. The effects of SCCO₂ treatment on the morphology, surface composition, thermal stability, photostability and mechanical properties of TiO₂ were studied by Fourier transform infrared spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, thermogravimetric analysis, UV-VIS spectroscopy, and single fiber test. The results showed that TiO₂ particles were generated on the fiber surface, which reduced the photo-degradation rate of cotton fiber. This is because TiO₂ can absorb UV rays and reduce the absorption of UV rays by the cotton fiber itself. The synthesis process of SCCO₂ is simple and environmentally friendly, which provides a promising technology for the synthesis of metal nitrogen dioxide on natural plant fibers. Full article

The development of novel coherent and brilliant sources, such as soft X-ray free electron laser (FEL) and high harmonic generation (HHG), enables new ultrafast analysis of the electronic and structural dynamics of a wide variety of materials. Soft X-ray FEL delivers high-brilliance beams with a short pulse duration, high spatial coherence and photon energy tunability. In comparison with FELs, HHG X-ray sources are characterized by a wide spectral bandwidth and few- to sub-femtosecond pulses. The approach will lead to the time-resolved reconstruction of molecular dynamics, shedding light on different photochemical pathways. The high peak brilliance of soft X-ray FELs facilitates investigations in a nonlinear regime, while the broader spectral bandwidth of the HHG sources may provide the simultaneous probing of multiple components. Significant technical breakthroughs in these novel sources are under way to improve brilliance, pulse duration, and to control spectral bandwidth, spot size, and energy resolution. Therefore, in the next few years, the new generation of soft X-ray sources combined with novel experimental techniques, new detectors, and computing capabilities will allow for the study of several extremely fast dynamics, such as vibronic dynamics. In the present review, we discuss recent developments in experiments, performed with soft X-ray FELs and HHG sources, operating near the carbon K-absorption edge, being a key atomic component in biosystems and soft materials. Different spectroscopy methods such as time-resolved pump-probe techniques, nonlinear spectroscopies and photoelectron spectroscopy studies have been addressed in an attempt to better understand fundamental physico-chemical processes. Full article

Magnesium borohydride (Mg(BH₄)₂) is an attractive compound for solid-state hydrogen storage due to its lucratively high hydrogen densities and theoretically low operational temperature. Hydrogen release from Mg(BH₄)₂ occurs through several steps. The reaction intermediates formed at these steps have been extensively studied for a decade. In this work, we apply spectroscopic methods that have rarely been used in such studies to provide alternative insights into the nature of the reaction intermediates. The commercially obtained sample was decomposed in argon flow during thermogravimetric analysis combined with differential scanning calorimetry (TGA-DSC) to differentiate between the H₂-desorption reaction steps. The reaction products were analyzed by powder X-ray diffraction (PXRD), near edge soft X-ray absorption spectroscopy at boron K-edge (NEXAFS), and synchrotron infrared (IR) spectroscopy in mid- and far-IR ranges (SR-FTIR). Up to 12 wt% of H₂ desorption was observed in the gravimetric measurements. PXRD showed no crystalline decomposition products when heated at 260–280 °C, the formation of MgH₂ above 300 °C, and Mg above 320 °C. The qualitative analysis of the NEXAFS data showed the presence of boron in lower oxidation states than in (BH₄)⁻. The NEXAFS data also indicated the presence of amorphous boron at and above 340 °C. This study provides additional insights into the decomposition reaction of Mg(BH₄)₂. Full article

In this paper, by means of high-resolution photoemission, soft X-ray absorption and atomic force microscopy, we investigate, for the first time, the mechanisms of damaging, induced by neutron source, and recovering (after annealing) of p-i-n detector devices based on hydrogenated amorphous silicon (a-Si:H). This investigation will be performed by mean of high-resolution photoemission, soft X-Ray absorption and atomic force microscopy. Due to dangling bonds, the amorphous silicon is a highly defective material. However, by hydrogenation it is possible to reduce the density of the defect by several orders of magnitude, using hydrogenation and this will allow its usage in radiation detector devices. The investigation of the damage induced by exposure to high energy irradiation and its microscopic origin is fundamental since the amount of defects determine the electronic properties of the a-Si:H. The comparison of the spectroscopic results on bare and irradiated samples shows an increased degree of disorder and a strong reduction of the Si-H bonds after irradiation. After annealing we observe a partial recovering of the Si-H bonds, reducing the disorder in the Si (possibly due to the lowering of the radiation-induced dangling bonds). Moreover, effects in the uppermost coating are also observed by spectroscopies. Full article

Improvements in the antithrombogenicity activity of biomaterials for cardiovascular applications are necessary to meet the demand for vascular grafts in the world. Zwitterionic compounds tend to be used due to their anti-fouling properties, which reduce platelet adhesions and protein absorptions. Therefore, in this research, potato starch (AL-N) and zwitterionic starch (AL-Z) (obtained by Williamson etherification) were included as fillers in polyurethane (PU) matrices from polycaprolactone diol (PCL), polyethylene glycol (PEG), pentaerythritol (PE) and isophorone diisocyanate (IPDI) in order to study their effect in terms of their physicochemical, mechanical and thermal properties. We conducted our evaluation using attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), contact angle analysis, swelling behavior, thermogravimetric analysis (TGA), tensile/strain analysis, scanning electron microscopy equipped with energy dispersive X-ray spectroscopy (SEM-EDS), dynamic mechanic analysis (DMA), differential scanning calorimetry (DSC), and X-ray diffraction (XRD). The results showed that AL-N and AL-Z modified these properties, where AL-N improved tensile strength, and AL-Z increased the hydrophilicity of polyurethanes matrices; additionally, AL-N had interactions with the soft segments, and AL-Z had interactions with the hard segments. Finally, both fillers reduced the degree of crystallinity and did not affect the thermal stability of polyurethanes. Full article

Medical titanium alloy Ti-6Al-4V (TC4) is an ideal surgical implant material for human tissue repair and replacement. TC4 implantation will be in close contact with human soft tissue and has mechanical compatibility problems. In order to solve this problem, the hydrogel was formed on the surface of TC4 by utilizing the adhesion of dopamine, and the storage modulus of the formed hydrogel matched that of human soft tissue. In this paper, the surface of TC4 was first modified with dopamine (DA) and 2-bromoisobutyryl bromide (BIBB). 2-(2-methoxyethoxy) ethyl methacrylate (MEO₂MA), oligo (ethylene oxide) methacrylate (OEGMA) and 2-methacryloyloxyethyl phosphorylcholine (MPC) are used as monomers, and methylenebisacrylamide (MBA) is used as cross-linking agent. Thermosensitive hydrogels were formed on the surface of modified TC4 by the ATRP technique. The successful synthesis of initiator and hydrogels on TC4 was demonstrated by Fourier transform infrared (FT-IR) and X-ray photoelectron spectroscopy (XPS). The morphology of the hydrogel was observed by the scanning electron microscope (SEM), and the water absorption and temperature sensitivity were investigated by the swelling property. The thermal and mechanical properties of these gels were measured using thermal analysis system (TAS) and dynamic mechanical analyzer (DMA). The results show that the hydrogel on TC4 has good thermal stability and storage modulus that matches human soft tissue. Full article

In hard X-ray applications that require high detection efficiency and short response times, such as synchrotron radiation-based Mössbauer absorption spectroscopy and time-resolved fluorescence or photon beam position monitoring, III–V-compound semiconductors, and dedicated alloys offer some advantages over the Si-based technologies traditionally used in solid-state photodetectors. Amongst them, gallium arsenide (GaAs) is one of the most valuable materials thanks to its unique characteristics. At the same time, implementing charge-multiplication mechanisms within the sensor may become of critical importance in cases where the photogenerated signal needs an intrinsic amplification before being acquired by the front-end electronics, such as in the case of a very weak photon flux or when single-photon detection is required. Some GaAs-based avalanche photodiodes (APDs) were grown by a molecular beam epitaxy to fulfill these needs; by means of band gap engineering, we realised devices with separate absorption and multiplication region(s) (SAM), the latter featuring a so-called staircase structure to reduce the multiplication noise. This work reports on the experimental characterisations of gain, noise, and charge collection efficiencies of three series of GaAs APDs featuring different thicknesses of the absorption regions. These devices have been developed to investigate the role of such thicknesses and the presence of traps or defects at the metal–semiconductor interfaces responsible for charge loss, in order to lay the groundwork for the future development of very thick GaAs devices (thicker than 100 $\mathsf{\mu }$m) for hard X-rays. Several measurements were carried out on such devices with both lasers and synchrotron light sources, inducing photon absorption with X-ray microbeams at variable and controlled depths. In this way, we verified both the role of the thickness of the absorption region in the collection efficiency and the possibility of using the APDs without reaching the punch-through voltage, thus preventing the noise induced by charge multiplication in the absorption region. These devices, with thicknesses suitable for soft X-ray detection, have also shown good characteristics in terms of internal amplification and reduction of multiplication noise, in line with numerical simulations. Full article

The extension of the pump-probe approach known from UV/VIS spectroscopy to very short wavelengths together with advanced simulation techniques allows a detailed analysis of excited-state dynamics in organic molecules or biomolecular structures on a nanosecond to femtosecond time level. Optical pump soft X-ray probe spectroscopy is a relatively new approach to detect and characterize optically dark states in organic molecules, exciton dynamics or transient ligand-to-metal charge transfer states. In this paper, we describe two experimental setups for transient soft X-ray absorption spectroscopy based on an LPP emitting picosecond and sub-nanosecond soft X-ray pulses in the photon energy range between 50 and 1500 eV. We apply these setups for near-edge X-ray absorption fine structure (NEXAFS) investigations of thin films of a metal-free porphyrin, an aggregate forming carbocyanine and a nickel oxide molecule. NEXAFS investigations have been carried out at the carbon, nitrogen and oxygen K-edge as well as on the Ni L-edge. From time-resolved NEXAFS carbon, K-edge measurements of the metal-free porphyrin first insights into a long-lived trap state are gained. Our findings are discussed and compared with density functional theory calculations. Full article