Search Results (178)

Lipid-based nanomedicines are already widely used in antitumor therapy and gene delivery. However, their complex structural features demand advanced mesoscopic structural characterization tools for effective research and development (R&D) and quality control. Synchrotron small-angle X-ray scattering (SAXS) is a powerful, non-invasive technique for probing nanoscale membrane organizations, monitoring in situ dynamic membrane assembly, and exploring the interactions of components in lipid-based drug delivery systems, including liposomes, lipoplexes, lipid nanoparticles (LNPs), and lyotropic liquid crystals (LLCs). Recent advances in high-flux synchrotron facilities, high-frequency detectors, and automated SAXS data processing pipelines permit a detailed structural characterization of lamellarity, bilayer spacing, internal phases, core–shell morphology, as well as “pump-probe” dynamic process studies for lipid nanomedicines. Though major challenges remain in sample polydispersity and model fitting, the advances in time-resolved synchrotron SAXS, high-throughput automation, and artificial intelligence (AI)-assisted modeling are rapidly reducing this barrier. This review summarizes SAXS methodology and introduces representative case studies in the field of lipid nanomedicines. The performance of BioSAXS beamline BL19U2 in the Shanghai synchrotron radiation facility (SSRF) and prospects of AI-guided drug screening at BL19U2 are highlighted to advance intelligent R&D and quality control for lipid nanomedicines. Full article

The study of the antimatter component in cosmic rays is essential for the understanding of their acceleration and propagation mechanisms, and is one of the most powerful tools for the indirect search of dark matter. Current methods rely on magnetic spectrometers for charge-sign discrimination, but these are not suitable for extending measurements to the TeV region within a short timeframe of a few decades. Since most of present and upcoming high-energy space experiments use large calorimeters, it is crucial to develop an alternative charge-sign discrimination technique that can be integrated with them. The Electron/Positron Space Instrument (EPSI) project, a two-year R&D initiative launched in 2023 with EU recovery funds, aims to address this challenge. The basic idea is to exploit the synchrotron radiation emitted by charged particles moving through Earth’s magnetic field. The simultaneous detection of an electron/positron with an electromagnetic calorimeter and synchrotron photons with an X-ray detector is enough to discriminate between the two particles at the event level. The main challenge is to develop an X-ray detector with a very large active area, high X-ray detection efficiency, and a low-energy detection threshold, compliant with space applications. In this paper, we give an overview of the EPSI project, with a focus on the general idea of the detection principle, the concept of the space instrument, and the design of the X-ray detector. Full article

This review highlights the significance of modern quantum-beam techniques, particularly neutron and synchrotron radiation sources, for advanced microstructural characterization of metallic systems. Following a brief introduction to neutron and synchrotron diffraction, selected studies demonstrate their application in probing thermally induced structural evolution in plastically deformed metals. Additively manufactured CoCrFeNi alloys and 316L stainless steels subjected to high-pressure torsion (HPT) were investigated by in situ neutron diffraction during heating, revealing the sequential regimes of recovery, recrystallization, and grain growth. Coupled with mechanical measurements, the results show that HPT followed by controlled thermal treatment improves the mechanical performance, offering strategies for designing engineering materials with enhanced properties. The thermal anisotropy behavior of Ti-45Al-7.5Nb alloys under in situ neutron diffraction is defined as anisotropic ordering upon heating, while the HPT-processed alloy displayed isotropic recovery of order at earlier temperatures. Complementary in situ synchrotron studies in rolled-sheet magnesium alloys unveiled microstructural rearrangement, grain rotation, recovery, and precipitate dissolution during annealing. And phase transformation, recovery, and recrystallization processes were detected in steel using HEXRD. This work emphasizes the complementary strengths of the neutron and synchrotron methods and recommends their broader application as powerful tools to unravel microstructure–property relationships in plastically deformed metals. Full article

The advancements in the 4th-generation synchrotron radiation light sources, characterized by their enhanced coherence and brightness, have led to more stringent requirements for the surface quality of X-ray mirrors used in beamlines. This poses a significant challenge to the metrology of X-ray mirrors. This research work focuses on high-precision measurement techniques for X-ray mirrors. The algorithmic principles of various stitching methods were introduced in detail, and a custom-built stitching measurement system was demonstrated. The system was used to perform a stitching measurement on an elliptical X-ray mirror, and the results showed high consistency with the data provided by JTEC. This verifies the effectiveness of the stitching interferometry method and the high measurement capability of our system. Full article

Ensuring the quality and safety of agricultural and food products is crucial for protecting consumer health, meeting market expectations, and complying with regulatory requirements. Quality and safety parameters are commonly assessed using chemical and microbiological analyses, which are time-consuming, impractical, and involve the use of toxic solvents, often disrupting the material’s original structure. An alternative technique, infrared spectroscopy, including near-infrared (NIR), mid-infrared (MIR), and short-wave infrared (SWIR), has emerged as a rapid, powerful, and minimally destructive technique for evaluating the quality and safety of food and agricultural products. This review focuses on discussing MIR spectroscopy, particularly Fourier transform infrared (FTIR) techniques, with emphasis on the attenuated total reflectance (ATR) measurement mode (globar infrared light source is commonly used) and on the use of synchrotron radiation (SR) as an alternative high-brightness light source. Both approaches enable the extraction of detailed spectral data related to molecular and functional attributes concerning quality and safety, thereby facilitating the assessment of crop disorders, food chemical composition, microbial contamination (e.g., mycotoxins, bacteria), and the detection of food adulterants, among several other applications. In combination with advanced chemometric techniques, FTIR spectroscopy, whether employing ATR as a measurement mode or SR as a high-brightness light source, is a powerful analytical tool for classification based on attributes, variety, nutritional and geographical origins, with or without minimal sample preparation, no chemical use, and short analysis time. However, limitations exist regarding calibrations, validations, and accessibility. The objective of this review is to address recent technological advancements and existing constraints of FTIR conducted in ATR mode and using SR as a light source (not necessarily in combination). It defines potential pathways for the comprehensive integration of FTIR and chemometrics for real-time quality and safety monitoring systems into the global food supply chain. Full article

X-ray absorption spectroscopy (XAS) and X-ray emission spectroscopy (XES) are analytical techniques enabling precise analysis of the electronic structure and local atomic environment in chemical compounds and materials. Their application spans materials science, chemistry, biology, and environmental sciences, supporting studies on catalytic mechanisms, redox processes, and metal speciation. A key advantage of both techniques is element selectivity, allowing the analysis of specific elements without matrix interference. Their high sensitivity to chemical state and coordination enables determination of oxidation states, electronic configuration, and local geometry. These methods are applicable to solids, liquids, and gases without special sample preparation. Modern XAS and XES studies are typically performed using synchrotron radiation, which provides an intense, monochromatic X-ray source and allows advanced in situ and operando experiments. Sub-techniques such as XANES (X-ray absorption near-edge structure), EXAFS (Extended X-ray Absorption Fine Structure), and RIXS (resonant inelastic X-ray scattering) offer enhanced insights into oxidation states, local structure, and electronic excitations. Despite their broad scientific use, applications in pharmaceutical research remain limited. Nevertheless, recent studies highlight their potential in analyzing crystalline active pharmaceutical ingredients (APIs), drug–biomolecule interactions, and differences in drug activity. This review introduces the fundamental aspects of XAS and XES, with an emphasis on practical considerations for pharmaceutical applications, including experimental design and basic spectral interpretation. Full article

Electrochemical CO₂ reduction reaction (CO₂RR) is a key technology for achieving carbon neutrality and efficient utilization of renewable energy, capable of converting CO₂ into high-value-added carbon-based fuels and chemicals. Copper (Cu)-based catalysts have attracted significant attention due to their unique performance in generating multi-carbon (C₂₊) products such as ethylene and ethanol; however, there are still many controversies regarding their complex reaction mechanisms, active sites, and the dynamic evolution of intermediates. In situ Raman spectroscopy, with its high surface sensitivity, applicability in aqueous environments, and precise detection of molecular vibration modes, has become a powerful tool for studying the structural evolution of Cu catalysts and key reaction intermediates during CO₂RR. This article reviews the principles of electrochemical in situ Raman spectroscopy and its latest developments in the study of CO₂RR on Cu-based catalysts, focusing on its applications in monitoring the dynamic structural changes of the catalyst surface (such as Cu⁺, Cu⁰, and Cu²⁺ oxide species) and identifying key reaction intermediates (such as *CO, *OCCO(*O=C-C=O), *COOH, etc.). Numerous studies have shown that Cu-based oxide precursors undergo rapid reduction and surface reconstruction under CO₂RR conditions, resulting in metallic Cu nanoclusters with unique crystal facets and particle size distributions. These oxide-derived active sites are considered crucial for achieving high selectivity toward C₂₊ products. Time-resolved Raman spectroscopy and surface-enhanced Raman scattering (SERS) techniques have further revealed the dynamic characteristics of local pH changes at the electrode/electrolyte interface and the adsorption behavior of intermediates, providing molecular-level insights into the mechanisms of selectivity control in CO₂RR. However, technical challenges such as weak signal intensity, laser-induced damage, and background fluorescence interference, and opportunities such as coupling high-precision confocal Raman technology with in situ X-ray absorption spectroscopy or synchrotron radiation Fourier transform infrared spectroscopy in researching the mechanisms of CO₂RR are also put forward. Full article

In this study, we examined how printing temperature affects the microstructure and mechanical properties of polylactic acid (PLA) composite reinforced with iron oxide i.e., magnetite manufactured using a material extrusion technique. The composite was printed at temperatures from 185 °C to 215 °C. Microstructure analysis via synchrotron radiation X-ray microtomography revealed changes in both iron oxide and porosity contents within the printed structures. Mechanical testing results demonstrated a limited effect of the printing temperature on tensile performance. Finite element computation is considered to predict the elasticity behavior of the printed composite by converting 3D images into 3D structural meshes. When implementing a two-phase model, the predictions show a leading role of the iron oxide content, and an overestimation of the stiffness of the composite. A three-phase model demonstrates a better matching of the experimental results suggesting a limited load transfer across the PLA-iron oxide interface with Young’s moduli in the interphase zone as small as 10% of PLA Young’s modulus. Magnetic actuation demonstrates that experiments on PLA-iron oxide plates reveal a pronounced thickness-dependent limitation, with the maximum deflection observed in thin strips of 0.4 mm. Full article

The ordered tetragonal FeNi L1₀ phase, tetrataenite, is a promising candidate for rare earth-free permanent magnets due to its competitive magnetic properties and the low cost of the constituent elements. In this work, we have investigated the effect of molybdenum and aluminum substitution on the formation of the ordered L1₀ phase. The alloys were prepared with die casting and melt spinning techniques, further processed using cold rolling and cryomilling, and finally annealed below the estimated order–disorder temperature (T_OD). To study the influence of composition and processing of the alloys, structural characterization and microstructural analysis were performed with synchrotron radiation X-ray diffractometry (SR-PXD) and Scanning Transmission Electron Microscopy (STEM), respectively. The presence of tetrataenite in the alloys investigated in this work could not be confirmed. In situ SR-PXD and STEM indicated minimal structural changes in the temperature stability range of the materials. A full-loop hysteresis curve acquired using a vibrating sample magnetometer (VSM) indicated no signs of magnetic hardening of the alloys with the measured coercivity being below 10 Oe, and thus consistent with FeNi without ordering. Full article

To determine the structure of carbohydrate polymers using conventional analytical technology, several complicated steps are required. We instead adopted a direct approach without the need for pretreatments, using an intense infrared (IR) laser for carbohydrate analysis. IR free-electron lasers (FELs) driven by a linear accelerator possess unique spectroscopic features, including extensive wavelength tunability and high laser energy in the IR region from 1000 cm⁻¹ (10 μm) to 4000 cm⁻¹ (2.5 μm). FELs can induce IR multiphoton dissociation reactions against various molecules by supplying vibrational excitation energy to the corresponding chemical bonds. Chitin from crayfish and cellulose fiber were irradiated by FELs tuned to νC–O (9.1–9.8 μm), νC–H (3.5 μm), and δH–C–O (7.2 μm) in glycosidic bonds, and their low-molecular-weight sugars were separated, which were revealed by combining synchrotron radiation IR spectroscopy and electrospray ionization mass spectrometry. An intense IR laser can be viewed as a “molecular scalpel” for dissecting and directly analyzing the internal components in rigid biopolymers. This method is simple and rapid compared with general analytical techniques. Full article

The development of molecules that interact with G-quadruplex (G4) sequences requires effective evaluation methods. Several techniques are currently available, including nuclear magnetic resonance (NMR) spectroscopy and X-ray crystallography, surface plasmon resonance (SPR), isothermal titration calorimetry (ITC) and mass spectrometry (MS), fluorescence using FRET-melting, G4-fluorescent intercalator displacement assay (G4-FID) and affinity chromatography. Among these, CD spectroscopy is gaining prominence due to its lower material requirements, faster experimentation and quicker data processing. However, conventional CD methods have limitations, such as higher sample volume required and the inability to handle high-throughput analysis efficiently. The use of synchrotron radiation in high-throughput analysis methods (HT-SRCD) has further advanced the investigation of small-molecule interactions with DNA G4 structures in the presence of various monovalent cations. HT-SRCD offers the capability to analyze multiple samples simultaneously, overcoming the limitations of conventional CD methods. To validate this approach, three biologically relevant G4 sequences—HTelo1, G3T3 and T95-2T—were investigated. Their interactions with a library of small tetrazole-based molecules, synthesized via a four-component Ugi reaction, and with a peptide sequence deriving from RHAU helicases (Rhau25), were evaluated. The results demonstrate that this method not only effectively discriminates between different ligands but also provides valuable insights into the selectivity and the modes of interaction of these ligands with the G4 sequences. Full article

Complex oxides with the general formula Gd₂(Ti_1−xZr_x)₂O₇ are promising candidates for radioactive waste immobilization due to their capacity to withstand radiation by dissipating part of the free energy driving defect creation and phase transitions. In this study, samples with varying zirconium content (xZr = 0.00, 0.15, 0.25, 0.375, 0.56, 0.75, 0.85, 1.00) were synthesized via the sol–gel method and thermally treated at 500 °C to obtain nanosized powders mimicking the defective structure of irradiated materials. Synchrotron-based techniques were employed to investigate their structural properties: High-Resolution X-ray Powder Diffraction (HR-XRPD) was used to assess long-range structure, while Pair Distribution Function (PDF) analysis and Extended X-ray Absorption Fine Structure (EXAFS) spectroscopy provided insights into the local structure. HR-XRPD data revealed that samples with low Zr content (xZr ≤ 0.25) are amorphous. Increasing Zr concentration led to the emergence of a crystalline phase identified as defective fluorite (xZr = 0.375, 0.56). Samples with the highest Zr content (xZr ≥ 0.75) were fully crystalline and exhibited only the fluorite phase. The experimental G(r) functions of the fully crystalline samples in the low r range are suitably fitted by the Weberite structure, mapping the relaxations induced by structural disorder in defective fluorite. These structural insights informed the subsequent EXAFS analysis at the Zr-K and Gd-L₃ edges, confirming the splitting of the cation–cation distances associated with different metal species. Moreover, EXAFS provided a local structural description of the amorphous phases, identifying a consistent Gd-O distance across all compositions. Full article

X-ray ptychography is an ultrahigh resolution imaging technique widely used in synchrotron radiation facilities. Its imaging performance relies on the quality of the acquired signals. However, the X-ray detectors used often suffer from signal loss due to sensor gaps, beamstops, defective pixels, overexposure, or other factors, resulting in degraded image quality. To suppress and compensate for the effects of signal loss, we proposed the known probe approach to partially recover the lost signals and introduced the high probe divergence strategy by investigating the effects of probe divergence on reconstruction quality under signal loss conditions. Both simulation and experiment results show that high probe divergence can effectively suppress the impact of signal loss on reconstruction quality while using a known probe as the initial probe for reconstruction can largely recover missing signals in Fourier space, resulting in a much better image than using a guessed initial probe. These strategies allow for high-quality imaging in the presence of signal loss without secondary data acquisition, significantly improving experimental efficiency and reducing radiation damage compared to previous strategies. Full article

Synchrotron radiation light sources have been successfully utilized in material science, biomedicine, and other fields due to their high intensity, excellent monochromaticity, coherence, and collimation. In recent years, synchrotron radiation has significantly expedited the advancement of medical applications, particularly through innovations in imaging and radiotherapy. For instance, synchrotron X-ray imaging has enabled high-contrast and spatial–temporal resolution images for early-stage diagnosis of breast cancer and cardiovascular diseases, offering superior diagnostic accuracy compared to conventional methods. Additionally, novel synchrotron radiation-based radiotherapy techniques, such as microbeam therapy and stereotactic radiotherapy, have shown great potential for clinical application by enabling precise tumor targeting while minimizing damage to surrounding healthy tissues. These advancements are projected to redefine imaging diagnostics and therapeutic strategies, particularly for resistant cancers, by offering enhanced precision, reduced radiation doses, and improved therapeutic outcomes. This review provides an overview of synchrotron radiation beamline characteristics, recent breakthroughs in imaging and radiotherapy, and their emerging applications in treating heart, breast, lung, bone, and brain conditions. Full article

Fat polymorphism plays a critical role in the structural and functional properties of fat-based food products. However, research on the polymorphism of monoglyceride oleogels remains limited. Previous work demonstrated the impact of composition and processing on the polymorphic transitions of monoglyceride oleogels, indicating that high shear and cooling rates accelerate β-polymorph formation. However, a detailed understanding on the effect of shear is still lacking. This research extends previous observations by using a CSS450 shear cell, allowing for precise control over cooling and shear rates. Two commercially available food-grade monoglycerides were mixed with rapeseed oil (10% w/w). Crystallization was performed with varying shear rates and analyzed with synchrotron radiation X-ray scattering techniques (SAXS and WAXS), differential scanning calorimetry and microscopy. The results showed that applying a low shear rate did not result in changes in the polymorphic transitions compared to static crystallization for both monoglyceride oleogels. However, increasing the shear rate resulted in the formation of the β-polymorph, even before the formation of the metastable sub-α polymorph. These findings provide new insights into the role of shear in monoglyceride oleogels, allowing for further optimization of fat structuring in food applications. Full article