Search Results (94)

This study investigates a 26th Dynasty Ptah–Sokar–Osiris wooden statuette excavated from the Tari cemetery, Giza Pyramids area, to decode ancient Egyptian manufacturing techniques and establish evidence-based conservation strategies of such wooden objects. Using minimal sampling (1.0–2.0 mm²), integrated XRF, synchrotron-based X-ray diffraction, FTIR, and confocal microscopy distinguished original technological choices from burial-induced alterations. The 85 cm Vachellia nilotica sculpture exhibits moderate structural preservation (cellulose crystallinity index 62.9%) with partial chemical deterioration (carbonyl index 2.22). Complete pigment characterization identified carbon black, Egyptian Blue (cuprorivaite, 55 ± 5 wt %), atacamite-dominated green (65 ± 5 wt %) with residual malachite (10 ± 2 wt %), orpiment (60 ± 5 wt %), red ochre (hematite, 60% ± 5 wt %), white pigments (93 ± 5 wt % calcite), and metallic gold (40 ± 5 wt %). Confocal microscopy revealed sophisticated multi-pigment mixing strategies, with black carbon systematically blended with chromophores for nuanced color effects. Atacamite predominance over malachite provides evidence for chloride-mediated diagenetic transformation over 2600 years of burial. Consistent calcite detection (~ 20–45%) across colored layers confirms systematic ground layer application, establishing technological baseline data for 26th Dynasty Lower Egyptian workshops. Near-complete organic binder loss, severe lignin oxidation, and ongoing salt-mediated mineral transformations indicate urgent conservation needs requiring specialized consolidants, paint layer stabilization, and controlled environmental storage. This investigation demonstrates synchrotron methods’ advantages while establishing a minimally invasive framework for studying polychrome wooden artifacts. Full article

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

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

Three-dimensionally (3D)-printed catalytic structures are revolutionizing catalysis and chemical engineering. Unlike traditional supports, modern triply periodic minimal surfaces (TPMS), lattices, and fractals actively influence mass and heat transfer and flow distribution. This review summarizes advancements in the classification, design, fabrication, and application of 3D-printed catalysts over the past decade. The article covers various constructive types (supports, integrated phases, multifunctional reactors) and materials (polymers, ceramics, metals, hybrids), along with fabrication techniques compliant with ISO/ASTM standards (FDM, SLA, DIW, SLM, EBM). It emphasizes post-processing and functionalization strategies (impregnation, calcination, sulfonation) and characterization tools (SAXS, CT, synchrotron-based techniques). A critical comparison highlights advantages, including tunable geometry, improved hydrodynamics, lower pressure drop, enhanced durability, and reproducibility. Three-dimensionally printed catalysts are an interdisciplinary platform combining materials science, chemical engineering, and digital manufacturing. They hold promise for sustainable chemistry, modular production, CO₂ utilization, photocatalysis, and biocatalysis, making them a key innovation for future catalytic reactors. 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

Double perovskites are represented by the formula A₂BB’O₆ and AA’BB’O₆. These materials have been synthesized using the solid-state reaction, sol–gel, Pechini, and hydrothermal methods. X-ray fluorescence, X-ray diffraction, magnetic measurements, transmission electron microscopy, X-ray photoelectron spectroscopy, temperature-programmed reduction, synchrotron X-ray diffraction, neutron powder diffraction, extended X-ray absorption fine structure, and Raman spectroscopy have been used for the characterization of double perovskites. X-ray diffraction, synchrotron X-ray diffraction, and neutron powder diffraction coupled with the Rietveld method determine the crystal structure of a sample. These materials present various properties and applications. The present review aims (i) to report a process to determine the symmetry, apparent size, and apparent strain using the Rietveld method; (ii) show how experimental characterization techniques complement each other in the investigation of double perovskites; (iii) describe how the synthesis method can help in the uncovering of double perovskites with improved properties; and (iv) exemplify some of the main applications of double perovskites. 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

Solid-state lithium batteries (SSLBs) have emerged as a promising alternative to conventional lithium-ion systems due to their superior safety profile, higher energy density, and potential compatibility with lithium metal anodes. However, a major challenge hindering their widespread deployment is the formation and growth of lithium dendrites, which compromise both performance and safety. This review provides a comprehensive and structured overview of recent advances in dendrite suppression strategies, with special emphasis on the role played by the nature of the solid electrolyte. In particular, we examine suppression mechanisms and material innovations within the three main classes of solid electrolytes: sulfide-based, oxide-based, and polymer-based systems. Each electrolyte class presents distinct advantages and challenges in relation to dendrite behavior. Sulfide electrolytes, known for their high ionic conductivity and good interfacial wettability, suffer from poor mechanical strength and chemical instability. Oxide electrolytes exhibit excellent electrochemical stability and mechanical rigidity but often face high interfacial resistance. Polymer electrolytes, while mechanically flexible and easy to process, generally have lower ionic conductivity and limited thermal stability. This review discusses how these intrinsic properties influence dendrite nucleation and propagation, including the role of interfacial stress, grain boundaries, void formation, and electrochemical heterogeneity. To mitigate dendrite formation, we explore a variety of strategies including interfacial engineering (e.g., the use of artificial interlayers, surface coatings, and chemical additives), mechanical reinforcement (e.g., incorporation of nanostructured or gradient architectures, pressure modulation, and self-healing materials), and modifications of the solid electrolyte and electrode structure. Additionally, we highlight the critical role of advanced characterization techniques—such as in situ electron microscopy, synchrotron-based X-ray diffraction, vibrational spectroscopy, and nuclear magnetic resonance (NMR)—for elucidating dendrite formation mechanisms and evaluating the effectiveness of suppression strategies in real time. By integrating recent experimental and theoretical insights across multiple disciplines, this review identifies key limitations in current approaches and outlines emerging research directions. These include the design of multifunctional interphases, hybrid electrolytes, and real-time diagnostic tools aimed at enabling the development of reliable, scalable, and dendrite-free SSLBs suitable for practical applications in next-generation energy storage. Full article

This study systematically investigated the corrosion evolution and protective mechanisms of X80 pipeline steel in Xinjiang’s saline soil environments under freeze–thaw cycling conditions. Combining regional soil characterization with laboratory-constructed corrosion systems, we employed electrochemical impedance spectroscopy, potentiodynamic polarization, and surface analytical techniques to quantify temporal–spatial corrosion behavior across 30 freeze–thaw cycles. Experimental results revealed a distinctive corrosion resistance pattern: initial improvement (cycles 1–10) attributed to protective oxide layer formation, followed by accelerated degradation (cycles 10–30) due to microcrack propagation and chloride accumulation. Synchrotron X-ray diffraction analyses identified sulfate–chloride ion synergism as the primary driver of localized corrosion disparities in heterogeneous soil matrices. A comparative evaluation of asphalt-coated specimens demonstrated a 62%–89% corrosion rate reduction, with effectiveness directly correlating with coating integrity and thickness (200–500 μm range). Molecular dynamics simulations using Materials Studio revealed atomic-scale ion transport dynamics at coating–substrate interfaces, showing preferential Cl⁻ permeation through coating defects. These multiscale findings establish quantitative relationships between environmental stressors, coating parameters, and corrosion kinetics, providing a mechanistic framework for optimizing protective coatings in cold-region pipeline applications. Full article

This study presents a multi-analytical investigation of the wooden components from Khufu’s Second Solar Boat, one of the valuable archaeological discoveries in ancient Egypt. The research integrates advanced imaging and analytical techniques to identify wood species, assess deterioration patterns, and characterize the fungal and bacterial biodeteriogens. The initial visual examination documented the state of preservation at the time of discovery. Subsequently, the identification of the wood species was carried out. The deterioration status was assessed using a variety of tools, including scanning electron microscopy (SEM) and high-resolution synchrotron radiation computed microtomography (SR-μCT) for morphological alterations, X-ray diffraction (XRD) for crystallinity changes and Fourier-transform infrared spectroscopy (FTIR) to assess chemical degradation indexes of wood. Moreover, molecular techniques were used to identify and characterize the presence of biodeterioration agents. Results indicate that ancient craftsmen used cedar wood for the boat construction. The analysed samples exhibited advanced biotic and abiotic degradation, as evidenced by microbiological assessments, XRD measurements of cellulose crystallinity, FTIR indices, SEM micrographs and SR-μCT data. These results provide crucial insights into the long-term degradation processes of archaeological wood in arid environments, enhancing our understanding of ancient Egyptian woodworking practices and informing future conservation strategies for similar artifacts. Full article

A 3D-printable, ARDUINO-based multipurpose X-ray stage of compact dimensions enabling in situ electric field and temperature-dependent measurements is put into practice and tested here. It can be routinely applied in combination with a technique of structural characterization of materials. Using high-performance X-ray laboratory equipment, two investigations were conducted to illustrate the device’s performance. The lattice characteristics and microstructure evolution of piezoelectric ceramics of barium titanate, BaTiO₃ (BT), and barium calcium zirconate titanate, with compositions of (Ba_0.92Ca_0.08) (Ti_0.95Zr_0.05)O₃ (BC8TZ5), were studied as a function of the applied electric field and temperature. The X-ray stage is amenable as an off-the-shelf device for a diffraction line in a synchrotron. It provides valuable information for poling piezoceramics and subsequent optimization of their performance. Full article

This study employs advanced structural characterization techniques, including anomalous small-angle X-ray scattering (ASAXS), small-angle X-ray scattering (SAXS), and X-ray photoelectron spectroscopy (XPS), to investigate erbium (Er³⁺)-doped silica-based glass-ceramic thin films synthesized via the sol–gel method. This research examines the SiO₂-TiO₂ and SiO₂-TiO₂-PO_2.5 systems, focusing on the formation, dispersion, and structural integration of Er³⁺-containing nanocrystals within the amorphous matrix under different thermal treatments. Synchrotron radiation tuned to the L_III absorption edge of erbium enabled ASAXS measurements, providing element-specific details about the localization of Er³⁺ ions. The findings confirm their migration into crystalline phases, such as erbium phosphate (EPO) and erbium titanate (ETO). SAXS and Guinier analysis quantified nanocrystal sizes, revealing trends influenced by their composition and heat treatment. Complementary XPS analysis of the Er 5p core-level states provided detailed information on the chemical and electronic environment of the Er³⁺ ions, confirming their stabilization within the crystalline structure. Transmission electron microscopy (TEM) highlighted the nanoscale morphology, verifying the aggregation of Er³⁺ ions into well-defined nanocrystals. The results offer a deeper understanding of their size, distribution, and interaction with the surrounding matrix. Full article

This study explores the use of shape memory alloys, specifically nickel-titanium (NiTi- Ti-rich), in plate joining processes through riveting. Through the shape memory effect (SME), SMAs offer innovative solutions for joining components, mainly in the aeronautical and aerospace fields, indicating their promising applications. This research presents several characterizations, including differential scanning calorimetry, compression dilatometry, X-ray diffraction using synchrotron radiation, and thermomechanical testing, to assess the feasibility and performance of shape memory alloy rivets. In addition, the samples were subjected to recrystallization heat treatment to evaluate their reusability. The results demonstrated that shape memory alloy rivets are effective, achieving a maximum load of 340 N for two joined components. However, their application is optimal for materials with yield strengths lower than the stress-induced SME. Moreover, the process enhances the joined components’ hardening and increases the rivet’s thermal hysteresis. This research confirms the viability of shape memory alloys for riveting processes, offering a new avenue for advanced joining techniques. The findings provide a foundation for their further development and application in various industries requiring precise and reliable joining methods. Full article

Serial femtosecond crystallography (SFX) with X-ray free-electron lasers (XFELs) has revolutionized classical X-ray diffraction experiments by utilizing ultra-short, intense, and coherent X-ray pulses. However, the SFX approach still requires thousands of nearly identical samples, leading to significant protein consumption. We propose utilizing Langmuir–Blodgett protein multilayers, which are characterized by long-range order, thermal stability, and the ability to induce protein crystallization, even in proteins that cannot be crystallized by conventional methods. This study aimed to combine the intrinsic properties of Langmuir–Blodgett multilayers with advanced XFEL techniques at the Linac Coherent Light Source. Since the macromolecule organization can be explored in nano or 2D crystals exploiting the properties of SFX–XFEL radiation that enable the capture of high-resolution diffraction images before radiation damage occurs, we propose Langmuir–Blodgett protein nanofilm technology as a novel approach for direct “on-chip” protein sample preparation. The present study extends previous investigations into Langmuir–Blodgett phycocyanin multilayer nanofilms using synchrotron radiation cryo-EM microscopy and second-order nonlinear imaging of chiral crystal (SONICC) experiments. We also examined the thermal stability of phycocyanin Langmuir–Blodgett multilayered films deposited on Si₃N₄ membranes to evaluate structural changes occurring at 150 °C compared with room temperature. Phycocyanin Langmuir–Blodgett films are worthy of investigation in view of their suitability for tissue engineering and other applications due to their thermal integrity and stability as the results of the present investigation reveal. Full article

In cultural heritage, paint stratigraphies are complex systems typically consisting of various paint layers with fine crystalline phases mixed with coarse pigment and filler grains. This complexity poses significant challenges for X-ray diffraction (XRD) analysis. In this work, we employed synchrotron radiation micro-X-ray diffraction in transmission geometry (SR-µTXRD) with linear mapping to develop a novel approach for studying the crystalline phases (pigments and fillers) in mock-up paint stratigraphies. A targeted approach was followed for qualitative, quantitative, and microstructural analysis, combining signals from micrometric crystallites and coarse single crystals as well as from randomly oriented and iso-oriented crystalline phases. This allows for identifying, localizing, and quantifying these phases even in low fractions and distinguishes the same phases across different layers with varying grain sizes or spatial orientations. Critical analysis of 2D XRD patterns, coupled with full-profile fitting performed by the Rietveld method, provides insights into material preparation (e.g., grinding), painting technique (e.g., color palette, use of fillers, brushing), and crystallo-chemical modifications over time. This analytical approach, integrating spatially resolved investigation with high-quality phase characterization, enhances the potential of specific XRD methodologies for a 2D investigation of multi-phase materials in cultural heritage, even without dedicated micro-mapping techniques. Full article