Search Results (661)

La-doped ZnO nanoclusters confined within mesoporous SBA-15 were synthesized using an impregnation–calcination method and evaluated for their visible-light-driven photocatalytic degradation of Rhodamine B (RhB). Small-angle X-ray diffraction (XRD) and transmission electron microscopy (TEM) confirmed the preservation of the 2D hexagonal mesostructure of SBA-15 post-loading. In contrast, wide-angle XRD and Fourier-transform infrared spectroscopy (FT-IR) analyses revealed that the incorporated ZnO existed predominantly as highly dispersed amorphous or ultrafine clusters within the mesopores. N₂ adsorption–desorption measurements exhibited Type IV isotherms with H1 hysteresis loops. Compared to pristine SBA-15, the specific surface area and pore volume of the composites decreased from 729.35 m² g⁻¹ to 521.32 m² g⁻¹ and from 1.09 cm³ g⁻¹ to 0.85 cm³ g⁻¹, respectively, accompanied by an apparent increase in the average pore diameter from 5.99 nm to 6.55 nm, attributed to non-uniform pore occupation. Under visible-light irradiation, the photocatalytic performance was highly dependent on the La doping level. Notably, the 5% La-ZnO/SBA-15 sample exhibited superior activity, achieving over 99% RhB removal within 40 min and demonstrating the highest apparent rate constant (k = 0.1152 min⁻¹), surpassing both undoped ZnO/SBA-15 (k = 0.0467 min⁻¹) and other doping levels. Reusability tests over four consecutive cycles showed a consistent degradation efficiency exceeding 93%, with only a ~7 percentage-point decline, indicating excellent structural stability and recyclability. Radical scavenging experiments identified h⁺, ·OH, and ·O₂⁻ as the primary reactive species. Furthermore, photoluminescence (PL) quenching observed at the optimal 5% La doping level suggested suppressed radiative recombination and enhanced charge carrier separation. Collectively, these results underscore the synergistic effect of La doping and mesoporous confinement in achieving fast, efficient, and recyclable photocatalytic degradation of organic pollutants. 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

Gamma-ray bursts (GRBs) are widely recognized to exhibit jet-like emission structures, though previous studies often assumed isotropic emission due to observational constraints. This assumption limited our understanding of the intrinsic properties of GRBs. Here, we analyze 40 GRBs with observed X-ray plateaus and jet features, all with measured redshifts. By applying jet corrections to prompt and plateau-phase quantities, we probe their intrinsic behavior. We find that the jet-corrected prompt emission energy ($E_{jet}$) depends less strongly on the jet-corrected X-ray luminosity at the end of the plateau ($L_{X,jet}$). An anti-correlation is also observed between the jet opening angle (${\theta }_{jet}$) and the rest frame peak energy ($E_{p,z}$): $E_{p,z}\propto {\theta }_{jet}^{-0.44\pm 0.13}$ for ISM and $E_{p,z}\propto {\theta }_{jet}^{-0.78\pm 0.13}$ for wind environments, indicating that more collimated jets yield higher peak energies. After jet correction, the $L_X$-$T_{a,z}$ correlation and the three-parameter $L_X$-$T_{a,z}$-$E_{\gamma ,iso}$, $L_X$-$T_{a,z}$-$L_p$ and $L_X$-$T_{a,z}$-$E_{p,z}$ relations are generally weakened. Among these, the first three remain relatively stable, suggesting they reflect intrinsic GRB physics, whereas the $L_X$-$T_{a,z}$-$E_{p,z}$ relation weakens significantly, implying it may be an artifact of the isotropic assumption. We also identify a new three-parameter correlation: ${\theta }_{jet}\left(ISM\right)\propto E_{jet}{\left(ISM\right)}^{0.36\pm 0.06}{E}_{p,z}^{-0.62\pm 0.09}$, ${\theta }_{jet}\left(Wind\right)\propto E_{jet}$${\left(Wind\right)}^{0.29\pm 0.09}$$E_{p,z}^{-0.61\pm 0.09}$. Full article

In response to the increasing consumer demand for healthier diets and the needs of individuals with gluten intolerance, chestnut flour (CF) emerges as a valuable unconventional ingredient for sustainable and functional nutrition. This study evaluated the nutritional, phytochemical, and functional properties of gluten-free biscuits formulated with whole rice flour (RF), CF, and their mixtures, where RF was replaced by CF at 0% (control), 10%, 30%, 70%, 90%, and 100% (w/w). In addition, in the 50% CF formulation, 5% of RF was substituted with fruit powders rich in phenolic compounds and recognized as fortifying agents, such as chokeberry (CP), açaí (AP), and blueberry (BP). Proximate composition, macro- and microelement content, total phenolic content (TPC), total flavonoid content (TFC), and antioxidant activity (DPPH and FRAP assays) were determined for the individual flours, composite flours, fruit powders, and biscuit formulations. Structural characteristics were assessed using Small- and Wide-Angle X-ray Scattering (SAXS/WAXS) analysis and Fourier Transform Infrared Spectroscopy (FTIR). Results showed that CF incorporation enhanced both the nutritional and functional profile of flours and biscuits, increasing protein, fiber, lipid, and mineral contents while reducing carbohydrates, and improving TPC, TFC, DPPH, and FRAP values. Fortification with 5% CP, AP, or BP further boosted the phytochemical content of the biscuits, with the chokeberry-enriched sample exhibiting the highest TPC (348.88 mg GAE/100 g d.s.), TFC (253.82 mg QE/100 g d.s.), DPPH (50.36%), and FRAP (21.07 μM Fe²⁺/g d.s.). The combination of 50% CF and 5% CP provided dual benefits, significant bioactive enrichment alongside the preservation of desirable technological properties. Complementary SAXS/WAXS and FTIR analyses indicated that CF and fruit powders enhanced molecular interactions and matrix cohesion, which may contribute to improved texture and antioxidant potential of the biscuits. Overall, this formulation offers a promising and practical approach to developing functional gluten-free biscuits with enhanced nutritional, phytochemical, functional, and structural characteristics. Full article

Inert polymeric implants must evolve to enhance their biological interactions with host tissue, triggering positive cellular responses and promoting tissue bonding and integration. Poly-ether-ether-ketone (PEEK) is widely used as an implant material; however, its inert nature results in limited biological interactions. Various surface modification techniques have been investigated to enhance its bioactivity and overall biological performance. In this study, the PEEK surface was bioactivated through a chemical treatment involving two steps: surface activation using low-pressure oxygen plasma, followed by biofunctionalization with phosphate and calcium ions. Comprehensive surface characterization by contact angle, scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and Fourier-transform infrared (FT-IR) confirmed the effect of plasma and the ionic surface incorporation. The biological response was evaluated through cell viability, adhesion, and proliferation in NIH/3T3 fibroblasts and HOS osteoblasts, and the results indicated the efficacy of the surface modifications. Therefore, the proposed treatments provide an efficient strategy to improve the biological performance of PEEK-based implants. Full article

Phase angle (PhA) is a widely used bioimpedance index associated with cell mass, membrane integrity, skeletal muscle mass and quality, and body fluid distribution. This study aims to investigate the relationship between PhA and body fat, which is poorly defined in the current literature. The analysis involved 1533 adults of both sexes from the National Health and Nutrition Examination Survey. Anthropometry, bioimpedance analysis, and dual-energy X-ray absorptiometry were used to estimate body mass index (BMI), PhA (at 50 kHz), and body fat, respectively. Non-linear cubic spline regression models were applied to examine the associations between PhA and fat mass (FM), BMI, fat mass index (FMI), and FM%. The relationship between PhA and body fat was non-linear. An initial positive slope was observed with FM, FMI and BMI, followed by a decline, whereas FM% exhibited a flatter initial pattern before decreasing. Men showed more pronounced flection points, at lower fat levels (FM: 23 kg; FMI: 9 kg/m²; BMI: 37 kg/m²; FM%: 25.5%) than women (FM: 34 kg; FMI: 16 kg/m²; BMI: 32 kg/m²; FM%: 42.5%). Although most associations were significant, the explained variance of the relationships was lower than 10%. In conclusion, this study demonstrates a weak and non-linear relationship between PhA and body fat. This suggests that PhA variability is predominantly influenced by factors other than fat, a point that warrants consideration in both clinical and routine practice. Full article

Due to industrialization and globalization, water sources are increasingly contaminated with drugs. Among the various methods available, adsorption remains one of the most widely used techniques for drug removal. This work was to develop polysulfone (PSF) membranes integrated with montmorillonite (MMT) clay. The fabricated membranes were subsequently evaluated for their performance in removing diclofenac (DCF) from aqueous solutions. The membranes were characterized using scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FTIR), contact angle measurements, as well as chemical and mechanical tests. Adding MMT at 1.5 and 2 wt% improved both hydrophilicity and mechanical strength. The natural hydrophilicity of MMT also accelerates the non-solvent/solvent exchange during phase inversion, resulting in higher porosity. These structural and surface modifications increased water permeability (16.36 L·m⁻²·h⁻¹·bar⁻¹), achieved 79% DCF removal, and enhanced antifouling properties. However, increasing the MMT clay content to 2.5 wt% caused particle aggregation, which reduced membrane performance. Fouling resistance tests with bovine serum albumin (BSA) as a model foulant showed a rejection rate of 89% and a flux recovery ratio (FRR) above 82% using an optimized membrane. These findings demonstrate that PSF/MMT membranes can serve as promising candidates for sustainable pharmaceutical wastewater treatment. Full article

This paper presents a study of the thermal and rheological properties of isosorbide, showing that its degradation temperature (around 100 °C) is much lower than values previously proposed in the literature. Furthermore, remarkable calorimetric and viscoelastic behaviors, with features usually observed in semi-crystalline systems are presented. The onset of the melting is measured at 45 °C, while a glass transition occurs at −45 °C, followed by cold crystallization. Wide-angle X-ray diffraction confirmed the coexistence of crystalline domains and an amorphous fraction, which behaves as a molecular glass, with an estimated crystallinity of approximately 70%. Thermogravimetric analyses conducted under both air and nitrogen and at multiple heating rates, in line with ICTAC recommendations, established the robustness of the 100 °C degradation onset. These findings provide new structure–property relationships for isosorbide and open up new avenues for further research and development in this area. Full article

Two heteroaromatic hybrid compounds were synthesized and characterized using various analytical techniques. The results indicate that the benzimidazole/oxadiazole (BZ/OZ) metal derivative exhibits a tridentate coordination mode, where the carbonyl, imidazole and oxadiazole groups participate in coordination with the metal, in a ratio of 2:1 of the ligand to the metal. The antibacterial activities of the organic ligand and its metal complex were determined by in vitro tests against both Gram-positive bacterial strains and Gram-negative bacterial strains using the broth microdilution method. The metal complex showed greater antibacterial activities compared to the precursor ligand against all evaluated microorganisms. The results obtained through in silico predictions revealed significant toxicological differences among the analyzed molecules, suggesting special attention in the use of the ligand due to its possible carcinogenicity in mice and a need for structural modifications in the complex to reduce its carcinogenicity and toxicity. Furthermore, a biophysical study of the interaction of the BZ/OZ derivatives with different model membranes was explored through differential scanning calorimetry (DSC), simultaneous small- and wide-angle X-ray diffraction (SAXD and WAXD) and infrared spectroscopy (FT-IR). The results indicate that the compounds influenced membrane properties without significantly altering the lamellar organization. The findings suggest potential applications in understanding lipid interactions, elucidating toxicology and developing antibacterial agents. Full article

A series of PTT-b-PTMG copolyesters was synthesized via direct esterification followed by melt polycondensation using purified terephthalic acid (PTA), bio-based 1,3-propanediol (PDO), and poly(tetramethylene glycol) (PTMG) of varying molecular weights (650–3000 g/mol). The resulting materials were comprehensively characterized in terms of chemical structure, molecular weight, thermal behavior, phase morphology, crystalline architecture, and mechanical performance using a range of analytical techniques: Fourier-transform infrared spectroscopy (FTIR), ¹H-NMR, gel permeation chromatography (GPC), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), wide-angle X-ray scattering (WAXS), small-angle X-ray scattering (SAXS), dynamic mechanical thermal analysis (DMA), tensile testing, and other standard physical methods. FTIR, ¹H-NMR, and GPC data confirmed the successful incorporation of both PTT-hard and PTMG-soft segments into the copolymer backbone. As the PTMG molecular weight increased, the average sequence length of the PTT-hard segments (L_n,T) also increased, leading to higher melting (T_m) and crystallization (T_c) temperatures, albeit with a slight reduction in overall crystallinity. DMA results indicated enhanced microphase separation between hard and soft domains with increasing PTMG molecular weight. WAXS and SAXS analyses further revealed that the crystalline structure and long-range ordering were strongly dependent on the copolymer composition and block architecture. Mechanical testing showed that tensile strength at break remained relatively constant across the series, while Young’s modulus increased significantly with higher PTMG molecular weight—concurrently accompanied by a decrease in elongation at break. Furthermore, the elastic deformability and recovery behavior of PTT-b-PTMG block copolymers were evaluated through cyclic tensile testing. TGA confirmed that all copolyesters exhibited excellent thermal stability. This study demonstrates that the physical and mechanical properties of bio-based PTT-b-PTMG elastomers can be effectively tailored by adjusting the molecular weight of the PTMG-soft segment, offering valuable insights for the rational design of sustainable thermoplastic elastomers with tunable performance. Full article

Thermoelectric (TE) materials represent a critical frontier in sustainable energy conversion technologies, providing direct thermal-to-electrical energy conversion with solid-state reliability. The optimizations of TE performance demand a nuanced comprehension of structure–property relationships across diverse length scales. This review summarizes established and emerging spectroscopic and microscopic techniques used to characterize inorganic and polymer TE materials, specifically poly(3,4-ethylenedioxythiophene): poly(styrenesulfonate) (PEDOT:PSS). For inorganic TE, ultraviolet–visible (UV–Vis) spectroscopy, energy-dispersive X-ray (EDX) spectroscopy, and X-ray photoelectron spectroscopy (XPS) are widely applied for electronic structure characterization. For phase analysis of inorganic TE materials, Raman spectroscopy (RS), electron energy loss spectroscopy (EELS), and nuclear magnetic resonance (NMR) spectroscopy are utilized. For analyzing the surface morphology and crystalline structure, chemical scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD) are commonly used. For polymer TE materials, ultraviolet−visible–near-infrared (UV−Vis−NIR) spectroscopy and ultraviolet photoelectron spectroscopy (UPS) are generally employed for determining electronic structure. For functional group analysis of polymer TE, attenuated total reflectance–Fourier-transform infrared (ATR−FTIR) spectroscopy and RS are broadly utilized. XPS is used for elemental composition analysis of polymer TE. For the surface morphology of polymer TE, atomic force microscopic (AFM) and SEM are applied. Grazing incidence wide-angle X-ray scattering (GIWAXS) and XRD are employed for analyzing the crystalline structures of polymer TE materials. These techniques elucidate electronic, structural, morphological, and chemical properties, aiding in optimizing TE properties like conductivity, thermal stability, and mechanical strength. This review also suggests future research directions, including in situ methods and machine learning-assisted multi-dimensional spectroscopy to enhance TE performance for applications in electronic devices, energy storage, and solar cells. Full article

Epoxy resins are valuable in aerospace, electronics, and high-performance industries; however, their inherently low thermal conductivity (TC) limits applications requiring effective heat dissipation. Recent reports suggest that certain liquid crystalline or partially crystalline epoxy formulations can achieve higher TC, even exceeding 1 W/(m·K). To investigate this, 17 epoxy formulations were prepared, including the commonly used diglycidyl ether of bisphenol A (DGEBA) and two custom-synthesized diepoxides: TME4, which contains rigid aromatic ester linkages with a C4 aliphatic spacer, and LCE-DP, featuring rigid imine bonds. Thermal conductivity was measured using four techniques: laser flash analysis (LFA), modified transient plane source (MTPS), time-domain thermoreflectance (TDTR), and displacement thermo-optic phase spectroscopy (D-TOPS). Additionally, small-angle and wide-angle X-ray scattering (SAXS/WAXS) were performed to detect crystalline or liquid crystalline domains. All formulations exhibited TC values ranging from 0.13 to 0.32 W/(m·K). The TME4–DDS systems, previously reported to be near 1 W/(m·K), consistently measured between 0.26 and 0.30 W/(m·K). Thus, under our synthesis and curing conditions, the elevated TC reported in prior studies was not reproduced, and no strong evidence of crystallinity was observed; indications of local ordering did not translate into higher conductivity. Variations in TC among methods often matched or exceeded the gains attributed to mesophase formation. More broadly, evidence for crystallinity in epoxy thermosets appears weak, consistent with the notion that crosslinking suppresses long-range ordering. Full article

The microstructure of polyacrylonitrile (PAN) precursor fibers has a profound influence on the performance of carbon fibers and depends on the spinning processes and processing conditions. This study compared the evolution of the microstructures and performance of PAN fibers between the wet-spinning and dry-jet wet-spinning processes, utilizing scanning electron microscopy, small/wide-angle X-ray scattering, dynamic mechanical analysis, and single-fiber tensile testing. Both spinning processes promoted the oriented alignment of microfibrils and fibrils, improved the crystal arrangement and molecular regularity, and facilitated the transition from a two-phase (crystalline/amorphous) structure to a single-phase structure, thereby gradually improving the fibers’ elastic character and mechanical properties. However, wet-spun fibers exhibited inherent defects (skin-core structure and large voids), which caused surface grooves, radial mechanical heterogeneity, and low breaking elongation during post-spinning. In contrast, dry-jet wet-spun fibers initially had a smooth surface and a homogeneous radial structure, which evolved into well-oriented, radially homogeneous structures during post-spinning. Furthermore, the dry-jet wet-spinning process produced greater increases in crystallinity (46%), crystal size (258%), and orientation index (146%) than the wet-spinning process did. The dry-jet wet-spinning process’s superiority in forming and optimizing the fiber microstructure gives it greater potential for producing high-quality PAN precursor fibers. Full article

With the increase in contamination by microbial agents (bacteria, viruses, etc.) in the fields of agri-food, healthcare, and environment, it is necessary to detect and quantify these biological elements present in complex fluids in a short time with high selectivity, high sensitivity, and, if possible, moderate cost. Acoustic wave biosensors, based on immuno-detection, appear to meet a certain number of these criteria. In this context, we are developing a generic antibody-based biointerface that can detect a wide range of pathogenic bacterial agents using a specific bioreceptor. Based on the silane–oxide chemistry, the process is transferable to any kind of surface that can be either oxidized in surface or activated with O₂-plasma, for instance. For this proof of concept, we have chosen to develop our biointerface on titanium and lithium niobate surfaces. The development of the biointerface consists of grafting antibodies via a self-assembled monolayer (SAM) composed of an aminopropyltriethoxysilane (APTES) and a linker (phenylene diisothiocyanate, PDITC). Two functionalization routes were tested for grafting APTES: in anhydrous toluene followed by a heating step at 110 °C or in chloroform at room temperature. The results obtained on titanium show comparable grafting efficiency between these two routes, allowing us to consider the transposition of the route at room temperature on lithium niobate. The latest route was chosen for fragile materials that do not require the heating steps necessary when using toluene for grafting aminopropyltriethoxysilane. Different surface characterization techniques were used, such as IR spectroscopy (FTIR-ATR), X-ray photoelectron spectroscopy (XPS), and contact angle (WCA), to verify the successful grafting of each layer. Biodetection experiments in static conditions were also carried out to demonstrate the specificity of pathogenic detection, testing an ideal medium with solely bacteria, with no other food sampling nutrients. This paper demonstrates the successful elaboration of a biointerface using APTES as the first anchoring layer, with chloroform as a mild solvent. The process is easily transferable to any kind of fragile surface. Moreover, following anti-L. monocytogenes antibodies, our biointerface shows a specificity of capture in static mode (at a concentration of 10⁷ CFU/mL for an incubation time of 4 h at 37 °C) of up to 98% compared to a species negative control (E. coli) and up to 85% in terms of strain specificity (L. innocua). Full article

In this work, bare copper oxide-based catalysts were synthesized and evaluated for their dual (photo)catalytic activity in two model reactions: hydrogen generation via formic acid decomposition (FAD) and the photocatalytic hydroxylation of benzene to phenol. Catalysts were prepared from copper nitrate and copper acetate precursors and calcined for either 10 min or 2 h. Their structural and surface properties were characterized by wide-angle X-ray diffraction (WAXD), Raman spectroscopy, and BET surface area analysis. FAD was conducted under mild thermal conditions and monitored via ¹H NMR spectroscopy. At the same time, benzene hydroxylation was performed under UV irradiation and analyzed by gas chromatography (GC) and high-performance liquid chromatography (HPLC). All synthesized catalysts outperformed commercial CuO in the selective oxidation of benzene. The nitrate-derived sample calcined for 10 min (NCuO 10 min) achieved the best performance, with a phenol yield of ~10% and a selectivity of up to 19%, attributed to improved surface properties and the presence of Cu(I) domains, as indicated by Raman spectroscopy. For FAD, complete conversion of formic acid was achieved at low temperatures, with selective H₂ and CO₂ evolution and complete suppression of CO, even under short reaction times and low catalyst loadings. These results demonstrate the potential of nitrate-derived CuO catalysts as versatile, dual-function materials for sustainable applications in selective aromatic oxidation and low-temperature hydrogen generation, without the need for noble metals or harsh conditions. Full article