Search Results (226)

This review summarizes the current state of research on perfluorinated sulfonic acid (PFSA) ionomers, including both classic Nafion and a wide range of alternative chemical modifications, as well as new-generation composite and stabilized membranes. The accumulation of a large body of experimental and modeling data in recent years highlights the need to rethink the differences between traditional ionomers and their modern counterparts, which is especially relevant in light of the development of new materials and their expanding applications. PFSA ionomers have a rich research history, playing a key role in the development of polymer-electrolyte fuel cell technologies and other electrochemical systems. At the same time, these materials have become a unique interdisciplinary platform, stimulating the development of new methods of characterization, modeling, and analysis. In PFSA research, technological progress is closely intertwined with fundamental science, encompassing electrochemistry, polymer physics, mechanics, chemistry, and multiscale modeling. The data we collected allowed us to identify new structural and functional patterns, analyze the behavior of ionomers in various states—from thin films and interfaces to bulk membranes—and summarize numerous previously fragmented relationships. Full article

Background: Pentamidine isethionate (PTM) and miltefosine (MF) are clinically relevant antiparasitic agents whose use is limited by toxicity, emerging resistance, and the lack of effective co-delivery strategies. Tetronic^® 1307 (T1307), an amphiphilic and thermoresponsive block copolymer, was investigated as a carrier to enable their combination therapy. Methods: PTM and MF were formulated in T1307-based micelles and thermoresponsive gels. The systems were characterized by small-angle neutron scattering (SANS), dynamic light scattering (DLS), and nuclear magnetic resonance spectroscopy (NMR). Antiparasitic activity was evaluated against Leishmania major promastigotes. Results: MF formed stable micelles that efficiently incorporated PTM, generating a “drug-in-drug” architecture. While T1307 alone showed limited PTM loading, MF promoted mixed micelle formation and enhanced PTM incorporation. At physiological temperature and adequate copolymer concentrations, drug-loaded micelles formed thermoreversible gels suitable for topical application. The combined formulations preserved drug activity and exhibited synergistic effects against L. major. Conclusions: T1307 is a promising platform for the co-delivery of PTM and MF, enabling synergistic combination therapy and thermoresponsive gel formation with potential to reduce systemic toxicity and improve treatment administration. Full article

Characterization of shale pore architecture forms the scientific basis for effective shale gas exploitation. Deep LMX FM shale from the Luzhou area was analyzed using SANS, LTPA, XRD, and SEM. This study quantitatively characterized the pore structure, focusing on closed-pore development and connectivity, and explored lithological controls. Pore-size distribution shows that micropores and small mesopores dominate the pore volume, with an average median pore diameter of 5.17 nm. Closed pores are abundant, indicated by a high average closed-pore ratio of 28.98%, reflecting generally poor connectivity. Pores smaller than 5 nm contribute 88.12% of the total SSA. Both pore volume and SSA correlate positively with TOC. In organic-rich and moderately organic-rich siliceous shales, these parameters also correlate positively with quartz content. In contrast, for organic-rich mixed shales, they correlate positively with clay mineral content. Among the lithofacies, organic-rich siliceous shale possesses relatively larger pore volume and SSA, along with better pore connectivity, making it the most favorable reservoir facies. Based on pore-structure characteristics and the regional structural setting, we recommend adopting close-spacing hydraulic fracturing with reduced cluster spacing in structurally stable areas to enhance stimulation. In structurally complex areas, engineering designs should prioritize risk mitigation to ensure operational success. Full article

Although membrane proteins are of major importance in both physiology and disease, they remain less studied than soluble proteins due to the complex amphiphilic environments required to preserve their structure and function. As a consequence, membrane proteins are under-represented in structural databases. In this work, we present a robust structural characterization of lipid nanodiscs designed to facilitate membrane protein studies by small-angle neutron scattering. By combining small-angle X-ray and neutron scattering, we investigate nanodiscs of three different sizes and three lipid compositions to accommodate a broad range of systems. Specifically, nanodiscs with diameters of approximately 9 nm, 12 nm, and 15 nm were examined. Beyond the commonly used di-myristoyl-phosphatidylcholine lipid, we produced and characterized polar lipid extracts from a Gram-negative bacterium (Escherichia coli) and a Gram-positive bacterium (Bacillus subtilis) under both protonated and deuterated conditions. In conclusion, solubility-enhanced variants of the scaffold protein yield more stable nanodiscs and are therefore preferable for extended structural investigations. The co-fitting of small-angle scattering data provides robust geometrical models of these nanodiscs, which can be treated as well-defined reference systems for future studies of membrane proteins in native-like lipid environments. Full article

Studying nanoscale self-assembly in real time using external stimuli unlocks new opportunities for dynamic and adaptive materials. While electrostatic self-assembly is well-established, real-time monitoring of its structural evolution under light irradiation remains largely unexploited. In this study, we employ light-responsive azobenzene dyes (Acid Yellow 38, AY38) and pH-sensitive polyamidoamine (PAMAM) dendrimers to investigate the kinetics of electrostatic self-assembly under UV irradiation. Using a custom in situ small-angle neutron scattering (SANS) setup, we track the real-time morphological transformations of self-assembled structures with sub-minute resolution. We introduce two distinct pathways: method A (pre-irradiated cis-AY38 for controlled, slow kinetics) and method B (direct UV-induced self-assembly, fast kinetics). The results reveal that trans-cis isomerization kinetics dictate the rate of self-assembly, influencing aggregate stability, ζ-potential evolution, and final morphology. Structural analysis using dynamic and static light scattering (DLS and SLS) and SANS elucidates a transition from spherical to ellipsoidal morphologies governed by electrostatic and dipole-dipole interactions. These findings establish photoisomerization-driven self-assembly as a robust mechanism for tunable nanoscale architectures, paving the way for adaptive photonic materials, targeted drug delivery, and reconfigurable nanostructures. Full article

This study investigates the structural dynamics of the TRAF2 C-terminal domain (TRAF2-C), a key adaptor protein in TNF receptor signaling. TRAF2 usually forms trimers, but its ability to dissociate into monomers is critical for regulating apoptosis, inflammation, and cell survival. Using Fluorescence Fluctuation Spectroscopy, dynamic light scattering, circular dichroism, and Small Angle Neutron Scattering, we analyzed TRAF2-C over a wide concentration range. At nanomolar levels, the protein dissociates easily, with trimers representing only a minor fraction, while micromolar concentrations strongly favor trimerization. Dissociation also reduces α-helical content without disrupting the overall fold. Molecular dynamics simulations and protein contact network analysis support this analysis, identifying interfacial residues and hydrogen bonds as key factors stabilizing oligomers and enabling dynamic asymmetry. Overall, these findings highlight TRAF2-C’s capacity to switch between monomeric and trimeric states as a crucial regulatory mechanism, offering insights into TRAF-mediated signaling and potential therapeutic strategies. Full article

This study establishes a robust small-angle neutron scattering (SANS) methodology for the quantitative characterization of γ matrix channel widths in the nickel-based single-crystal superalloy DD10. By combining SANS with TEM analyses and modeling the one-dimensional SANS data via a polydisperse lamellar model, we accurately determined the channel width distribution across macroscopic sample volumes. In the virgin state, the mean channel widths were nearly isotropic, measuring 17.8 ± 0.1 nm along [002] and 20.5 ± 0.1 nm along [020]. After standard heat treatment (solution and two-step aging), significant anisotropic coarsening was observed, with widths increasing to 36.8 ± 0.2 nm along [002] and 28.0 ± 0.1 nm along [020], indicating stress-free rafting. Elemental mapping revealed substantial redistribution of key alloying elements: Al content in γ′ precipitates increased by 2.6 at.%, while Cr in the γ channels rose by 5.9 at.%. These quantitative results demonstrate that SANS provides reliable, bulk-statistical insights into nanoscale channel geometry, highlighting its critical role in influencing elemental diffusion kinetics and microstructural evolution during thermal exposure. Full article

Mesoporous silica nanoparticles have been synthesized through sol–gel synthesis in basic conditions. Gemini surfactants having urea in the headgroups were used as pore-forming agents. The effect of the spacer length of the surfactant on the particle morphology was studied on the sub-micrometer and nanometer scales using nitrogen porosimetry, small-angle X-ray scattering (SAXS), ultra-small-angle neutron scattering, and scanning and transmission electron microscopy (SEM, TEM). Depending on the spacer, spherical and/or cylindrical nanoparticles formed in different proportions, as revealed by statistical analysis of SEM micrographs. All prepared materials showed the hexagonal pore structure characteristic of the MCM-41 molecular sieves, with the exception of the sample prepared using the gemini surfactant with the shortest spacer length. The influence of the spacer length on the lattice parameter of the pore network, as well as the average size of the ordered domains, has been assessed by SAXS and TEM. Detailed analysis of the TEM images revealed a spread of the lattice parameter in a range of 10–20%. The broadening of the diffraction peaks was shown to be due to the combination of the effects of the finite domain size and the variance of the lattice parameter across the crystalline domains. The structural differences between the silica gels synthesized with the different surfactants were related to the variation of the micelle morphologies, reported in previous light scattering and small-angle scattering experiments. No connection could be revealed between the micelle shape and size and the pore sizes, showing that surfactants with a broad range of spacer lengths can equally well be used for the preparation of MCM-41 materials. Full article

Polymeric vesicles, characterized by enhanced colloidal stability, excellent mechanical properties, controllable surface functionality, and adjustable membrane thickness, are extremely useful in nano- and bio-technology for potential applications as nanosized carriers for drugs and enzymes. However, a few preparative steps are necessary to achieve a unilamellar vesicle with a narrow size distribution. Herein, we report the spontaneous formation of unilamellar polymeric vesicles with nanometer sizes (<50 nm), fabricated by simply mixing diblock copolymers (P(EO-AGE)(2K-2K) and P(EO-AGE)(0.75K-2K)) with differing hydrophilic mass fractions in aqueous solutions. Depending on the mixing ratio of block copolymers and the temperature, the block copolymer mixtures self-assemble into various nanostructures, such as spherical and cylindrical micelles, or vesicles. The self-assembled structures of the block copolymer mixtures were characterized by small-angle neutron scattering, resulting in a phase diagram drawn as a function of temperature and the mixing condition. Notably, the critical temperature for the micelle-to-vesicle phase transition can be easily controlled by altering the mixing conditions; it decreases with an increase in the concentration of one of the block copolymers. Full article

Cyclodextrin-based nanosponges (CDNSs) are novel polymers composed of cross-linked cyclodextrin (CD) macrocyclic units, whose characteristics make them great candidates for drug delivery systems with adjustable properties for the drug release process. Examination of the molecular structure and dynamics of CDNSs is a necessary starting point in the first step toward their broad application. Spectroscopic methods are effective analytical tools for probing the structure–property relationships of polymer structures. Infrared (IR) and Raman spectroscopies provide insight into the behavior of hydrogen bond (H-bond) networks influencing the properties of CDNS polymeric networks. Scattering techniques such as inelastic neutron scattering (INS) and Brillouin light scattering (BLS) probe elastic properties, while small-angle neutron scattering (SANS) examines the structural inhomogeneities and water sorption abilities of CDNS materials. Complete evaluation is possible using nuclear magnetic resonance (NMR), which can provide data on CDNS network dynamics. This article summarizes the results of a wide examination of CDNSs with the use of spectroscopic methods and reveals the links between the microscopic behavior and macroscopic properties of CDNSs, enabling the customization of their properties for various biomedical purposes. Full article

Polarized Small-Angle Neutron Scattering is a versatile low-energy neutron scattering technique that allows for the access of magnetic information on nanosize objects of size 2–100 nm, from individual properties like the magnetization distribution inside the object to the collective behaviors, e.g., spin-glass effects or long-range magnetic ordering. The multi-scale possibilities of this technique is particularly relevant to encompass simultaneously the individual and collective many-body phenomena. In this article, we report the direct measurement of the magnetic form factor of “Prussian Blue Analog” molecular-based Ferromagnetic nanoparticles ${\mathrm{Cs}}_{\mathrm{x}}^{\mathrm{I}}{\mathrm{Ni}}^{\mathrm{II}}\left[{\mathrm{Cr}}^{\mathrm{III}}{\left(\mathrm{CN}\right)}_6\right]$ embedded in a polymer matrix with use of Polarized Small-Angle Neutron Scattering. We show that PSANS is particularly adapted to evaluate the internal magnetization distribution in nanoparticles and determine their magnetic morphology. Full article

This study developed a neutron-beam-focusing supermirror for grazing-incidence small-angle neutron scattering (GISANS) measurements. We adopted point-to-point beam focusing based on an ellipse whose two foci correspond to a virtual point source and a spot on the detector surface. The focusing supermirror was fabricated by depositing NiC/Ti supermirror film with ion-beam sputtering on a precise elliptic surface of fused quartz figured using the elastic emission machining technique. Neutron measurements at the pulsed neutron reflectometer BL17 of the MLF, J-PARC, successfully demonstrated that the focusing supermirror enhances the beam intensity twentyfold compared with an optimally collimated beam, achieving a signal-to-background ratio of the focal spot as high as 500. The mirror can be readily installed and used at BL17 for time-of-flight GISANS measurements. Full article

The elliptical cylindrical mirror has been utilized in neutron small-angle scattering and reflectometry to enhance the neutron intensity at the sample position. However, the performance of the elliptical cylindrical mirror can be impacted by surface slope errors, reflectivity, and misalignments. In this work, the performance of the elliptical cylindrical mirror under different error conditions has been analyzed comprehensively, and a 250-mm-long elliptical cylindrical mirror was designed and developed. The simulations show that a source size below 1 mm is required to achieve a peak gain above 6, with a theoretical peak gain of 16× with a 0.1 mm source. The rotational misalignment of 0.03° around the Y-axis can decrease gain from 16× to 6×. The designed mirror was fabricated with a surface figure error of 110 nm (RMS), and a roughness below 0.5 nm (RMS), and was coated with an m = 4 supermirror. The mirror was aligned and tested in the dedicated neutron beamline of the Chinese mianyang research reactor, and the results show a peak gain of 12.77 with a 0.1 mm slit source. Full article

Poloxamer-based drug delivery systems are widely used in the pharmaceutical sector. The structural characterization of these systems is crucial for the development of new drug delivery systems and for the optimization of their properties. In this study, we utilized small-angle neutron scattering (SANS) to investigate the structures of poloxamer-based drug delivery systems. The samples were measured using the SANS technique on the VSANS-V16 instrument at Helmholtz-Zentrum Berlin (HZB), Germany. The samples contained 20% poloxamer (P407) and 0.2% of a drug (ibuprofen, ketoprofen, diclofenac) in deuterated water (D₂O) for SANS. The samples varied in terms of temperature analysis (25 °C, common storage temperature; 37 °C, human body temperature; 40 °C, fever temperature). The data analysis involved modeling the data using a Python-based routine. The model used consisted of an isotropic solution of polydisperse spherical micelles. The intensity as a function of the scattering vector was modeled as the product of the form factor and the interparticle structure factor, with the latter described within the local monodisperse approximation regime. Additionally, a scattering contribution was observed, which was associated with the presence of crystalline superstructures formed by micelles that organized into a cubic structure. The data analysis provided important information about the system, such as the average radius, the size distribution, and the thickness of the layer surrounding the micellar core. The results will contribute to the development and optimization of new drug delivery systems that are more effective and safer for medical applications. Full article

Herein we describe the development of the first model amphiphilic polymer conetwork (APCN) comprising a short hydrophobic hexa(L-alanine) segment being the outer block of an amphiphilic four-armed star block copolymer with inner poly(ethylene glycol) (PEG) blocks bearing benzaldehyde terminal groups and end-linked with another four-armed star PEG homopolymer (tetraPEG star) bearing aryl-substituted acylhydrazide terminal groups. The present successful synthesis that yielded the peptide-containing model APCN was preceded by several unsuccessful efforts that followed different synthetic strategies. In addition to the synthetic work, we also present the structural characterization of the peptide-bearing APCN in D₂O using small-angle neutron scattering (SANS). Full article