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Small‐angle X‐ray tensor tomography and the related wide‐angle X‐ray tensor tomography are X‐ray imaging techniques that tomographically reconstruct the anisotropic scattering density of extended samples. In previous studies, these methods have been used to image samples where the scattering density depends slowly on the direction of scattering, typically modeling the directionality, i.e. the texture, with a spherical harmonics expansion up until order ℓ = 8 or lower. This study investigates the performance of several established algorithms from small‐angle X‐ray tensor tomography on samples with a faster variation as a function of scattering direction and compares their expected and achieved performance. The various algorithms are tested using wide‐angle scattering data from an as‐drawn steel wire with known texture to establish the viability of the tensor tomography approach for such samples and to compare the performance of existing algorithms. [ABSTRACT FROM AUTHOR]

This study presents the characterization of cross-linking parameters of a liquid crystalline epoxy monomer with an aromatic diamine as a curing agent. The mixture tested consisted of bis [4-(10,11-epoxyundecanoyloxy)benzoate] p-phenylene (LCEM) and 1,3-phenylenediamine (1,3-PDA). This paper focuses on the structural characterization of such systems using X-ray analysis. To investigate this, a comprehensive analysis was conducted using Differential Scanning Calorimetry (DSC) and Wide-Angle X-ray Scattering (WAXS). Through DSC analysis, the curing behavior and transition temperature of the liquid crystal epoxy system were established. To fully characterize the cross-linking of the system, a novel technique called DSC-TOPEM® was employed. The use of this technique enabled real-time monitoring of the curing process and provided precise information on the cross-linking energy, which resulted in the finding that the mixture was cross-linking faster than expected. WAXS analysis was performed to assess the structural changes formed during the cross-linking. The results of this analysis confirm that lower cross-linking temperatures of the mixture cause better ordering of mesogens than higher ones. [ABSTRACT FROM AUTHOR]

This paper reports a novel α-gel formulation technology referred to as polymer complexed lamella (PCL) that uses hydroxypropyl methyl cellulose (HPMC) and glycerol. The PCL method suppressed lipid crystallization even after drying. This effect was maximized by the addition of HPMC and glycerol at high temperature. HPMC and lipids coexisted when mixed at high temperature, which decreased the mobility of HPMC, an effect that was enhanced by the strong interaction of glycerol with HPMC. These results indicate that mixing of HPMC with glycerol directly regulates the lipid structure and suppresses crystallization. PCL also maintained the effect of occlusion related to the moisturization of skin, even if the membrane was repeatedly bent such as in facial expressions. [ABSTRACT FROM AUTHOR]

Crystallographic texture is a key organization feature of many technical and biological materials. In these materials, especially hierarchically structured ones, the preferential alignment of the nano constituents heavily influences the macroscopic behavior of the material. To study local crystallographic texture with both high spatial and angular resolution, we developed Texture Tomography (TexTOM). This approach allows the user to model the diffraction data of polycrystalline materials using the full reciprocal space of the crystal ensemble and describe the texture in each voxel via an orientation distribution function, hence it provides 3D reconstructions of the local texture by measuring the probabilities of all crystal orientations. The TexTOM approach addresses limitations associated with existing models: it correlates the intensities from several Bragg reflections, thus reducing ambiguities resulting from symmetry. Further, it yields quantitative probability distributions of local real space crystal orientations without further assumptions about the sample structure. Finally, its efficient mathematical formulation enables reconstructions faster than the time scale of the experiment. This manuscript presents the mathematical model, the inversion strategy and its current experimental implementation. We show characterizations of simulated data as well as experimental data obtained from a synthetic, inorganic model sample: the silica–witherite biomorph. TexTOM provides a versatile framework to reconstruct 3D quantitative texture information for polycrystalline samples; it opens the door for unprecedented insights into the nanostructural makeup of natural and technical materials.

Appreciating that the role of the solute–solvent and other outer-sphere interactions is essential for understanding chemistry and chemical dynamics in solution, experimental approaches are needed to address the structural consequences of these interactions, complementing condensed-matter simulations and coarse-grained theories. High-energy X-ray scattering (HEXS) combined with pair distribution function analysis presents the opportunity to probe these structures directly and to develop quantitative, atomistic models of molecular systems in situ in the solution phase. However, at concentrations relevant to solution-phase chemistry, the total scattering signal is dominated by the bulk solvent, prompting researchers to adopt a differential approach to eliminate this unwanted background. Though similar approaches are well established in quantitative structural studies of macromolecules in solution by small- and wide-angle X-ray scattering (SAXS/WAXS), analogous studies in the HEXS regime—where sub-ångström spatial resolution is achieved—remain underdeveloped, in part due to the lack of a rigorous theoretical description of the experiment. To address this, herein we develop a framework for differential solution scattering experiments conducted at high energies, which includes concepts of the solvent-excluded volume introduced to describe SAXS/WAXS data, as well as concepts from the time-resolved X-ray scattering community. Our theory is supported by numerical simulations and experiment and paves the way for establishing quantitative methods to determine the atomic structures of small molecules in solution with resolution approaching that of crystallography.

The black pigments used in Late Period (11th–17th centuries) painted pottery in the Yocavil Valley were characterized. Changes and continuities in the composition of this material over an extended span were evaluated. A regional sample of 47 potsherds from the Loma Rica, San José, and Santa María styles was collected, and for the first time micro wide‐angle X‐ray scattering was used in these ceramic styles. The results indicate the simultaneous presence of iron oxides (hematite) and solid solutions of manganese and iron oxides (jacobsite–magnetite). Besides, the paints were prepared by mixing the pigments with clay‐based binding materials. [ABSTRACT FROM AUTHOR]

Chitin, a ubiquitous biopolymer, holds paramount scientific and economic significance. Historically, it has been primarily isolated from marine crustaceans. However, the surge in demand for chitin and the burgeoning interest in biopolymers have necessitated the exploration of alternative sources. Among these methods, the mulberry silkworm (Bombyx mori) has emerged as a particularly intriguing prospect. To isolate chitin from Bombyx mori, a chemical extraction methodology was employed. This process involved a series of meticulously orchestrated steps, including Folch extraction, demineralization, deproteinization, and decolorization. The resultant chitin was subjected to comprehensive analysis utilizing techniques such as attenuated total reflectance–Fourier transform infrared spectroscopy (ATR-FTIR), 13C nuclear magnetic resonance (NMR) spectroscopy, and wide-angle X-ray scattering (WAXS). The obtained results allow us to conclude that the Bombyx mori represents an attractive alternative source of α-chitin. [ABSTRACT FROM AUTHOR]

Palm oil (PO), a semi-solid fat at room temperature, is a popular food ingredient. To steer the fat functionality, sucrose esters (SEs) are often used as food additives. Many SEs exist, varying in their hydrophilic-to-lipophilic balance (HLB), making them suitable for various food and non-food applications. In this study, a stearic–palmitic sucrose ester with a moderate HLB (6) was studied. It was found that the SE exhibited a complex thermal behavior consistent with smectic liquid crystals (type A). Small-angle X-ray scattering revealed that the mono- and poly-esters of the SE have different packings, more specifically, double and single chain-length packing. The polymorphism encountered upon crystallization was repeatable during successive heating and cooling cycles. After studying the pure SE, it was added to palm oil, and the crystallization behavior of the mixture was compared to that of pure palm oil. The crystallization conditions were varied by applying cooling at 20 °C/min (fast) and 1 °C/min (slow) to 0 °C, 20 °C or 25 °C. The samples were followed for one hour of isothermal time. Differential scanning calorimetry (DSC) showed that nucleation and polymorphic transitions were accelerated. Wide-angle X-ray scattering (WAXS) unraveled that the α-to-β′ polymorphic transition remained present upon the addition of the SE. SAXS showed that the addition of the SE at 0.5 wt% did not significantly change the double chain-length packing of palm oil, but it decreased the domain size when cooling in a fast manner. Ultra-small-angle X-ray scattering (USAXS) revealed that the addition of the SE created smaller crystal nanoplatelets (CNPs). The microstructure of the fat crystal network was visualized by means of polarized light microscopy (PLM) and cryo-scanning electron microscopy (cryo-SEM). The addition of the SE created a finer and space-filling network without the visibility of separate floc structures. [ABSTRACT FROM AUTHOR]

The precipitation kinetics of precipitates with different orientations and segregation in an ultrafine grained (UFG) Al–Cu–Mg alloy (AA2024) aged at 210 °C have been investigated using situ small angle X-ray scattering (SAXS), situ wide angle X-ray (WAXS) and Transmission Electron Microscopy (TEM). For UFG alloy, the number and size of (111) S'/S phases are larger than those of (130) S'/S phases on the whole, because spacing of slip plane near (111) S'/S phases is larger than that near (130) S'/S phases, resulting in solute atoms are easier to diffusion near (111) S'/S phases, and (111) S'/S phases are easier to grow, meanwhile, resulting in the critical shear stress for dislocation moving near (111) S'/S phases is smaller than that near (130) S'/S phases, further leading to the dislocation density near (111) S'/S phases is 1.07–1.19 times larger compared to that near (130) S'/S phases during ageing process, which provides more nucleation sites for (111) S'/S phases. After ageing for 10–40 min, the segregation degree of Cu and Mg atoms near dislocations and grain boundaries is increased in UFG alloy, while after ageing for 80 min, the segregation of Cu atoms is decreased and Mg atoms continue to increase, the segregation of Mg atoms begin to decrease after ageing for 120 min.

Hygroexpansion, CP/MAS 13C-NMR, WAXS and SAXS measurements were carried out on sheets made from four different commercial pulps of varying lignin content. Non-directional laboratory sheets were made at different press levels from the pulps following different degrees of beating. The sheets were dried both freely and with restraints. Measurements were made on sheets before and after moisture cycling to determine hygroexpansion coefficients, changes in cellulose average lateral fibril dimensions and average cellulose crystallite sizes, with the aim of understanding macroscale and nanoscale changes as the result of moisture cycling. Within the sheets consistent and statistically significant structural changes were observed on both macro and nanoscale. On the macroscale, moisture cycling consistently induced irreversible shrinkage in sheets dried with restraints, but less so in the case of sheets dried freely. The hygroexpansion coefficients were typically higher for freely dried sheets compared with sheets dried with constraints. On the nanoscale, moisture cycling consistently caused an increase in the average crystallite sizes (WAXS) and the average lateral fibril dimensions (CP/MAS 13C-NMR), though the latter occurred with poor statistical significance. These changes were interpreted as an increase in the degree of order in the cellulose fibril interior/cellulose crystallite. There were no profound differences in the nanoscale changes observed for sheets dried with restraints and for sheets dried freely. Changes in the fibre wall nanostructure were of similar magnitudes when comparing results from freely dried low grammage sheets (less abundant inter-fibre joints) with freely dried sheets of higher grammage (more abundant inter-fibre joints). No obvious correlations were found between the macroscale and nanoscale measurements. The proposed explanation for this was that the nanoscale structural changes occurred similarly throughout the entirety of the fibre wall, independent of the proximity to an inter-fibre joint, and that the nanoscale structural changes were mainly the result of water penetrating into the interior of cellulose fibril aggregates. By using the same fibril model for evaluation of CP/MAS 13C-NMR and WAXS data, good-to-reasonable agreement were found for estimates of the degree of cellulose crystallinity. [ABSTRACT FROM AUTHOR]

Palm oil (PO) is still widely used for the production of all types of food products. Due to its triacylglycerol (TG) composition, PO is semisolid at ambient temperature, offering possibilities for many applications. In order to tailor the fat crystal network for certain applications, it remains imperative to understand the structural build-up of the fat crystal network at the full-length scale and to understand the effect of processing conditions. In this study, PO was crystallized under four temperature protocols (fast (FC) or slow (SC) cooling to 20 °C or 25 °C) and was followed for one hour of isothermal time. A broad toolbox was used to fundamentally unravel the structural build-up of the fat crystal network at different length scales. Wide-angle and small-angle X-ray scattering (WAXS and SAXS) showed transitions from α-2L to β'-2L over time. Despite the presence of the same polymorphic form (β'), chain length structure (2L), and domain size, ultra-small-angle X-ray scattering (USAXS) showed clear differences in the mesoscale. For all samples, the lamellar organization was confirmed. Both cooling speed and isothermal temperature were found to affect the size of the crystal nanoplatelets (CNPs), where the highest cooling speed and lowest isothermal temperature (FC and 20 °C) created the smallest CNPs. The microstructure was visualized with polarized light microscopy (PLM) and cryo-scanning electron microscopy (cryo-SEM), showing clear differences in crystallite size, clustering, and network morphology. Raman spectroscopy was applied to confirm differences in triglyceride distribution in the fat crystal network. This study shows that both cooling rate and isothermal temperature affect the fat crystal network formed, especially at the meso- and microscale. [ABSTRACT FROM AUTHOR]

The Femtosecond X-ray Experiments (FXE) instrument at the European X-ray Free-Electron Laser (EuXFEL) provides an optimized platform for investigations of ultrafast physical, chemical and biological processes. It operates in the energy range 4.7–20 keV accommodating flexible and versatile environments for a wide range of samples using diverse ultrafast X-ray spectroscopic, scattering and diffraction techniques. FXE is particularly suitable for experiments taking advantage of the sub-MHz repetition rates provided by the EuXFEL. In this paper a dedicated setup for studies on ultrafast biological and chemical dynamics in solution phase at sub-MHz rates at FXE is presented. Particular emphasis on the different liquid jet sample delivery options and their performance is given. Our portfolio of high-speed jets compatible with sub-MHz experiments includes cylindrical jets, gas dynamic virtual nozzles and flat jets. The capability to perform multi-color X-ray emission spectroscopy (XES) experiments is illustrated by a set of measurements using the dispersive X-ray spectrometer in von Hamos geometry. Static XES data collected using a multi-crystal scanning Johann-type spectrometer are also presented. A few examples of experimental results on ultrafast time-resolved X-ray emission spectroscopy and wide-angle X-ray scattering at sub-MHz pulse repetition rates are given.

The SAXSMAT beamline P62 (Small-Angle X-ray Scattering beamline for Materials Research) is a new beamline at the high-energy storage ring PETRA III at DESY. This beamline is dedicated to combined small- and wide-angle X-ray scattering (SAXS/WAXS) techniques for both soft and hard condensed matter systems. It works mainly in transmission geometry. The beamline covers an energy range from 3.5 keV to 35.0 keV, which fulfills the requirements of the user community to perform anomalous scattering experiments. Mirrors are used to reduce the intensity of higher harmonics. Furthermore, the mirrors and 2D compound refracting lenses can focus the beam down to a few micrometres at the sample position. This option with the high photon flux enables also SAXS/WAXS tensor tomography experiments to be performed at this new beamline in a relatively short time. The first SAXS/WAXS pattern was collected in August 2021, while the first user experiment was carried out two months later. Since January 2022 the beamline has been in regular user operation mode. In this paper the beamline optics and the SAXS/WAXS instrument are described and two examples are briefly shown.

This study presents the characterization of cross-linking parameters of a liquid crystalline epoxy monomer with an aromatic diamine as a curing agent. The mixture tested consisted of bis [4-(10,11-epoxyundecanoyloxy)benzoate] p-phenylene (LCEM) and 1,3-phenylenediamine (1,3-PDA). This paper focuses on the structural characterization of such systems using X-ray analysis. To investigate this, a comprehensive analysis was conducted using Differential Scanning Calorimetry (DSC) and Wide-Angle X-ray Scattering (WAXS). Through DSC analysis, the curing behavior and transition temperature of the liquid crystal epoxy system were established. To fully characterize the cross-linking of the system, a novel technique called DSC-TOPEM® was employed. The use of this technique enabled real-time monitoring of the curing process and provided precise information on the cross-linking energy, which resulted in the finding that the mixture was cross-linking faster than expected. WAXS analysis was performed to assess the structural changes formed during the cross-linking. The results of this analysis confirm that lower cross-linking temperatures of the mixture cause better ordering of mesogens than higher ones.

This study characterizes the microstructure and mineralogy of 132 (ODP sample), 1000 and 1880 million‐year‐old chert samples. By using ultra‐small‐angle X‐ray scattering (USAXS), wide‐angle X‐ray scattering and other techniques, the preservation of organic matter (OM) in these samples is studied. The scarce microstructural data reported on chert contrast with many studies addressing porosity evolution in other sedimentary rocks. The aim of this work is to solve the distribution of OM and silica in chert by characterizing samples before and after combustion to pinpoint the OM distribution inside the porous silica matrix. The samples are predominantly composed of alpha quartz and show increasing crystallite sizes up to 33 ± 5 nm (1σ standard deviation or SD). In older samples, low water abundances (∼0.03%) suggest progressive dehydration. (U)SAXS data reveal a porous matrix that evolves over geological time, including, from younger to older samples, (1) a decreasing pore volume down to 1%, (2) greater pore sizes hosting OM, (3) decreasing specific surface area values from younger (9.3 ± 0.1 m2 g−1) to older samples (0.63 ± 0.07 m2 g−1, 1σ SD) and (4) a lower background intensity correlated to decreasing hydrogen abundances. The pore‐volume distributions (PVDs) show that pores ranging from 4 to 100 nm accumulate the greater volume fraction of OM. Raman data show aromatic organic clusters up to 20 nm in older samples. Raman and PVD data suggest that OM is located mostly in mesopores. Observed structural changes, silica–OM interactions and the hydrophobicity of the OM could explain the OM preservation in chert. [ABSTRACT FROM AUTHOR]

Three oleogelator molecules (Triacontane (TC), Stearic acid (SA), and Behenyl Lignocerate (BL)) were studied individually, in pairs, or all together to make an oleogel using triolein as the oil. WAXS, SAXS and USAXS were used to elucidate the solid structures from angstroms to a few micrometers. A two‐dimensional mapping of atomic positions for each molecule was carried out to understand the crystalline multilayer structures formed. We assumed that the molecules were rigidly extended and that they underwent no significant (hindered) rotations so that the free energy is determined by the Lennard‐Jones interactions of closely packed multilayers. TC molecules were predicted to form a tilt angle of θt≈33°, yielding a SAXS line at q≈0.194 Å─1, in acceptable agreement with the measured q=0.181Å−1. For SA crystals θt≈33° (predicted) yielding a SAXS line at q=0.150Å−1 compared to q=0.159Å−1 (observed). No mixed crystals were observed for any pair of molecules or when all three were used. USAXS data showed that SA forms large nanocrystals compared to TC and BL. All three combinations of molecular pairs showed basic scatterers smaller or similar to those of individual molecules. The theory presented here, together with the experimental results, showed why no mixed crystals are formed from two or all three molecules. Data from the USAXS region suggested that, when using all three molecules, a more compact fractal structure was obtained, compared with those if one or two of the molecules were used. [ABSTRACT FROM AUTHOR]

In this study, the in‐plane linear thermal expansion behaviors from −20 °C to 100 °C along the flow direction (FD) for injection molded isotactic homo polypropylene (hPP) and their elastomer blends are thoroughly investigated. The elastomers used in this study are two different poly(ethylene‐co‐octene)(EO) thermoplastic elastomers which have the same density but different melt flow rate (MFR), 5.0 and 30 (dg/10 min). Thus, the blends are designated as hPP‐EO5.0 having the EO with 5.0 of MFR and hPP‐EO30 having the EO with 30 of MFR. It is found that from −20 °C to 40 °C, the linear thermal expansion profiles for neat hPP, hPP‐EO5.0, and hPP‐EO30 overlapped, indicating that with or without the EO, their linear thermal expansions proceeded under the same mechanism. On the other hand, above 40 °C, their thermal expansion behaviors greatly changed; the linear thermal expansions of hPP‐EO5.0 and hPP‐EO30 are suppressed to be much lower than that of neat hPP. The morphological observation by a transmission electron microscope (TEM) reveals that the shapes of the EO domains in the blend systems are found to be elongated along the FD. Thus, it would be expected that the suppressed linear thermal expansions of the hPP‐EO blends are attributed to the suppression of the linear thermal expansions of the hPP amorphous layers in the lamellae due to the retraction of the elongated EO domains caused due to the instability of the interfacial tension at elevated temperatures. Yet, temperature variable small‐angle X‐ray scattering (SAXS) results reveal that the linear thermal expansions of the hPP amorphous layers in the EO blends, on the contrary, increase. One of the plausible mechanisms is proposed to elucidate seemingly contradictory phenomenon that the EO blends have their suppressed bulk linear thermal expansions while enhanced linear thermal expansions of the hPP amorphous layers. Finally, the suitable elastomer design for low coefficient of linear thermal expansion (CLTE) PP is proposed. [ABSTRACT FROM AUTHOR]

The Femtosecond X-ray Experiments (FXE) instrument at the European X-ray Free-Electron Laser (EuXFEL) provides an optimized platform for investigations of ultrafast physical, chemical and biological processes. It operates in the energy range 4.7-20 keVaccommodating flexible and versatile environments for a wide range of samples using diverse ultrafast X-ray spectroscopic, scattering and diffraction techniques. FXE is particularly suitable for experiments taking advantage of the sub-MHz repetition rates provided by the EuXFEL. In this paper a dedicated setup for studies on ultrafast biological and chemical dynamics in solution phase at sub-MHz rates at FXE is presented. Particular emphasis on the different liquid jet sample delivery options and their performance is given. Our portfolio of high-speed jets compatible with sub- MHz experiments includes cylindrical jets, gas dynamic virtual nozzles and flat jets. The capability to perform multi-color X-ray emission spectroscopy (XES) experiments is illustrated by a set of measurements using the dispersive X-ray spectrometer in von Hamos geometry. Static XES data collected using a multicrystal scanning Johann-type spectrometer are also presented. A few examples of experimental results on ultrafast time-resolved X-ray emission spectroscopy and wide-angle X-ray scattering at sub-MHz pulse repetition rates are given. [ABSTRACT FROM AUTHOR]

The SAXSMAT beamline P62 (Small-Angle X-ray Scattering beamline for Materials Research) is a new beamline at the high-energy storage ring PETRA III at DESY. This beamline is dedicated to combined small- and wide-angle X-ray scattering (SAXS/WAXS) techniques for both soft and hard condensed matter systems. It works mainly in transmission geometry. The beamline covers an energy range from 3.5 keV to 35.0 keV, which fulfills the requirements of the user community to perform anomalous scattering experiments. Mirrors are used to reduce the intensity of higher harmonics. Furthermore, the mirrors and 2D compound refracting lenses can focus the beam down to a few micrometres at the sample position. This option with the high photon flux enables also SAXS/WAXS tensor tomography experiments to be performed at this new beamline in a relatively short time. The first SAXS/ WAXS pattern was collected in August 2021, while the first user experiment was carried out two months later. Since January 2022 the beamline has been in regular user operation mode. In this paper the beamline optics and the SAXS/ WAXS instrument are described and two examples are briefly shown. [ABSTRACT FROM AUTHOR]

The effect on softwood fiber wall nanostructure of kraft cooking, oxygen delignification and refining was evaluated by X-ray scattering. A recently developed simulation method for modelling small angle X-ray scattering (SAXS) data was used to estimate the apparent average sizes of solids (AAPS) and interstitial spaces in the fiber wall (AACS). Fiber saturation point and wide angle X-ray scattering were also used to calculate the pore volume in the fiber wall and the crystallite size of the fibril, respectively. The experimental modelled SAXS data was able to give consistent values for each kraft-cooked and oxygen-delignified pulp. Kraft delignification seems to have the major influence on the fiber nanostructure modification, while oxygen delignification has little or no significant impact even for different kappa numbers. The particle sizes values were more stable than the cavities sizes and no significant differences were seen between different delignification processes, refining or delignification degree. Pulps evaluated after PFI-refining, showed an increase in the fiber wall porosity evaluated by FSP and an increase in the interstitial spaces in the fiber wall, while the crystallite size and the particle sizes were very little or not affected at all. [ABSTRACT FROM AUTHOR]

Abstract Cotton (Gossypium species) was used as textile fibre already in the early Indus culture, and since then it has been cultivated in Tropical and Subtropical regions around the whole planet. The species G. hirsutum is nowadays the dominant cotton crop with more than 90% of the world market, while G. barbadense, G. herbaceum and G. arboreum combined, the other cultivated species of Gossypium genus total a minor part of world’s cotton production. Even in places where cotton was not cultivated, it could be an important trade item and income source for local textile centres, with the imported raw cotton lint being spun, woven and for some part exported from such sites around the globe. This all occurred far away from Finland, until changes brought by the development of long-distance trade and the Industrial Revolution. Based on archaeological finds, cotton as a textile material reached Finland relatively late, in the early Middle Ages. The article focuses on the problematic nature of identifying these cotton finds: whereas modern cotton fibres are easy to identify, the archaeological finds can at first sight be confused with bast or un-degummed silk fibres. This issue will be approached through reviewing recent Finnish cotton finds in heritage textiles. Additionally, the article examines whether the four cultivated cotton species could be differentiated using both classical and newly developed fibre identification methods, such as optical microscopy methods, a Scanning Electron Microscope (SEM), Fourier-transform infrared spectroscopy (FTIR) or Wide-Angle X-ray Scattering (WAXS).

Painting materials used in Spanish American Colonial art comprised pigments and binders from European origin as well as those that were already known in pre-Hispanic times. In recent years, we have identified for the first time the mineral atacamite, a basic copper chloride (Cu2Cl(OH)3), in Andean Colonial art pieces (Viceroyalty of Peru, 16th–18th centuries). This work proposes a methodology based on a multitechnical approach to identify and establish the origin (natural or synthetic) of the atacamite pigment in Andean cultural heritage objects. Optical microscopy (OM), scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS), portable X-ray fluorescence spectroscopy (pXRF), attenuated total reflection infrared spectroscopy (FTIR-ATR), micro-Raman spectroscopy, and wide-angle X-ray scattering (WAXS) were applied to analyse green pigments from the altarpiece of the Church of Ancoraimes, atacamite mineral samples from Chile, and atacamite obtained as a secondary product from traditional recipes used to produce verdigris, a copper acetate. Viride salsum by Teófilo Presbítero (SXII) and the Spanish translation by Andrés de Laguna (1566) of “De Materia Médica” from Dioscorides are both texts that include recipes involving the use of metallic copper as a starting material. These studies will contribute to the history of Spanish American Colonial art and to the knowledge on technological capacities and skills in the Andean region during this period.

[Display omitted] Real-time in situ X-ray analysis was used to shed light on the topotactic transformation of NH 4 TiOF 3 into nanostructured TiO 2 mesocrystals. Specifically, for the system formed in the presence of the PEG-2000 templating polymer, XRD analysis showed that the overall transformation occurs through four separate transitions, consistent with previous reports. The applicability of synchrotron wide-angle X-ray scattering (WAXS) to real-time in situ analysis has enabled precise temperature mapping of these four transitions and the identification of stability boundaries for the first time. [ABSTRACT FROM AUTHOR]

Palm oil (PO), a semi-solid fat at room temperature, is a popular food ingredient. To steer the fat functionality, sucrose esters (SEs) are often used as food additives. Many SEs exist, varying in their hydrophilic-to-lipophilic balance (HLB), making them suitable for various food and non-food applications. In this study, a stearic–palmitic sucrose ester with a moderate HLB (6) was studied. It was found that the SE exhibited a complex thermal behavior consistent with smectic liquid crystals (type A). Small-angle X-ray scattering revealed that the mono- and poly-esters of the SE have different packings, more specifically, double and single chain-length packing. The polymorphism encountered upon crystallization was repeatable during successive heating and cooling cycles. After studying the pure SE, it was added to palm oil, and the crystallization behavior of the mixture was compared to that of pure palm oil. The crystallization conditions were varied by applying cooling at 20 °C/min (fast) and 1 °C/min (slow) to 0 °C, 20 °C or 25 °C. The samples were followed for one hour of isothermal time. Differential scanning calorimetry (DSC) showed that nucleation and polymorphic transitions were accelerated. Wide-angle X-ray scattering (WAXS) unraveled that the α-to-β′ polymorphic transition remained present upon the addition of the SE. SAXS showed that the addition of the SE at 0.5 wt% did not significantly change the double chain-length packing of palm oil, but it decreased the domain size when cooling in a fast manner. Ultra-small-angle X-ray scattering (USAXS) revealed that the addition of the SE created smaller crystal nanoplatelets (CNPs). The microstructure of the fat crystal network was visualized by means of polarized light microscopy (PLM) and cryo-scanning electron microscopy (cryo-SEM). The addition of the SE created a finer and space-filling network without the visibility of separate floc structures.

Chitin, a ubiquitous biopolymer, holds paramount scientific and economic significance. Historically, it has been primarily isolated from marine crustaceans. However, the surge in demand for chitin and the burgeoning interest in biopolymers have necessitated the exploration of alternative sources. Among these methods, the mulberry silkworm (Bombyx mori) has emerged as a particularly intriguing prospect. To isolate chitin from Bombyx mori, a chemical extraction methodology was employed. This process involved a series of meticulously orchestrated steps, including Folch extraction, demineralization, deproteinization, and decolorization. The resultant chitin was subjected to comprehensive analysis utilizing techniques such as attenuated total reflectance–Fourier transform infrared spectroscopy (ATR-FTIR), 13C nuclear magnetic resonance (NMR) spectroscopy, and wide-angle X-ray scattering (WAXS). The obtained results allow us to conclude that the Bombyx mori represents an attractive alternative source of α-chitin.

Cotton (Gossypium species) was used as textile fibre already in the early Indus culture, and since then it has been cultivated in Tropical and Subtropical regions around the whole planet. The species G. hirsutum is nowadays the dominant cotton crop with more than 90% of the world market, while G. barbadense, G. herbaceum and G. arboreum combined, the other cultivated species of Gossypium genus total a minor part of world's cotton production. Even in places where cotton was not cultivated, it could be an important trade item and income source for local textile centres, with the imported raw cotton lint being spun, woven and for some part exported from such sites around the globe. This all occurred far away from Finland, until changes brought by the development of long-distance trade and the Industrial Revolution. Based on archaeological finds, cotton as a textile material reached Finland relatively late, in the early Middle Ages. The article focuses on the problematic nature of identifying these cotton finds: whereas modern cotton fibres are easy to identify, the archaeological finds can at first sight be confused with bast or un-degummed silk fibres. This issue will be approached through reviewing recent Finnish cotton finds in heritage textiles. Additionally, the article examines whether the four cultivated cotton species could be differentiated using both classical and newly developed fibre identification methods, such as optical microscopy methods, a Scanning Electron Microscope (SEM), Fourier-transform infrared spectroscopy (FTIR) or Wide-Angle X-ray Scattering (WAXS). [ABSTRACT FROM AUTHOR]

Characterization of the mechanical response of polymers and composite materials relies heavily on the macroscopic stress–strain response in uniaxial tensile configurations. To provide representative information, the deformation process must be homogeneous within the gauge length, which is a condition that is rarely achieved due to stress concentration or inhomogeneities within the specimen. In this work, the development of a biaxial mechanical testing device at the CoSAXS beamline at MAX IV Laboratory is presented. The design facilitates simultaneous measurement of small‐ and wide‐angle X‐ray scattering (SAXS/WAXS), allowing assessment of the microstructural configuration before, after and during the continuous deformation process at multiple length scales. The construction also supports multiple deformation conditions, while guaranteeing stability even at high loads. Furthermore, the mechanical experiments can be complemented with spatially resolved mesoscopic surface deformation measurements using 3D‐surface digital image correlation (DIC). Polycarbonate (PC) was used to demonstrate the varied material response to multi‐axial deformation, as PC is isotropic with a high glass transition temperature (∼150°) and high strength. As a result, a clear correlation between full‐field methods and the microstructural information determined from WAXS measurements is demonstrated. When a uniaxial load is applied, homogeneous strain regions could be observed extending perpendicular to the applied load. When a secondary axial load was added (biaxial mode), it was observed that high strain domains were created near the centre of the sample and at the boundaries after yield. With increased strain, the deformation in the main deformation direction also increases. Mechanical reliability was demonstrated by carrying out static loading of polyacrylonitrile‐based carbon fibre (CF) bundles. As a result, the nonlinear stiffening behaviour typically observed in CFs was seen, while no evidence of the creation of new voids during loading was observed. The results support the reliability and broad applicability of the developed technique. [ABSTRACT FROM AUTHOR]

Painting materials used in Spanish American Colonial art comprised pigments and binders from European origin as well as those that were already known in pre-Hispanic times. In recent years, we have identified for the first time the mineral atacamite, a basic copper chloride (Cu2Cl(OH)3), in Andean Colonial art pieces (Viceroyalty of Peru, 16th–18th centuries). This work proposes a methodology based on a multitechnical approach to identify and establish the origin (natural or synthetic) of the atacamite pigment in Andean cultural heritage objects. Optical microscopy (OM), scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS), portable X-ray fluorescence spectroscopy (pXRF), attenuated total reflection infrared spectroscopy (FTIR-ATR), micro-Raman spectroscopy, and wide-angle X-ray scattering (WAXS) were applied to analyse green pigments from the altarpiece of the Church of Ancoraimes, atacamite mineral samples from Chile, and atacamite obtained as a secondary product from traditional recipes used to produce verdigris, a copper acetate. Viride salsum by Teófilo Presbítero (SXII) and the Spanish translation by Andrés de Laguna (1566) of "De Materia Médica" from Dioscorides are both texts that include recipes involving the use of metallic copper as a starting material. These studies will contribute to the history of Spanish American Colonial art and to the knowledge on technological capacities and skills in the Andean region during this period. [ABSTRACT FROM AUTHOR]

Type I collagen physiological scaffold for tissue regeneration is considered one of the widely used biomaterials for tissue engineering and medical applications. It is hierarchically organized: five laterally staggered molecules are packed within fibrils, arranged into fascicles and bundles. The structural organization is correlated to the direction and intensity of the forces which can be loaded onto the tissue. For a tissue-specific regeneration, the required macro- and microstructure of a suitable biomaterial has been largely investigated. Conversely, the function of multiscale structural integrity has been much less explored but is crucial for scaffold design and application. In this work, collagen was extracted from different animal sources with protocols that alter its structure. Collagen of tendon shreds excised from cattle, horse, sheep and pig was structurally investigated by wide- and small-angle X-ray scattering techniques, at both molecular and supramolecular scales, and thermo-mechanically with thermal and load-bearing tests. Tendons were selected because of their resistance to chemical degradation and mechanical stresses. The multiscale structural integrity of tendons' collagen was studied in relation to the animal source, anatomic location and source for collagen extraction. [ABSTRACT FROM AUTHOR]

Bone is a complex, biological tissue made up primarily of collagen fibrils and biomineral nanoparticles. The importance of hierarchical organization in bone was realized early on, but the actual interplay between structural features and the properties on the nanostructural and crystallographic level is still a matter of intense discussion. Bone is the only mineralized tissue that can be remodeled and, at the start of the formation of new bone during this process, a structure called a cement line is formed on which regular bone grows. Here, the orientational relationship of nanostructural and crystallographic constituents as well as the structural properties of both nanostructural and crystallographic constituents around cement lines and the Haversian system in human lamellar bone are investigated. A combination of small- and wide-angle X-ray scattering tensor tomography is employed together with diffraction tomography and synchrotron computed tomography to generate a multi-modal image of the sample. This work shows that the mineral properties vary as a function of the distance to the Haversian canal and, importantly, shows that the cement line has differing mineral properties from the surrounding lamellar bone, in particular with respect to crystallite size and degree of orientation. Cement lines make up a significant portion of the bone matrix despite their small size, hence the reported findings on an altered mineral structure, together with the spatial modulation around the Haversian canal, have implications for the formation and mechanics of bone.

Palm oil (PO) is still widely used for the production of all types of food products. Due to its triacylglycerol (TG) composition, PO is semisolid at ambient temperature, offering possibilities for many applications. In order to tailor the fat crystal network for certain applications, it remains imperative to understand the structural build-up of the fat crystal network at the full-length scale and to understand the effect of processing conditions. In this study, PO was crystallized under four temperature protocols (fast (FC) or slow (SC) cooling to 20 °C or 25 °C) and was followed for one hour of isothermal time. A broad toolbox was used to fundamentally unravel the structural build-up of the fat crystal network at different length scales. Wide-angle and small-angle X-ray scattering (WAXS and SAXS) showed transitions from α-2L to β’-2L over time. Despite the presence of the same polymorphic form (β’), chain length structure (2L), and domain size, ultra-small-angle X-ray scattering (USAXS) showed clear differences in the mesoscale. For all samples, the lamellar organization was confirmed. Both cooling speed and isothermal temperature were found to affect the size of the crystal nanoplatelets (CNPs), where the highest cooling speed and lowest isothermal temperature (FC and 20 °C) created the smallest CNPs. The microstructure was visualized with polarized light microscopy (PLM) and cryo-scanning electron microscopy (cryo-SEM), showing clear differences in crystallite size, clustering, and network morphology. Raman spectroscopy was applied to confirm differences in triglyceride distribution in the fat crystal network. This study shows that both cooling rate and isothermal temperature affect the fat crystal network formed, especially at the meso- and microscale.

This study investigates the thermal behavior of polyethylene 2,5‐furandicarboxylate using Raman spectroscopy. The study finds that multiple changes in the Raman spectrum at two different heating rates of 1 and 0.5 K/min provide different information about the thermal behavior of the sample. The study also shows that the derivative of the half‐width of the band at 1737 cm−1, which characterizes the stretching of the C=O double bond of the ester group, allows us to trace back to the DSC thermogram. The crystallinity was followed with quite a good precision and using two different spectral zones around 1029 and 1737 cm−1. The calculated crystallinity rate could be compared with the crystallinity rates obtained by integrating the total heat flow by DSC and that obtained by wide angle X‐ray scattering (WAXS). As a result, this study also allows us to understand the conformational changes that take place during heating, and especially those responsible for crystallization, which is the great advantage of Raman spectroscopy compared with other standard methods. [ABSTRACT FROM AUTHOR]

Finite size effects in partial pair distribution functions generate artefacts in the scattering structure factor and scattering intensity. It is shown how they can be overcome using a binned version of the Debye scattering equation. Accordingly, reverse Monte Carlo simulations are used for very small nanoparticles of LaFeO3 with diameters below 10 nm to simultaneously analyse X‐ray scattering data and extended X‐ray absorption fine structure spectra at the La K and Fe K edges. The structural information obtained is consistent regarding local structure and long‐range order. [ABSTRACT FROM AUTHOR]

In this study, the interplay among the phospholipid 1,2-dimyristoyl-sn-glycero-3-phosphocholine (DMPC) as a model membrane, the nonsteroidal anti-inflammatory drug naproxen, and the saponin β -aescin are investigated. The naproxen amount was fixed to 10 mol%, and the saponin amount varies from 0.0 to 1.0 mol%. Both substances are common ingredients in pharmaceutics; therefore, it is important to obtain deeper knowledge of their impact on lipid membranes. The size and properties of the DMPC model membrane upon naproxen and aescin addition were characterized with differential scanning calorimetry (DSC), small- and wide-angle X-ray scattering (SAXS, WAXS), and photon correlation spectroscopy (PCS) in a temperature-dependent study. The interaction of all substances was dependent on the lipid phase state, which itself depends on the lipid's main phase transition temperature T m . The incorporation of naproxen and aescin distorted the lipid membrane structure and lowers T m . Below T m , the DMPC–naproxen–aescin mixtures showed a vesicle structure, and the insertion of naproxen and aescin influenced neither the lipid chain–chain correlation distance nor the membrane thickness. Above T m , the insertion of both molecules instead induced the formation of correlated bilayers and a decrease in the chain–chain correlation distance. The presented data clearly confirm the interaction of naproxen and aescin with DMPC model membranes. Moreover, the incorporation of both additives into the model membranes is evidenced. [ABSTRACT FROM AUTHOR]

Tracking the Raman scattering bands of polyethylene terephthalate (PET) during thermal heating has allowed to establish criteria for monitoring the crystallinity ratio within a few seconds. The existing criteria, based on Raman bands at 998 cm−1 and at 1096 cm−1, present certain disparities from the crystallinity ratio given by the total heat flow in differential scanning calorimetry (DSC). Based on the evolution of the Raman bands, a newfound method allowing the effective calculation of crystallinity ratio is proposed. For the same, the band at 1727 cm−1, which is characteristic of the C=O carbonyl bonds of the ester group of PET, is used. The new criterion, designated r1727,2, was compared and validated by DSC and XRD. This novel approach also provides access to information on the various conformational states of the bonds under study, that is, their proportions and positions with respect to the plane of the macromolecule aromatic rings. Evidently, this allows to reveal the characteristic thermal behavior of the PET microstructure such as the glass transition, crystallization, and melting. This method can be useful for the close detection, quantification, understanding, and tracing of the micromechanisms involved at the macromolecular conformations scale during thermal cycles. [ABSTRACT FROM AUTHOR]

On a sample of the Turin Shroud (TS), we applied a new method for dating ancient linen threads by inspecting their structural degradation by means of Wide-Angle X-ray Scattering (WAXS). The X-ray dating method was applied to a sample of the TS consisting of a thread taken in proximity of the 1988/radiocarbon area (corner of the TS corresponding to the feet area of the frontal image, near the so-called Raes sample). The size of the linen sample was about 0.5 mm × 1 mm. We obtained one-dimensional integrated WAXS data profiles for the TS sample, which were fully compatible with the analogous measurements obtained on a linen sample whose dating, according to historical records, is 55–74 AD, Siege of Masada (Israel). The degree of natural aging of the cellulose that constitutes the linen of the investigated sample, obtained by X-ray analysis, showed that the TS fabric is much older than the seven centuries proposed by the 1988 radiocarbon dating. The experimental results are compatible with the hypothesis that the TS is a 2000-year-old relic, as supposed by Christian tradition, under the condition that it was kept at suitable levels of average secular temperature—20.0–22.5 °C—and correlated relative humidity—75–55%—for 13 centuries of unknown history, in addition to the seven centuries of known history in Europe. To make the present result compatible with that of the 1988 radiocarbon test, the TS should have been conserved during its hypothetical seven centuries of life at a secular room temperature very close to the maximum values registered on the earth.

Synthesis of high-surface-area graphene oxide for application in next-generation devices is still challenging. In this study, we present a simple and green-chemistry procedure for the synthesis of oxygen-enriched graphene materials, having very large surface areas compared with those reported for powdered graphene-related solids. Using the hydrothermal treatment of carbon nanohorns by a green-chemistry H2O2 oxidant under elevated pressure, the progressive creation of a stable carbon nanomaterial, denoted as open-sensu-shaped graphene oxide (OSSGO) by us, is observed. This oxygen-enriched nanographene contains π–π stacked few-layered graphene ribbons curved at the termini derived from the original cone tip. OSSGO is intensively analyzed and cross-characterized by spectroscopy, diffraction, adsorption, and elemental analysis methods. Based on the obtained results, we propose a mechanism of transformation from horns to a structure with several layers of sensu-form stacked graphene oxide. As this transformation process proceeds gradually, one can obtain numerous transition nanoarchitectures of tunable morphology and surface physicochemistry, including materials with an extremely high surface area. As OSSGO bears a fraction of the electron-withdrawing and O–H acidic functionalities, electrochemical studies, especially galvanostatic charge–discharge curves and specific capacitance values (significantly higher than those for other carbon-based materials), show potential applications in next-generation supercapacitors. As a result of the large surface areas, we also predict future applications in programmable adsorbents and catalysts with broad-range activity, while the list of applications is incomplete. [ABSTRACT FROM AUTHOR]

The present study emphasizes appending the knowledge of structure-property relations, elasto-mechanical properties. The knowledge of the elasto-mechanical properties of cotton fibers plays a significant role in industrial applications, these properties determine the fabric stiffness, hardness, and tailorability of cotton. For various cotton samples studied here, whose molecular orientations were unknown, and few studies are reported to study its basic structural properties. However, the linked atom least square fit (LALS) and crystallographic tool PLATON has been utilized to obtain the crystal structure of LRA and Shankar cotton fibers using XRD data. The elastic constant matrix for the monoclinic unit cell with the lattice parameters a = 7.350 Å, b = 8.220 Å and c = 10.370 Å and γ = 96.28° has been obtained by considering Treloar's assumptions. These elastic constants are incorporated to the ELATE tensor analysis tool along with the Voigt principle to evaluate elastic moduli. It is observed that the spatial variations of these elastic moduli deviate from the spherical shape, which shows the existence of the anisotropic property of the fibers. With all these structures and physicomechanical parameters analyzed for the cotton samples studied, the structure-property dependencies have been obtained utilizing the functional data analysis technique. [ABSTRACT FROM AUTHOR]

One of the main research work in the field of polymeric materials was, is and always will be the improvement of their mechanical properties. Comprehensive structural studies of UHMWPE reactor powder, the features of its dissolution and the formation of a gel-state, as well as UHMWPE films oriented up to various draw ratios, were carried out using scanning electron microscopy, differential scanning calorimetry, and X-ray diffraction. For comparison, decalin and vaseline oil were chosen as solvents. The mechanical properties of oriented UHMWPE films were also studied. In the process of orientation drawing, basing on the developed structural-kinetic principles of strengthening for highly oriented speciments gel-cast from UHMWPE powders, the average values of tensile strength of 4.7 GPa (about 6% of the samples had strength values up to 6.0 GPa) and an Young's modulus of 170 GPa (about 6% of the samples had Young's modulus values of 200 GPa). These values are among the highest according to the world scientific literature. A significant increase in the mechanical characteristics of highly oriented UHMWPE films was achieved using experimentally confirmed scientific approaches to revealing the structure-property relationship at each stage of the gel process. [ABSTRACT FROM AUTHOR]

In 2021, Wide-angle X-ray Scattering (WAXS) was applied to a sample of the Turin Shroud as a new method for dating ancient linen threads by inspecting their structural degradation. The major result of the research was to estimate the natural aging of the linen of the Shroud, through which it was found to be compatible with the hypothesis of a 2000-year-old relic, and not a medieval fabric. The present work regards the theoretical natural aging of the linen versus different alleged historical–geographical paths of the Shroud through cities where the presence of icons of Jesus Christ is attested. The theoretical results of the natural aging of the Shroud, calculated for the year 2021, agree extremely well with the experimental results for at least one alleged path. The results also show that if the Shroud were medieval and kept in Europe for 7 centuries, natural aging that is one order of magnitude less than that measured by WAXS would have resulted. Today, the Shroud is kept in a reliquary with a controlled atmosphere, at 19~20 °C temperature, and 50% relative humidity. These values are shown to be unsuitable for maintaining the depolymerization of the cellulose at a level that is sufficiently low enough to preserve the image visible on the Shroud for a long time. [ABSTRACT FROM AUTHOR]

X-ray diffraction based microscopy techniques such as high-energy diffraction microscopy (HEDM) rely on knowledge of the position of diffraction peaks with high precision. These positions are typically computed by fitting the observed intensities in detector data to a theoretical peak shape such as pseudo-Voigt. As experiments become more complex and detector technologies evolve, the computational cost of such peak-shape fitting becomes the biggest hurdle to the rapid analysis required for real-time feedback in experiments. To this end, we propose BraggNN, a deep-learning based method that can determine peak positions much more rapidly than conventional pseudo-Voigt peak fitting. When applied to a test dataset, peak center-of-mass positions obtained from BraggNN deviate less than 0.29 and 0.57 pixels for 75 and 95% of the peaks, respectively, from positions obtained using conventional pseudo-Voigt fitting (Euclidean distance). When applied to a real experimental dataset and using grain positions from near-field HEDM reconstruction as ground-truth, grain positions using BraggNN result in 15% smaller errors compared with those calculated using pseudo-Voigt. Recent advances in deep-learning method implementations and special-purpose model inference accelerators allow BraggNN to deliver enormous performance improvements relative to the conventional method, running, for example, more than 200 times faster on a consumer-class GPU card with out-of-the-box software.

Xi-cam is an extensible platform for data management, analysis and visualization. Xi-cam aims to provide a flexible and extensible approach to synchrotron data treatment as a solution to rising demands for high-volume/high-throughput processing pipelines. The core of Xi-cam is an extensible plugin-based graphical user interface platform which provides users with an interactive interface to processing algorithms. Plugins are available for SAXS/WAXS/GISAXS/GIWAXS, tomography and NEXAFS data. With Xi-cam's `advanced' mode, data processing steps are designed as a graph-based workflow, which can be executed live, locally or remotely. Remote execution utilizes high-performance computing or de-localized resources, allowing for the effective reduction of high-throughput data. Xi-cam's plugin-based architecture targets cross-facility and cross-technique collaborative development, in support of multi-modal analysis. Xi-cam is open-source and cross-platform, and available for download on GitHub.

The effect of a stable magnetic field (1 T) on precipitation kinetics in an Al–Cu–Mg alloy (AA2024) aged at different temperatures has been systematically studied by small angle X-ray scattering (SAXS), transmission electron microscope (TEM) and wide angle X-ray scattering (WAXS). The synchrotron SAXS and WAXS results reveal that the precipitation kinetics in different scales is facilitated by magnetic field at ageing process. Based on the WAXS findings, under the magnetic field, the precipitation of CuAl2Mg, Al7Cu2Fe and CuAl2 phases is accelerated at all ageing process, and the highest enhancement of relative intensity of them reaches 262%. Among them, at low ageing temperature (at 130 °C), the percentage of relative intensity of CuAl2Mg and Al7Cu2Fe phases between with and without magnetic field are increased by 48%–120% and 93%–257%, respectively, as compared to the values 1 of above two phases observed at other ageing temperature (at 160–240 °C). Modifications of the precipitation kinetics under magnetic field could be associated with two reasons. One is solute diffusion increase, this is attributed to the increase of solute diffusion coefficient, which results from the change of frequency factor of atom caused by magnetic field. Another is critical nucleation energy decrease and critical nucleation rate increase, which is attributed to the presence of magnetic field energy under magnetic field.

Herein, optimization of zeolite NaA/NaX synthesis conditions in order to obtain the final product with high surface area and pore volume was investigated. An optimal synthesis condition was 5 days aging time and crystallization time of 9 h with the co-addition of cetyltrimethylammonium bromide (CTAB) and heptane. All those optimal synthesis conditions provided mixed phase between zeolite NaA and NaX, and addition of those organic phases improved the surface area and pore volume of the final synthesized zeolite. The role of CTAB and heptane on increasing the surface area of zeolite was studied by in situ small-angle X-ray scattering (SAXS). The SAXS results evidenced that small nucleation precursor was formed upon the addition of organic phase, and this nucleation precursor can provide zeolite with high-characteristic XRD signals of mixed phase of zeolite A and X after the crystallization process. The synthesized zeolite obtained from optimal synthesis condition with high surface area was further used as a catalyst support by impregnating with 5, 10, 15, and 20wt%Ni for catalyzing CO2 methanation reaction. The results found that 15wt%Ni/zeolite expressed the highest catalytic activity with high CH4 selectivity and stability. This was due to high dispersion of Ni species on catalyst surface and high metal-support interaction between Ni and zeolite. These results indicated that the mixed phase zeolite support can be a potential catalyst support for this reaction. [ABSTRACT FROM AUTHOR]

Mechanical properties of amorphous poly(butylene terephthalate)/poly(carbonate) (PBT/PC) blends were studied at various temperatures. Two distinct regions associated with the mechanical response at various temperatures were identified. Also the temperature‐related microstructural evolution of amorphous PBT/PC blends was explored at 30°C and 50°C by synchrotron radiation WAXS. The mesophase of PBT could be obtained from the melt by rapid quenching. The presence of PC suppresses the mesophase formation during rapid quenching and also suppresses PBT crystallization during deformation. Structure models were proposed to describe the deformation process of amorphous PBT/PC blends at 30°C and 50°C. [ABSTRACT FROM AUTHOR]

With the ability to cross biological barriers, encapsulate and efficiently deliver drugs and nucleic acid therapeutics, and protect the loaded cargos from degradation, different soft polymer and lipid nanoparticles (including liposomes, cubosomes, and hexosomes) have received considerable interest in the last three decades as versatile platforms for drug delivery applications and for the design of vaccines. Hard nanocrystals (including gold nanoparticles and quantum dots) are also attractive for use in various biomedical applications. Here, microfluidics provides unique opportunities for the continuous synthesis of these hard and soft nanomaterials with controllable shapes and sizes, and their in situ characterization through manipulation of the flow conditions and coupling to synchrotron small-angle X-ray (SAXS), wide-angle scattering (WAXS), or neutron (SANS) scattering techniques, respectively. Two-dimensional (2D) and three-dimensional (3D) microfluidic devices are attractive not only for the continuous production of monodispersed nanomaterials, but also for improving our understanding of the involved nucleation and growth mechanisms during the formation of hard nanocrystals under confined geometry conditions. They allow further gaining insight into the involved dynamic structural transitions, mechanisms, and kinetics during the generation of self-assembled nanostructures (including drug nanocarriers) at different reaction times (ranging from fractions of seconds to minutes). This review provides an overview of recently developed 2D and 3D microfluidic platforms for the continuous production of nanomaterials, and their simultaneous use in in situ characterization investigations through coupling to nanostructural characterization techniques (e.g., SAXS, WAXS, and SANS). [ABSTRACT FROM AUTHOR]

Crystallographic texture is a key organization feature of many technical and biological materials. In these materials, especially hierarchically structured ones, the preferential alignment of the nano constituents heavily influences the macroscopic behavior of the material. To study local crystallographic texture with both high spatial and angular resolution, we developed Texture Tomography (TexTOM). This approach allows the user to model the diffraction data of polycrystalline materials using the full reciprocal space of the crystal ensemble and describe the texture in each voxel via an orientation distribution function, hence it provides 3D reconstructions of the local texture by measuring the probabilities of all crystal orientations. The TexTOM approach addresses limitations associated with existing models: it correlates the intensities from several Bragg reflections, thus reducing ambiguities resulting from symmetry. Further, it yields quantitative probability distributions of local real space crystal orientations without further assumptions about the sample structure. Finally, its efficient mathematical formulation enables reconstructions faster than the time scale of the experiment. This manuscript presents the mathematical model, the inversion strategy and its current experimental implementation. We show characterizations of simulated data as well as experimental data obtained from a synthetic, inorganic model sample: the silica-witherite biomorph. TexTOM provides a versatile framework to reconstruct 3D quantitative texture information for polycrystalline samples; it opens the door for unprecedented insights into the nanostructural makeup of natural and technical materials., (open access.)