Plant-based meat alternatives are seeing considerable interest due to their potential to reduce environmental burden and enhance population health. The food industry, therefore, seeks routes to provide the consumer with whole-cut plant-based products that closely resemble meat products. High-moisture extrusion (HME) of plant proteins enables the industrial manufacturing of meat-like products with highly hierarchical structural organisation of fibres. The major bottleneck in serving the growing market for these products is a lack of insight into
how multiscale structures evolve during shear processing. Furthermore, it remains an open question of how two biopolymers, one being a plant protein and the other being a polysaccharide, contribute to the anisotropic structure formation during HME. This study shows how the complementary use of small-angle neutron scattering (SANS) and small-angle X-ray scattering (SAXS) can add clarity to these matters, benefiting from the different contrasts in scattering length density (SLD) encountered with each of these methods. It is demonstrated that two
biopolymers have differences in the development of structural anisotropy. The protein fibril alignment starts in the extruder section with its further development along the cooling die. On the other hand, for polysaccharide fibres, the strongest local alignment has been found in the transition zone.
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We describe an experiment that strongly supports a two-path interferometric model in which the spin-up and spin-down components of each neutron propagate coherently along spatially separated parallel paths in a typical neutron spin-echo small-angle scattering (SESANS) experiment. Specifically, we show that the usual semi-classical, single-path treatment of Larmor precession of a polarized neutron in an external magnetic field predicts a damping as a function of the spin-echo length of the SESANS signal obtained with a periodic phase grating when the transverse width of the neutron wave packet is finite. However, no such damping is observed experimentally, implying either that the Larmor model is incorrect or that the transverse extent of the wave packet is very large. In contrast, we demonstrate theoretically that a quantum-mechanical interferometric model in which the two mode-entangled (i.e., intraparticle entangled) spin states of a single neutron are separated in space when they interact with the grating accurately predicts the measured SESANS signal, which is independent of the wave packet width.

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Cellulose membranes were prepared from an EMIMAc ionic liquid solution by nonsolvent-induced phase separation (NIPS) in coagulation baths of water–acetone mixtures, ethanol–water mixtures and water at different temperatures. High water volume fractions in the coagulation bath result in a highly reproducible gel-like structure with inhomogeneities observed by small-angle neutron scattering (SANS). A structural transition of cellulose takes place in water–acetone baths at very low water volume fractions, while a higher water bath temperature increases the size of inhomogeneities in the gel-like structure. These findings demonstrate the value of SANS for characterising and understanding the structure of regenerated cellulose films in their wet state. Such insights can improve the engineering and structural tuning of cellulose membranes, either for direct use or as precursors for carbon molecular sieve membranes.@en

The organization of chromatin in the nuclei of rat lymphocyte was studied by time-of-flight spin-echo small-angle neutron scattering (ToF-SESANS). The procedures of the measurements in ToF and monochromatic SESANS modes were compared. It is shown that the sensitivity of the ToF method is significantly higher than that of the monochromatic mode. As a result, the SESANS correlation function can always be extracted from the ToF measurement of polarization, while this is not always the case with the monochromatic mode. The applicability of SESANS to fractal objects at the micrometre scale is demonstrated. The SESANS correlation function is well fitted by the exponential decay G(z) = exp(−z/ξ) with the correlation length ξ = 3.7 ± 0.1 µm. The exponential decay of the SESANS correlation function can be connected to the logarithmic correlation function γ(r) = ln(r/ξ) and the cubic law of the scattering intensity I(Q) = Q−3, which is in agreement with the concept of scattering from fractal objects. This finding is interpreted as evidence of a very specific logarithmic fractal structure of the large-scale organization of chromatin. The model of the logarithmic fractal is visualized as a hierarchical object obeying the volume-conservation principle at different scales.@en

Polymeric micelles, due to their easy preparation and versatile properties, have been widely applied as one of the most popular carriers for chemotherapeutic agents. Such micelles primarily prevent the leakage of drugs during transportation and thus protect healthy tissue. Controlled drug release, which releases the drugs at the site of interest using internal or external stimuli as triggers, can further improve the safety of the drug delivery process. In this paper, we investigate whether ionizing radiation can be used to initiate release, focusing on using Cerenkov light as a possible trigger. For this purpose, micelles composed of the degradable polymer poly(ϵ-caprolactone-b-ethylene glycol) (PCL-PEO) were first loaded with the photosensitizer chlorin e6 (Ce6) and subsequently exposed to gamma or X-ray radiation of varying radiation doses. The results reveal that Ce6 was released from the micelles under radiation, regardless of the energy of incident photons, showing that Cerenkov light was not the driving force behind the observed release. SANS measurements showed that the volume fraction of the micelles containing Ce6 was reduced after exposure to radiation. This change in volume fraction suggests that the number of micelles was reduced, which was probably responsible for the release of Ce6. The exact mechanism, however, remains unclear. Subsequently, the PCL-PEO micelles were loaded with Ce6 and one of the following drugs: doxorubicin (Dox), docetaxel (DTX), and paclitaxel (PTX). Under radiation exposure, Dox, which is quite stable in single-loaded micelles, shows an enhanced release profile in the presence of Ce6, while DTX and PTX remained in the micelles, regardless of the presence of Ce6.

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The first measurements of magnetic correlation functions are presented using time-of-flight Spin-echo modulated small angle neutron scattering (SEMSANS) on the Larmor instrument at the ISIS pulsed neutron source. The accessible length scale is beyond that of the conventional SANS. A simplified model is presented to calculate the expected correlation functions for various magnetisation fields applied to the sample. As an example, we present the experimental data of a soft iron sample at various configurations of magnetisation field.

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The development of direct probes of entanglement is integral to the rapidly expanding field of complex quantum materials. Here we test the robustness of entangled neutrons as a quantum probe by measuring the Clauser-Horne-Shimony-Holt contextuality witness while varying the beam properties. Specifically, we show that the mode entanglement of the spin and path subsystems of individual neutrons prepared in two different experiments using two different apparatuses persists even after varying the entanglement length, coherence length, and neutron energy difference of the paths. The two independent apparatuses acting as entangler-disentangler pairs are static-field magnetic Wollaston prisms and resonance-field radio-frequency flippers. Our results show that the spatial and energy properties of the neutron beam may be significantly altered without reducing the contextuality witness value below the Tsirelson bound, meaning that maximum entanglement is preserved. We also show that two paths may be considered distinguishable even when the path states significantly overlap. Therefore, we have shown that our experimental results are consistent with the distinguishable subsystem assumption down to a separation of less than 100 nm, proving entanglement and the contextual nature of reality on short length scales. This work is the key step in the realization of the modular, robust technique of entangled neutron scattering, which can extract entanglement information from a sample without the knowledge of the microscopic sample Hamiltonian: only semiquantitative knowledge of the correlation lengths of the relevant degrees of freedom and the timescales of the characteristic dynamics is required.

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In-situ Neutron Diffraction and Small-Angle Neutron Scattering (SANS) are employed for the first time simultaneously in order to reveal the interaction between the austenite to ferrite phase transformation and the precipitation kinetics during isothermal annealing at 650 and at 700 °C in three steels with different vanadium (V) and carbon (C) concentrations. Austenite-to-ferrite phase transformation is observed in all three steels at both temperatures. The phase transformation is completed during a 10 h annealing treatment in all cases. The phase transformation is faster at 650 than at 700 °C for all alloys. Additions of vanadium and carbon to the steel composition cause a retardation of the phase transformation. The effect of each element is explained through its contribution to the Gibbs free energy dissipation. The austenite-to-ferrite phase transformation is found to initiate the vanadium carbide precipitation. Larger and fewer precipitates are detected at 700 than at 650 °C in all three steels, and a larger number density of precipitates is detected in the steel with higher concentrations of vanadium and carbon. After 10 h of annealing, the precipitated phase does not reach the equilibrium fraction as calculated by ThermoCalc. The external magnetic field applied during the experiments, necessary for the SANS measurements, causes a delay in the onset and time evolution of the austenite-to-ferrite phase transformation and consequently on the precipitation kinetics.

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The modulated intensity by zero effort small-angle neutron scattering (MI-SANS) technique is used to measure scattering with a high energy resolution on samples normally ill-suited for neutron resonance spin echo. The self-diffusion constant of water is measured over a q-t range of 0.01-0.2Å-1 and 70-500ps. In addition to demonstrating the methodology of using time-of-flight MI-SANS instruments to observe diffusion in liquids, the results support previous measurements on water performed with different methods. This polarized neutron technique simultaneously measures the intermediate scattering function for a wide range of time and length scales. Two radio frequency flippers were used in a spin-echo setup with a 100kHz frequency difference in order to create a high-resolution time measurement. The results are compared with self-diffusion measurements made by other techniques and the general applicability of MI-SANS at a pulsed source is assessed.

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Fullerene derivatives are used in a wide range of applications including as electron acceptors in solution-processable organic photovoltaics. We report agglomeration of fullerene derivatives in optically opaque solutions of PC₆₁BM and PC₇₁BM, with concentrations ranging from 30 mg mL^-1 up to 90 mg mL^-1, in different solvents with relevance to organic photovoltaics, using a novel neutron scattering technique, Spin-Echo Small Angle Neutron Scattering (SESANS). From SESANS, agglomerates with correlation lengths larger than 1 μm are found in some PC₆₁BM solutions, in contrast no agglomerates are seen in PC₇₁BM solutions. These results clearly show that PC₇₁BM is fundamentally more soluble than PC₆₁BM in the solvents commonly used in photovoltaic inks and corroborating similar observations previously achieved using other experimental techniques. Computer models are presented to study the energetics of solution and agglomeration of both species, ascribing the difference to a kinetic effect probably related to the larger anisotropy of PC₇₁BM. Also, this work showcases the power of SESANS to probe agglomerates of fullerene derivatives in completely opaque solutions for agglomerates of the order of one to several microns.

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Interphase precipitation occurring during solid-state phase transformations in micro-alloyed steels is generally studied through transmission electron microscopy, atom probe tomography, and ex situ measurements of Small-Angle Neutron Scattering (SANS). The advantage of SANS over the other two characterization techniques is that SANS allows for the quantitative determination of size distribution, volume fraction, and number density of a statistically significant number of precipitates within the resulting matrix at room temperature. However, the performance of ex situ SANS measurements alone does not provide information regarding the probable correlation between interphase precipitation and phase transformations. This limitation makes it necessary to perform in situ and simultaneous studies on precipitation and phase transformations in order to gain an in-depth understanding of the nucleation and growth of precipitates in relation to the evolution of austenite decomposition at high temperatures. A furnace is, thus, designed and developed for such in situ studies in which SANS measurements can be simultaneously performed with neutron diffraction measurements during the application of high-temperature thermal treatments. The furnace is capable of carrying out thermal treatments involving fast heating and cooling as well as high operation temperatures (up to 1200 °C) for a long period of time with accurate temperature control in a protective atmosphere and in a magnetic field of up to 1.5 T. The characteristics of this furnace give the possibility of developing new research studies for better insight of the relationship between phase transformations and precipitation kinetics in steels and also in other types of materials containing nano-scale microstructural features.

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The development of qualitatively new measurement capabilities is often a prerequisite for critical scientific and technological advances. Here we introduce an unconventional quantum probe, an entangled neutron beam, where individual neutrons can be entangled in spin, trajectory and energy. The spatial separation of trajectories from nanometers to microns and energy differences from peV to neV will enable investigations of microscopic magnetic correlations in systems with strongly entangled phases, such as those believed to emerge in unconventional superconductors. We develop an interferometer to prove entanglement of these distinguishable properties of the neutron beam by observing clear violations of both Clauser-Horne-Shimony-Holt and Mermin contextuality inequalities in the same experimental setup. Our work opens a pathway to a future of entangled neutron scattering in matter.

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Pronounced fibres are formed through simple shearing of a dense calcium caseinate dispersion. Both mechanical tests and scanning electron microscopy images demonstrate that the material is anisotropic. It is hypothesised that calcium caseinate aggregates, under shear, align into micro-fibres and bundle further into a hierarchical structure. Yet no direct evidence at the sub-micron length scale can support the assumption. Small angle neutron scattering (SANS) experiments were conducted on calcium caseinate samples prepared at different conditions. Analysis of the SANS data revealed that the micro-fibres have a diameter of ∼100nm and a length of ∼300nm. The addition of enzyme and air contributed to longer and thinner micro-fibres. Furthermore, the extent of fibre alignment at the micro-scale and the macroscopic anisotropy index followed the same trends with varying processing conditions. It is concluded that the material does indeed possess a hierarchical structure and the micro-fibres are responsible for the anisotropy on the macro-scale.

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Phospholipid gum mesostructures formed in crude soybean oil after water degumming (WD) and enzymatic degumming (ED) were studied at a range of phospholipid and water concentrations. For ED, phospholipase C (PLC), phospholipase A2 (PLA2) and a mixture of phospholipases Purifine 3G (3G) were used. Both WD and ED resulted in lamellar liquid-crystalline phases, however, of different topology. The dependence of the bilayer spacings (as observed by SANS and SAXS) on the ratio between amount of water and amphiphilic lipids differed for WD and PLA2 ED vs PLC and 3G ED. This difference was also observed for dynamics at molecular scale as observed by time-domain (TD) NMR and attributed to partial incorporation of diglycerides and free fatty acids into gum bilayers after PLC and 3G ED. Feasibility of using TD-NMR relaxometry for quantification of the gum phase and estimation of degumming efficiency was demonstrated.

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In-situ Small-Angle Neutron Scattering (SANS) is used to determine the time evolution of the chemical composition of precipitates at 650 °C and 700 °C in three micro-alloyed steels with different vanadium (V) and carbon (C) concentrations. Precipitates with a distribution of substoichiometric carbon-to-metal ratios are measured in all steels. The precipitates are initially metastable with a high iron (Fe) content, which is gradually being substituted by vanadium during isothermal annealing. Eventually a plateau in the composition of the precipitate phase is reached. Faster changes in the precipitate chemical composition are observed at the higher temperature in all steels because of the faster vanadium diffusion at 700 °C. At both temperatures, the addition of more vanadium and more carbon to the steel has an accelerating effect on the evolution of the precipitate composition as a result of a higher driving force for precipitation. Addition of vanadium to the nominal composition of the steel leads to more vanadium rich precipitates, with less iron and a smaller carbon-to-metal ratio. Atom Probe Tomography (APT) shows the presence of precipitates with a distribution of carbon-to-metal ratios, ranging from 0.75 to 1, after 10 h of annealing at 650 °C or 700 °C in all steels. These experimental results are coupled to ThermoCalc equilibrium calculations and literature findings to support the Small-Angle Neutron Scattering results.

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Various theories beyond the Standard Model predict new particles with masses in the sub-eV range with very weak couplings to ordinary matter which can possess spin-dependent couplings to electrons and nucleons. We report null results of a search for possible exotic spin-dependent couplings of the neutron which could be induced by the exchange of light weakly coupled bosons or spin-gravity coupling conducted using a spin-echo neutron spectrometer. We constrain the products gA2 and gAgV of the axial vector coupling of the neutron to the matter of the Earth through the exchange of a weakly coupled vector boson for force ranges between the metre scale and the radius of the Earth. We also constrain the constants in some theories of exotic spin-gravity couplings.

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A cold-rolled Ti-V high strength low alloy (HSLA) steel was isothermally annealed at 650 °C and 700 °C for different times. A unique combination of techniques including visible light microscopy (VLM), transmission electron microscopy (TEM), matrix dissolution, small angle neutron scattering (SANS) and hardness measurement has been employed to investigate the evolution of microstructure, hardness and precipitate composition, size and volume fraction. Results show that recrystallization is completed after annealing 8 h at 650 °C and 30 min at 700 °C. Three types of precipitates were identified: large Ti(C,N), medium-size (Ti,V)(C,N) and small (Ti,V)C. The Ti/(Ti+V) atomic ratio in the (Ti,V)C precipitates decreases with increasing radius in the 1–15 nm range, which can be explained by the initial nucleation of a TiC-rich core. The average size of the (Ti,V)C precipitates increases, whereas the number density decreases during annealing. The volume fractions of the three types of precipitates were separately determined by the matrix dissolution method. The volume fractions of (Ti,V)C precipitates obtained by matrix dissolution are comparable even slightly more accurate than those obtained by SANS. The hardness first increases and then decreases when annealing at both temperatures, which can be correlated well with the observed microstructural and precipitate evolution.

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Microemulsion systems consisting of D₂O, an alkane, an anionic internal olefin sulfonate surfactant, salt and secondary butyl alcohol (SBA) as co-solvent are studied in a systematic way. In four different sample sets, either the salt content, SBA content or alkane carbon number was varied in order to study the effects of the individual compounds on the structure sizes making up the microemulsion. Using complementary small-angle neutron scattering techniques SANS and Spin-Echo SANS, it was found that the microemulsion systems exhibit the largest structures in the optimum state (domain size of d/2 =144 nm in the model by Teubner and Strey), where the structure is considered bicontinuous. In comparison, at under- and over-optimum states where the structures consist of emulsified spherical droplets, the smallest measured diameter was 2R = 44 nm. Furthermore, the structure sizes in bicontinuous microemulsions decrease exponentially (down to d/2 =15 nm for pentadecane and 5 wt% SBA) as function of both SBA content and alkane carbon number. The observed trends in structure sizes combined with the trends observed in the area per surfactant molecule, are qualitatively explained with the extended Winsor R-ratio, the HLD-NAC model and surfactant film flexibility arguments.

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The precipitation kinetics of vanadium carbides and its interaction with the austenite-to-ferrite phase transformation is studied in two micro-alloyed steels that differ in vanadium and carbon concentrations by a factor of two, but have the same vanadium-to-carbon atomic ratio of 1:1. Dilatometry is used for heat-treating the specimens and studying the phase transformation kinetics during annealing at isothermal holding temperatures of 900, 750 and 650 °C for up to 10 h. Small-Angle Neutron Scattering (SANS) and Atom Probe Tomography (APT) measurements are performed to study the vanadium carbide precipitation kinetics. Vanadium carbide precipitation is not observed after annealing for 10 h at 900 and 750 °C, which is contrary to predictions from thermodynamic equilibrium calculations. Vanadium carbide precipitation is only observed during or after the austenite-to-ferrite phase transformation at 650 °C. The precipitate volume fraction and mean radius continuously increase as holding time increases, while the precipitate number density starts to decrease after 20 min, which corresponds to the time at which the austenite-to-ferrite phase transformation is finished. This indicates that nucleation and growth are dominant during the first 20 min, while later precipitate growth with soft impingement (overlapping diffusion fields) and coarsening take place. APT shows gradual changes in the precipitate chemical composition during annealing at 650 °C, which finally reaches a 1:1 atomic ratio of vanadium-to-carbon in the core of the precipitates after 10 h.@en

The archetype cubic chiral magnet MnSi is home to some of the most fascinating states in condensed matter, such as skyrmions and a non-Fermi-liquid behavior in conjunction with a topological Hall effect under hydrostatic pressure. Using small angle neutron scattering, we study the evolution of the helimagnetic, conical, and skyrmionic correlations with increasing hydrostatic pressure. We show that the helical propagation vector smoothly reorients from (111) to (100) at intermediate pressures. At higher pressures, above the critical pressure, the long-range helimagnetic order disappears at zero magnetic field. Nevertheless, skyrmion lattices and conical spirals form under magnetic fields, in a part of the phase diagram where a topological Hall effect and a non-Fermi-liquid behavior have been reported. These unexpected results shed light on the puzzling behavior of MnSi at high pressures and the mechanisms that destabilize the helimagnetic long-range order at the critical pressure.

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