In this work, Zr addition is proposed to refine the nanoparticle dispersion in an ODS RAF steel of composition Fe-14Cr-2W-0.3Zr-0.24Y (wt.%). Three batches of material are obtained using pre-alloyed atomized powder, where yttrium is directly introduced in the melt, and manufactured through three different processing routes. First route is based on the newly developed STARS route that aims to avoid subsequent mechanical alloying. The second route explores the impact of mechanical alloying in pre-oxidized powders. The third route uses mechanically alloyed powders without the pre-oxidation process. The ODS-powders were individually consolidated by hot isostatic pressing and later hot rolled. The obtained materials were characterized by small-angle neutron scattering (SANS) and X-ray absorption spectroscopy (XAS) techniques. SANS and XAS analysis point out the absence of oxide nanoparticles in the material based on the STAR route. SANS analysis confirms that the mechanically alloyed materials do exhibit the presence of nanoparticles. These are identified as Zr-O-rich nanoprecipitates by XAS and the calculated A-ratio by SANS is linked with the phase Y2Zr2O7. Their radii are in the range of 3–3.6 nm. XAS results show that mechanical alloying minimizes the initial differences regarding the oxidation state between the ODS powders with and without pre-oxidation.@en

We have designed and realized a temperature and pressure controlled cell for Neutron Reflectometry (NR) and Small Angle Neutron Scattering (SANS) that is compatible with simultaneous optical transmission and resistivity measurements. The cell can accommodate samples up to 102 mm (4 inch) in diameter, can be pressurized from vacuum up to 10 bar gas pressure and the sample temperature can be controlled up to 350°C. The four single crystal quartz windows ensure both a good neutron and optical transmission and hence can be used in combination with in-situ optical transmission measurements. We present the cell and illustrate its performance with a series of neutron reflectometry experiments performed on Ta based thin films under a hydrogen containing atmosphere.

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An ODS steel with nominal composition Fe–14Cr–2W–0.4Ti-0.3Y2O3 (wt.%) was produced by mechanical alloying and compacted by hot isostatic pressing (HIP) followed by hot cross rolling (HCR). To check the effects of thermal aging at relevant temperatures of operation in fusion power plants, the alloy was thermally aged at 873 K for 2000 h. In this work, small-angle neutron scattering (SANS) and X-ray absorption spectroscopy (XAS) techniques are used for the advanced characterization of secondary phases and the oxide nanoparticle dispersion. SANS results show that the oxide nanoparticles remain stable after the thermal aging treatment. Composition of the oxide nanoparticles was identified as Y2TiO5 or Y2Ti2O7 by SANS, while non-stoichiometry was found by XAS analysis. Laves phase precipitation after the thermal aging treatment is further confirmed by SANS, from the magnetic anisotropic contribution to the scattering intensity associated to this metallic phase, and by XANES.@en

We conduct simulations of Spin Echo Small Angle Neutron Scattering (SESANS) by employing Monte Carlo methods to a setup using four magnetic Wollaston prisms. Our primary focus involves the validation of these models, encompassing monochromatic scenarios across various neutron wavelengths to ascertain the reliability of the simulations. Subsequently, we extend this validation to encompass simulations in time-of-flight mode. Our model consistently and precisely predicts the scattering patterns emanating from dilute spheres in both monochromatic and time-of-flight modes. Notably, it also accurately reproduces the intricate encoding associated with scattering occurring between the third and fourth magnetic Wollaston prism, which provides us with another approach to increase the solid angle coverage of a SESANS instrument. This validation process conclusively demonstrates the efficacy of our simulation methods. Importantly, it paves the way for simulating more intricate and realistic instrumental configurations, broadening the horizons for future research endeavours.@en

Waterborne polyurethane (WPU) has attracted significant interest as a promising alternative to solvent-based polyurethane (SPU) due to its positive impact on safety and sustainability. However, significant limitations of WPU, such as its weaker mechanical strength, limit its ability to replace SPU. Triblock amphiphilic diols are promising materials to enhance the performance of WPU due to their well-defined hydrophobic-hydrophilic structures. Yet, our understanding of the relationship between the hydrophobic-hydrophilic arrangements of triblock amphiphilic diols and the physical properties of WPU remains limited. In this study, we show that by controlling the micellar structure of WPU in aqueous solution via the introduction of triblock amphiphilic diols, the postcuring efficiency and the resulting mechanical strength of WPU can be significantly enhanced. Small-angle neutron scattering confirmed the microstructure and spatial distribution of hydrophilic and hydrophobic segments in the engineered WPU micelles. In addition, we show that the control of the WPU micellar structure through triblock amphiphilic diols renders WPU attractive in the applications of controlled release, such as drug delivery. Here, curcumin was used as a model hydrophobic drug, and the drug release behavior from WPU-micellar-based drug delivery systems was characterized. It was found that curcumin-loaded WPU drug delivery systems were highly biocompatible and exhibited antibacterial properties in vitro. Furthermore, the sustained release profile of the drug was found to be dependent on the structure of the triblock amphiphilic diols, suggesting the possibility of controlling the drug release profile via the selection of triblock amphiphilic diols. This work shows that by shedding light on the structure-property relationship of triblock amphiphilic diol-containing WPU micelles, we may enhance the applicability of WPU systems and move closer to realizing their promising potential in real-life applications.

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Understanding the relationship between structure, ionic conductivity, and synthesis is the key to the development of superionic conductors. Here, a series of Li_3-3xM_1+xCl₆ (−0.14 < x ≤ 0.5, M = Tb, Dy, Ho, Y, Er, Tm) solid electrolytes with orthorhombic and trigonal structures are reported. The orthorhombic phase of Li–M–Cl shows an approximately one order of magnitude increase in ionic conductivities when compared to their trigonal phase. Using the Li–Ho–Cl components as an example, their structures, phase transition, ionic conductivity, and electrochemical stability are studied. Molecular dynamics simulations reveal the facile diffusion in the z-direction in the orthorhombic structure, rationalizing the improved ionic conductivities. All-solid-state batteries of NMC811/Li_2.73Ho_1.09Cl₆/In demonstrate excellent electrochemical performance at both 25 and −10 °C. As relevant to the vast number of isostructural halide electrolytes, the present structure control strategy guides the design of halide superionic conductors.

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We report the design, construction, and initial tests of a hyperpolariser to produce polarised ¹²⁹Xe and ³He gas for medical imaging of the lung. The hyperpolariser uses the Spin-Exchange Optical Pumping method to polarise the nuclear spins of the isotopic gas. Batch mode operation was chosen for the design to produce polarised ¹²⁹Xe and polarised ³He. Two-side pumping, electrical heating and a piston to transfer the polarised gas were some of the implemented techniques that are not commonly used in hyperpolariser designs. We have carried out magnetic resonance imaging experiments demonstrating that the ³He and ¹²⁹Xe polarisation reached were sufficient for imaging, in particular for in vivo lung imaging using ¹²⁹Xe. Further improvements to the hyperpolariser have also been discussed.

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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 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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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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As protons have a localized depth-dose distribution, proton therapy nowadays is a form of radiotherapy that is being implemented for part of the cancer patients. Compared to photon therapy it allows more precise targeting of tumours and sparing of surrounding healthy tissue. Besides patient treatment, research on proton therapy topics is being done to gain more knowledge on and keep improving the technique. Since the 1950s almost 100 proton therapy facilities are operating clinically worldwide. One of those facilities is HollandPTC, a proton therapy center located in Delft, The Netherlands. The ProBeam Varian cyclotron serves two treatment gantries, an eye treatment room, and a research experimental room. The experimental room is dedicated to research topics in the proton therapy field and is equipped with a fixed horizontal beam line that can be used for physics experiments and also for radiobiological experiments. In order to perform those types of research the beam needs to be fully characterized in terms of dose, shape, size and energy, this is the purpose of this work. The second goal was to commence with a setup for creating homogeneous fields by means of passive scattering and determine the optimal distances required between the elements of the setup. The single pencil beam characterization has been done by performing a large variety of experiments, making use of setups with different types of detectors. The experiments include beam spot, beam envelope, beam current, and depth-dose distribution measurements, and have been performed for nominal beam energies between 70 and 240MeV. For the passively scattered field a dual ring setup has been implemented. Spread-out Bragg peaks have been created with a ridge filter. An energy of 150 MeV was used, as the scattering elements have been designed for this energy specifically. The single pencil beam characterization resulted in beam spot sizes at the isocenter varying from 3.54 mm for 240 MeV, up to 5.47 mm for 70 MeV, with an asymmetry of 1.7% at most. The beam envelope measurements showed that the beam spot size just after the exit window is 2-3 mm and diverges up to 12 mm at 2 m from the exit window. The beam current measurements gave the transmission efficiency of the system, ranging from 0.04% for a 70 MeV beam up to 5.6% for 240 MeV, increasing exponentially. The depth-dose measurements provided the difference between the nominal beam energy and the beam energy at the isocenter. The difference becomes smaller as the nominal beam energy increases and is 2.4% for a 70 MeV nominal beam and 0.3% for a 230 MeV nominal beam. With the dual ring setup fields of up to 25 cm in diameter have been formed with a uniformity of at least 97%. The ridge filter created a spread-out Bragg peak of 2.8 cm with a uniformity of 98% and also gave good results for other beam energies (100-200MeV). It can be concluded that the goals of the project have been reached as the beam has been characterized in terms of shape, current, and energy. Also some preliminary work for the passive field has been accomplished. The work on the dual ring setup can be further expanded by placing the ridge filter and a collimator in the setup, after which the field can be characterized in terms of dose. The results obtained from the single pencil beam characterization allowed for the first physics experiments to start at the experimental room of HollandPTC during the last year.

The initial formation stages of surfactant-templated silica thin films which grow at the air-water interface were studied using combined spin-echo modulated small-angle neutron scattering (SEMSANS) and small-angle neutron scattering (SANS). The films are formed from either a cationic surfactant or nonionic surfactant (C16EO8) in a dilute acidic solution by the addition of tetramethoxysilane. Previous work has suggested a two stage formation mechanism with mesostructured particle formation in the bulk solution driving film formation at the solution surface. From the SEMSANS data, it is possible to pinpoint accurately the time associated with the formation of large particles in solution that go on to form the film and to show their emergence is concomitant with the appearance of Bragg peaks in the SANS pattern, associated with the two-dimensional hexagonal order. The combination of SANS and SEMSANS allows a complete depiction of the steps of the synthesis that occur in the subphase.@en

SESANS data analysis has been implemented in the SasView software package, allowing SESANS experiments to be analyzed using a numerical Hankel transformation of isotropic small-angle scattering (SAS) models. The error of the numerical approximation is three orders of magnitude below typical experimental errors. All advanced data fitting features of SasView (multi-model fitting, batch fitting, and simultaneous/constrained fitting) are now also available for SESANS and this is demonstrated by examples of fitting SAS models to SESANS measurements.

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We investigate the morphological development of polystyrene (PS)-C 60 nanocomposites along the length of a prototype co-rotating twin-screw extruder with sampling capabilities. The effects of C 60 concentration and output on the morphological evolution along the extruder are studied employing a suite of characterization techniques covering a wide range of length-scales, thereby shedding new light on the dispersion mechanism in this model system. We show that the relatively new spin-echo small-angle neutron scattering (SESANS) technique is well suited to probe both the distribution and the dispersion of C 60 . SESANS complements optical microscopy (OM) data as it covers sampling areas several orders of magnitude larger than OM. The multi-scale morphological information conveyed by OM, SESANS, SANS and rheological data shows that for larger outputs, C 60 agglomerates are eroded as they travel along the extruder, resulting in C 60 dispersion and distribution at both molecular and micrometric levels. The picture is more complex when smaller feed rates are used, as the evolution of C 60 dispersion depends on the C 60 loading. For larger C 60 contents, agglomeration develops along the extruder, whereas dispersion is improved for smaller C 60 contents. Overall, it is concluded that an over-high feed rate in extrusion does not necessarily result in a bigger size of the nanoparticle agglomerates because of the complex interplay between stresses and residence time. @en

Several methods of polarized neutron scattering call for a zero magnetic field (ZF) region to reduce magnetic field integral aberrations while preserving the neutron polarization. Though the design for large angle neutron scattering has been presented in various places, the design characterization and tuning has not been discussed before. In this report, the tuning procedure will be discussed with both neutron polarization transport method and utilization of fluxgate magnetometers. As a tuning procedure, polarized neutrons are sensitive to any local field distortions along all trajectories within the beam, but the process is slow. With fluxgates, the entire beam region cannot be accessed simultaneously, but very fast and precise measurements can be made in accessible regions of interest. Consequently, we would like to benchmark the usage of fluxgates as a fast tuning probe compared with polarization measurements made with neutrons. Polarization transport results for tuned ZF chambers, up to 2.25 m in length, are presented.

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The energy resolution of the conventional way of measuring a small change in a phonon dispersion curve using neutron scattering is restricted by the relatively coarse intrinsic resolution ellipsoid of the neutron triple-axis spectrometer (TAS). By implementing inelastic neutron spin echo on the host TAS using the Larmor precession of the neutron spin, the energy resolution of such measurements can be further improved without reducing the resolution ellipsoid. Measurements of the temperature-dependent phonon energy change are demonstrated using superconducting magnetic Wollaston prisms at the HB-1 instrument of the High-Flux Isotope Reactor at Oak Ridge National Laboratory, and the achievable resolution is <10 µeV.@en

We investigated the effect of the feeding formulation (premixed powders of pure components versus solvent-blended mixture) of polystyrene–C60 composites on the dispersion and reagglomeration phenomena developing along the barrel of a twin-screw extruder. The dispersion of C60 in the PS matrix is studied over different length scales using a combination of optical microscopy, spin-echo small-angle neutron scattering (SESANS), small-angle neutron scattering (SANS), small-angle X-ray scattering (SAXS), and wide-angle X-ray scattering (WAXS). When a solvent-blended mixture is used as the feeding formulation, the inlet material contains essentially molecularly dispersed C60 as revealed by the nanodomains with very small phase contrast. However, C60 reagglomeration occurs along the extruder, creating a morphology still containing only nanodomains but with much higher phase contrast. In the case of mixed powders, the material evolves from the initial macroscopic mixture of pure polystyrene and C60 into a composite simultaneously containing micro- and nanoaggregates of C60 as well as C60 molecularly dispersed in the matrix. Our results show that the two different initial feeding formulations with widely different initial morphologies converge along the extruder, through opposite morphological pathways, into a similar final nanomorphology which is dictated by the interplay between the thermodynamics of the system and the flow. Correlations between the morphological evolution along the extruder and the thermorheological properties of the composites are identified.@en

The neutron Larmor diffraction technique has been implemented using superconducting magnetic Wollaston prisms in both single-arm and double-arm configurations. Successful measurements of the coefficient of thermal expansion of a single-crystal copper sample demonstrates that the method works as expected. The experiment involves a new method of tuning by varying the magnetic field configurations in the device and the tuning results agree well with previous measurements. The difference between single-arm and double-arm configurations has been investigated experimentally. We conclude that this measurement benchmarks the applications of magnetic Wollaston prisms in Larmor diffraction and shows in principle that the setup can be used for inelastic phonon line-width measurements. The achievable resolution for Larmor diffraction is comparable to that using Neutron Resonance Spin Echo (NRSE) coils. The use of superconducting materials in the prisms allows high neutron polarization and transmission efficiency to be achieved.@en