The horizontal time-of-flight neutron reflectometer at the reactor of the Delft University of Technology, The Netherlands, has been completely renewed, relocated, and upgraded and allows for the study of air/liquid, solid/liquid, and solid/air interfaces. Innovations in the redesign include (i) a completely flexible double disk chopper system allowing to choose the optimal wavelength resolution with exchangeable neutron guide sections between the chopper disks to increase intensity, (ii) a movable second diaphragm just before the sample position to better control the beam footprint on the sample and effectively decrease counting times, and (iii) guides along the entire flight path of the neutron reflectometer. The performance of the renewed reflectometer is illustrated with measurements of hydrogen sensing materials.

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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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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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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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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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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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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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Nanostructured metal hydrides are able to efficiently detect hydrogen in optical sensors. In the literature, two nanostructured systems based on metal hydrides have been proposed for this purpose each with its own detection principle: continuous sub-100 nm thin films read out via optical reflectance/transmittance changes and nanoparticle arrays for which the detection relies on localized surface plasmon resonance. Despite their apparent similarities, their optical and structural response to hydrogen has
never been directly compared. In response, for the case of Pd1−yAuy (y = 0.15−0.30) alloys, we directly compare these two systems and establish that they are distinctively different. We show that the dissimilar optical response is not caused by the different optical readout principles but results from a fundamentally different structural
response to hydrogen due to the different nanostructurings. The measurements empirically suggest that these differences cannot be fully accounted by surface effects but that the nature of the film−substrate interaction plays an important role and affects both the hydrogen solubility and the metal-to-metal hydride transition. In a broader perspective, our results establish that the specifics of nanoconfinement dictate the structural properties of metal hydrides, which in turn control the properties of nanostructured devices including the sensing characteristics of optical hydrogen sensors and hydride-based active plasmonic systems.@en

Percutaneous medical devices are prone to bacterial contamination that causes dramatic clinical conditions. At the percutaneous level of dental implant systems, microbial pathogens induce biofilm formation that may result in bone resorption and dental implant loss. In view of peri-implantitis caused by bacterial inflammation at the percutaneous abutment region, we here establish a novel drug release system based on layer-by-layer (LbL)-deposited poly(acrylic acid) (PAA) and poly-L-lysine (PLL) coatings on titanium (Ti). Detailed multilayer coating characterization was performed by different microscopy and spectroscopy techniques to probe physical and chemical properties. Our data revealed a significant difference in roughness average between ten double layers coated (141 nm ±30) and uncoated Ti discs (115 nm ±40). Although roughness of the coatings increased significantly after immersion in water for 24 h at 37 °C, this physical property remained below 200 nm. Coating stability was confirmed under neutral and acidic pH, mimicking healthy and diseased/inflammatory environments, respectively. LbL coatings supported in vitro human keratinocytes growth, demonstrating absence of cytotoxic effects. Tetracycline (TC) showed an initial burst release under neutral and acidic conditions, which further demonstrated robust antibacterial efficacy against Porphyromonas gingivalis. However, a convenient pH-dependent 2-folds increase in TC release was observed for coatings incubated at pH = 4.5. Sustained TC release was observed from coatings up till 15 days of incubation in both pH conditions. These results demonstrate the potential application of this simple surface modification to leverage anti-bacterial efficacy at the percutaneous abutment region.

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A time-of-flight modulation of intensity by zero effort spectrometer mode has been developed for the Larmor instrument at the ISIS pulsed neutron source. The instrument utilizes resonant spin flippers that employ electromagnets with pole shoes, allowing the flippers to operate at frequencies up to 3 MHz. Tests were conducted at modulation frequencies of 103 kHz, 413 kHz, 826 kHz, and 1.03 MHz, resulting in a Fourier time range of ∼0.1 ns to 30 ns using a wavelength band of 4 Å-11 Å.

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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 detection of hydrogen in a fast, efficient and accurate way is vital for its safe handling in industrial processes and in its use as an energy carrier. Thin film metal hydrides are able to probe the hydrogen pressure, often relying on a change of the optical properties of a sensing layer comprised of palladium and alloys thereof. Apart from hysteresis, these palladium-based thin films suffer from a limited operating range. Here, we study the optical and structural properties of palladium capped hafnium and tantalum thin films. Both tantalum and hafnium thin films offer a stable and hysteresis-free optical response to hydrogen over a much larger pressure range than palladium-based films. Remarkably, the hydrogen content in both cases proves to be linear with the optical signal. In a wider perspective, these results illustrate that palladium-capped transition metals provide ample opportunities to design optical hydrogen sensors with desired properties.

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RF coils have been routinely used for Larmor labelling on the Offspec instrument at ISIS. These coils encode directional information via the neutron polarization using a series of parallelogram-shaped pole shoes which can be tuned to different angles with an RF gradient flipper in the centre of each magnet. We report on measurements of the magnetic field integral through the coils in reflection geometry for a range of scattering angles and different pole shoe angles. Such information is mapped out by measuring the phase of the neutron polarisation and the measurements are discussed in light of data on patterned silicon gratings with a dewetted polymer and the visibility of in-plane structures to SERGIS.

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Nanosteels are used in automotive applications to accomplish resource-efficiency while providing high-tech properties. Quantitative data and further understanding on the precipitation kinetics in Nanosteels can contribute to fulfil this goal. Small-Angle Neutron Scattering measurements are performed on a Fe-C-Mn-V steel, previously heat-treated in a dilatometer at 650°C for several holding times from seconds to 10 hours. The evolution of the precipitate volume fraction, size distribution and number density is calculated by fitting the experimental Small-Angle Neutron Scattering curves. The effect of phase transformation on precipitation kinetics is also discussed. Complementary Transmission Electron Microscopy, Scanning Electron Microscopy and Inductively Coupled Plasma Optical Emission Spectroscopy measurements are performed to support the Small-Angle Neutron Scattering data analysis. @en

A review is given of double and single arm Larmor diffraction. With the former a lattice-spacing resolution down to 10-6 can be obtained. The latter is a good high-resolution alternative if the sample or sample environment disturbs the magnetic field, e.g. ferromagnetic samples or applied magnetic fields. By choosing the tilt angle of the precession fields the optimum resolution can be set at a scattering angle at choice. The resolution for both single-crystal and polycrystalline samples is discussed in depth and is compared with conventional neutron-diffraction techniques.@en

Hydrogen detection is essential for its implementation as an energy vector. So far, palladium is considered to be the most effective hydrogen sensing material. Here we show that palladium-capped hafnium thin films show a highly reproducible change in optical transmission in response to a hydrogen exposure ranging over six orders of magnitude in pressure. The optical signal is hysteresis-free within this range, which includes a transition between two structural phases. A temperature change results in a uniform shift of the optical signal. This, to our knowledge unique, feature facilitates the sensor calibration and suggests a constant hydrogenation enthalpy. In addition, it suggests an anomalously steep increase of the entropy with the hydrogen/metal ratio that cannot be explained on the basis of a classical solid solution model. The optical behaviour as a function of its hydrogen content makes hafnium well-suited for use as a hydrogen detection material.

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We describe theoretical and practical aspects of spin-echo modulated small-angle neutron scattering (SEMSANS) as well as the potential combination with SANS. Based on the preliminary technical designs of SKADI (a SANS instrument proposed for the European Spallation Source) and a SEMSANS add-on, we assess the practicability, feasibility and scientific merit of a combined SANS and SEMSANS setup by calculating tentative SANS and SEMSANS results for soft matter, geology and advanced material samples that have been previously studied by scattering methods. We conclude that lengths from 1 nm up to 0.01 mm can be observed simultaneously in a single measurement. Thus, the combination of SANS and SEMSANS instrument is suited for the simultaneous observation of a wide range of length scales, e.g. for time-resolved studies of kinetic processes in complex multiscale systems.@en

The performance of the new neutron powder diffraction instrument PEARL that is installed at the research reactor of Delft University of Technology is reported. It is based on the optimization concepts developed by Cussen [Nucl. Instrum. Methods Phys. Res. Sect. A (2007), 583, 394-406], which lead to high performance competing with existing constant-wavelength neutron powder diffractometers, despite the relatively low source brightness of the 2MW reactor of Delft University of Technology.This manuscript describes the novel neutron powder diffractometer PEARL at Delft University of Technology and shows the first experimental results.

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Nanostructuring is widely applied in both battery and hydrogen materials to improve the performance of these materials as energy carriers. Nanostructuring changes the diffusion length as well as the thermodynamics of materials. We studied the impact of nanostructuring on the hydrogenation in a model system consisting of a thin film of magnesium sandwiched between two titanium layers and capped with palladium. While we verified optically the coexistence of the metallic α-MgDx and the insulating β-MgD2–y phase, neutron reflectometry shows significant deviations from the thermodynamic solubility limits in bulk magnesium during the phase transformation. This suggests that the kinetics of the phase transformation in nanostructured battery and hydrogen storage systems is enhanced not only as a result of the reduced length scale but also due to the increased solubility in the parent phases.@en