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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.