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.

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.

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.

The development at the Delft University of Technology (TU Delft, The Netherlands) of an experimental set-up dedicated to high-temperature in situ EXAFS measurements of radioactive, air-sensitive and corrosive fluoride salts is reported. A detailed description of the sample containment cell, of the furnace design, and of the measurement geometry allowing simultaneous transmission and fluorescence measurements is given herein. The performance of the equipment is tested with the room-temperature measurement of thorium tetrafluoride, and the Th—F and Th—Th bond distances obtained by fitting of the EXAFS data are compared with the ones extracted from a refinement of neutron diffraction data collected at the PEARL beamline at TU Delft. The adequacy of the sample confinement is checked with a mapping of the thorium concentration profile of molten salt material. Finally, a few selected salt mixtures (LiF:ThF₄) = (0.9:0.1), (0.75:0.25), (0.5:0.5) and (NaF:ThF₄) = (0.67:0.33), (0.5:0.5) are measured in the molten state. Qualitative trends along the series are discussed, and the experimental data for the (LiF:ThF₄) = (0.5:0.5) composition are compared with the EXAFS spectrum generated from molecular dynamics simulations.