Use of a miniature diamond-anvil cell in a joint X-ray and neutron high-pressure study on copper sulfate pentahydrate

Single-crystal X-ray and neutron diffraction data are usually collected using separate samples. This is a disadvantage when the sample is studied at high pressure because it is very difficult to achieve exactly the same pressure in two separate experiments, especially if the neutron data are collected using Laue methods where precise absolute values of the unit-cell dimensions cannot be measured to check how close the pressures are. In this study, diffraction data have been collected under the same conditions on the same sample of copper(II) sulfate pentahydrate, using a conventional laboratory diffractometer and source for the X-ray measurements and the Koala single-crystal Laue diffractometer at the ANSTO facility for the neutron measurements. The sample, of dimensions 0.40 × 0.22 × 0.20 mm3 and held at a pressure of 0.71 GPa, was contained in a miniature Merrill–Bassett diamond-anvil cell. The highly penetrating diffracted neutron beams passing through the metal body of the miniature cell as well as through the diamonds yielded data suitable for structure refinement, and compensated for the low completeness of the X-ray measurements, which was only 24% on account of the triclinic symmetry of the sample and the shading of reciprocal space by the cell. The two data-sets were combined in a single `XN' structure refinement in which all atoms, including H atoms, were refined with anisotropic displacement parameters. The precision of the structural parameters was improved by a factor of up to 50% in the XN refinement compared with refinements using the X-ray or neutron data separately.

Unraveling the magnetic softness in Fe–Ni–B-based nanocrystalline material by magnetic small-angle neutron scattering

Magnetic small-angle neutron scattering is employed to investigate the magnetic interactions in (Fe0.7Ni0.3)86B14 alloy, a HiB-NANOPERM-type soft magnetic nanocrystalline material, which exhibits an ultrafine microstructure with an average grain size below 10 nm. The neutron data reveal a significant spin-misalignment scattering which is mainly related to the jump of the longitudinal magnetization at internal particle–matrix interfaces. The field dependence of the neutron data can be well described by micromagnetic small-angle neutron scattering theory. In particular, the theory explains the `clover-leaf-type' angular anisotropy observed in the purely magnetic neutron scattering cross section. The presented neutron data analysis also provides access to the magnetic interaction parameters, such as the exchange-stiffness constant, which plays a crucial role towards the optimization of the magnetic softness of Fe-based nanocrystalline materials.

Non-ambient X-ray and neutron diffraction of novel relaxor ferroelectric xBi2(Zn2/3,Nb1/3)O3–(1 – x)BaTiO3

The first determination of the phase diagram of the novel ferroelectric relaxor xBi(Zn2/3Nb1/3)O3–(1 − x)BaTiO3 (BZN-BT) has been achieved with a combination of high-resolution X-ray and neutron diffraction up to the miscibility limit near x(BZN) = 20.0% over a temperature range 20 < T < 400 K. The combined X-ray and neutron data show that the instability within the xBZN-(1−x)BT system reaches a maximum at x = 3.9% and is driven by B-site displacement and distortion of the oxygen octahedra in the polar phases. Composition-dependent effects include a narrow Amm2-dominated region focused at x = 3.9%, significant convergence of the lattice parameters in both P4mm and Amm2 phases, and sharp maxima in piezoelectric coefficient d 33 and maximum polarization P max. Lattice parameter dilation at x ≥ 4.0% was observed for both P4mm and Amm2 unit cells, alongside the first appearance of Pm 3 m at 295 K and the onset of significant dielectric relaxation. Low-temperature neutron diffraction indicated a weak or non-existent temperature dependence on the transition from ferroelectric at x = 3.9% to ferroelectric relaxor at x = 4.0%. Temperature-dependent phase transitions were eliminated near x = 3.0%, with the ferroelectric limit observed at x = 5.0% and a transition to a low-loss relaxor dielectric near x = 8.0%.

Calculation and experimental analysis of benchmark experiments with a fast neutron spectrum and models of sodium and lead cooled fast reactors using different evaluated nuclear data libraries

The paper presents the results of a comparative analysis of criticality calculations using a Monte-Carlo code with the BNAB-93 and BNAB-RF neutron group constants, as well as with evaluated neutron data files from the Russian ROSFOND evaluated nuclear data library and other evaluated nuclear data libraries (ENDF, JEFF, JENDL) from different years. A set of integral experiments on BFS critical assemblies carried out in different years at the Institute of Physics and Power Engineering (60 different critical configurations) was analyzed. The considered integral experiments are included in the database of evaluated experimental neutronic data used to justify the neutronic performance of sodium and lead cooled fast reactors, to verify codes and nuclear data as well as to estimate uncertainties in neutronic parameters due to the nuclear data uncertainties. It has been shown that the ROSFOND evaluated nuclear data library is a library that minimizes the calculation and experimental discrepancies for the considered set of integral experiments. The paper also presents the results of criticality calculations for models of sodium and lead cooled fast reactors based on different evaluated neutron data libraries and provides estimates for the uncertainty in criticality associated with nuclear data.

THE TCA BENCHMARK FOR VALIDATION OF TEMPERATURE FEEDBACK CALCULATIONS

The TCA benchmark was investigated as a possible candidate for validation of temperature feedback calculations. This benchmark has low-enriched uranium fuel, light water moderation and reflection, and a temperature range of 20–60 °C. The use of three different nuclear data libraries was considered, viz. ENDF/B-VIII.0, JEFF-3.3, and JENDL-4.0. Since the results were not as good as hoped for, additional studies were performed to identify the cause(s) of discrepancies. The benchmark values depend on a choice of delayed neutron data, so it was investigated whether this could be the cause of discrepancies. Also, an assessment was made based on critical configurations only, i.e. avoiding the use of delayed neutron data, whether the calculations exhibit a bias in relation to the benchmark in the results for the effect of temperature. Indications were found that such a bias exists. It is concluded that the choice of delayed neutron data has a significant effect on the benchmark values themselves. The use of three major nuclear data libraries leads to a range of benchmark values for each configuration, rather than one value. Also, one has to take into account the possibility of a bias in the calculation of temperature effects. It is not clear at this point what the cause of the bias is.

A beginner’s guide to neutron macromolecular crystallography

Hydrogen atoms drive biological structure and function, but the lightest element is often unseen in three-dimensional macromolecule structures, hampering our understanding of biochemical processes. This guide will i) present how neutron crystallography uniquely reveals the experimental positions of hydrogen atoms and resolves mechanical controversies, ii) briefly introduce beamlines at neutron facilities, iii) discuss sample requirements and preparation and iv) familiarize the reader with neutron data and refinement statistics.

Precision neutronic calculations of experiments on the neutron transmission through the reflector layers at the BFS critical facilities for expanding the verification database to justify lead cooled fast reactor designs

The paper presents the results of the efforts concerned with expanding the verification database and estimating the calculation uncertainty of the power density in the steel reflector of lead cooled fast reactor designs based on experiments performed in different years at the BFS critical assemblies by analyzing and revising earlier calculation and experimental studies on the transmission of neutrons through the steel reflector layers. The discussion includes experiments at the BFS-66 critical assembly to model neutron and photon fluxes in the reactor core shielding compositions, as well as experiments at the BFS-64 and BFS-80-2 critical assemblies to model the transmission of neutrons and gamma quanta through the reflector layers of various materials. The information provided in earlier materials with the descriptions of the above experiments has been analyzed and expanded through respective data required to prepare precision calculation models for Monte-Carlo neutronic codes. Precision neutronic models have been developed based on actualized and updated data with a detailed description of the BFS heterogeneous structure and experimental devices, and test calculations have been carried out to confirm their efficiency. The calculations of key neutronic characteristics measured at the BFS-66, -64 and -80-2 assemblies were performed using codes based on the Monte Carlo method (MCU-BR, MCNP, MMK-RF, MMK-ROKOKO) with BNAB-RF and MDBBR50 neutron data and the ROSFOND evaluated neutron data library. The developed precision calculation neutronic models of the experiments discussed can be used to justify lead cooled fast reactor designs, to verify neutronic codes and neutron data, and to evaluate the associated uncertainties.