Versatile in situ powder X-ray diffraction cells for solid–gas investigations

Two multipurpose sample cells of quartz (SiO2) or sapphire (Al2O3) capillaries, developed for the study of solid–gas reactions in dosing or flow mode, are presented. They allow fast change of pressure up to 100 or 300 bar (1 bar = 100 000 Pa) and can also handle solid–liquid–gas studies

Metal hydride hydrogen storage and compression systems for energy storage technologies

Along with a brief overview of literature data on energy storage technologies utilising hydrogen and metal hydrides, this article presents results of the related R&D activities carried out by the authors. The focus is put on proper selection of metal hydride materials on the basis of AB5- and AB2-type intermetallic compounds for hydrogen storage and compression applications, based on the analysis of PCT properties of the materials in systems with H2 gas. The article also presents features of integrated energy storage systems utilising metal hydride hydrogen storage and compression, as well as their metal hydride based components developed at IPCP and HySA Systems

Muon spin relaxation as a probe of potential carbon-based hydrogen absorbers

Literature reports of hydrogen absorption by nanostructured carbons range from nothing to tens of weight percent. We studied pristine graphite and two potassium-graphite intercalation compounds (GICs) using muon spin relaxation (μSR), because the positive muon is expected to behave like a light hydrogen isotope. The graphite did not trap muons, but at low temperatures a component of the μSR spectrum from the two GICs could only be modelled by the Kubo-Toyabe function. This result demonstrates that muons were trapped by these samples and implies that \chem{H} atoms would also be localised in these traps, in qualitative agreement with accepted hydrogen absorption results. Thus μSR is confirmed to be a valuable probe of the relative ability of carbon-based samples to bind hydrogen atoms

Tetrahedral occupancy in the

The crystallography of the \chem{Pd}-\chem{D}x system has been studied by in situ neutron powder diffraction at 309\un{{}^{\circ}C}, in the supercritical region, and, after quenching in the pure β phase to 50\un{{}^{\circ}C}, in the two-phase region at 50\un{{}^{\circ}C}. Rietveld profile analysis of the supercritical diffraction patterns showed that 14% of D interstitials were occupying tetrahedral interstices, in sharp contrast to previous studies at lower temperatures. Tetrahedral occupancy was maintained through the two-phase region at 50\un{{}^{\circ}C}. These results are discussed in the light of first-principles total-energy calculations of hydrogen states in palladium

Thermal desorption spectrometer for measuring ppm concentrations of trapped hydrogen

This paper describes an ultra-high-vacuum thermal desorption spectrometer, designed to study hydrogen in steels at ∼1 wt ppm (∼50 atomic ppm) concentration. The high sensitivity achieved also facilitates the analysis of surface phenomena. The instrument was evaluated with model materials and provided good measurements of diffusible hydrogen. A hydrogen peak at ∼350 °C was identified for steels exposed to water during hydrogen charging, and attributed to water molecules adsorbed on the sample surface for samples exposed to the laboratory atmosphere for times as short as 1 min. Recommendations are made for precautions to be taken when handling the samples

Mechanism of the Alpha-to-Beta phase transformation in the LaNi5-H2 system

High-energy synchrotron in situ X-ray powder diffraction has been used to elucidate the mechanism of the hydriding phase transformation in a LaNi5 model hydrogen storage intermetallic in real time. The transformation proceeds at 10 °C via the transient growth of an interfacial phase, the γ phase, with lattice parameters intermediate between those of the α (dilute solid solution) and β (concentrated hydride) phases. The γ phase forms to partially accommodate the 24% change in unit cell volume between the α and β phases during hydriding and dehydriding. The α, γ and β phases coexist at the nanoscopic level

Sensitivity of peak positions to flight-path parameters in a deep-inelastic scattering neutron TOF spectrometer

The effects of small changes in flight-path parameters (primary and secondary flight paths, detector angles), and of displacement of the sample along the beam axis away from its ideal position, are examined for an inelastic time-of-flight (TOF) neutron spectrometer, emphasising the deep-inelastic regime. The aim was to develop a rational basis for deciding what measured shifts in the positions of spectral peaks could be regarded as reliable in the light of the uncertainties in the calibrated flight-path parameters. Uncertainty in the length of the primary or secondary flight path has the least effect on the positions of the peaks of H, D and He, which are dominated by the accuracy of the calibration of the detector angles. This aspect of the calibration of a TOF spectrometer therefore demands close attention to achieve reliable outcomes where the position of the peaks is of significant scientific interest and is discussed in detail. The corresponding sensitivities of the position of peak of the Compton profile, J(y), to flight-path parameters and sample position are also examined, focusing on the comparability across experiments of results for H, D and He. We show that positioning the sample to within a few mm of the ideal position is required to ensure good comparability between experiments if data from detectors at high forward angles are to be reliably interpreted

Distinguishing new science from calibration effects in the electron-volt neutron spectrometer VESUVIO at ISIS

The "standard" procedure for calibrating the Vesuvio eV neutron spectrometer at the ISIS neutron source, forming the basis for data analysis over at least the last decade, was recently documented in considerable detail by the instrument’s scientists. Additionally, we recently derived analytic expressions of the sensitivity of recoil peak positions with respect to fight-path parameters and presented neutron–proton scattering results that together called in to question the validity of the "standard" calibration. These investigations should contribute significantly to the assessment of the experimental results obtained with Vesuvio. Here we present new results of neutron–deuteron scattering from D2 in the backscattering angular range (theata > 90 degrees) which are accompanied by a striking energy increase that violates the Impulse Approximation, thus leading unequivocally the following dilemma: (A) either the "standard" calibration is correct and then the experimental results represent a novel quantum dynamical effect of D which stands in blatant contradiction of conventional theoretical expectations; (B) or the present "standard" calibration procedure is seriously deficient and leads to artificial outcomes. For Case(A), we allude to the topic of attosecond quantumdynamical phenomena and our recent neutron scattering experiments from H2 molecules. For Case(B),some suggestions as to how the "standard" calibration could be considerably improved are made