A clamp pressure cell for neutron scattering experiments at low temperatures and in external magnetic fields under pressure up to 2 GPa has been fabricated and tested. The cell provides optical access to the sample space that allows instantaneous pressure determination during sample loading, cooling and measuring using ruby and/or samarium doped strontium tetraborate fluorescence monitoring. A new calibration curve of the pressure-induced shift of the 7 D0 − 5 F0 (0-0) line in the fluorescent spectrum of SrB4O7:Sm 2+ for moderate pressures, P 2 GPa, is given.

A diamond cell optimized for single-crystal neutron diffraction is described. It is adapted for work at several of the single-crystal diffractometers of the Spallation Neutron Source and the High Flux Isotope Reactor at the Oak Ridge National Laboratory (ORNL). A simple spring design improves portability across the facilities and affords load maintenance from offline pressurization and during temperature cycling. Compared to earlier prototypes, pressure stability of polycrystalline diamond (Versimax®) has been increased through double-conical designs and ease of use has been improved through changes to seat and piston setups. These anvils allow ∼30%-40% taller samples than possible with comparable single-crystal anvils. Hydrostaticity and the important absence of shear pressure gradients have been established with the use of glycerin as a pressure medium. Large single-crystal synthetic diamonds have also been used for the first time with such a clamp-diamond anvil cell for pressures close to 20 GPa. The cell is made from a copper beryllium alloy and sized to fit into ORNL’s magnets for future ultra-low temperature and high-field studies. We show examples from the Spallation Neutron Source’s SNAP and CORELLI beamlines and the High Flux Isotope Reactor’s HB-3A and IMAGINE beamlines.

Gas-solid interfaces enable a multitude of industrial processes, including heterogeneous catalysis; however, there are few methods available for studying the structure of this interface under operating conditions. Here, we present a new sample environment for interrogating materials under gas-flow conditions using time-of-flight neutron scattering under both constant and pulse probe gas flow. Outlined are descriptions of the gas flow cell and a commissioning example using the adsorption of N by Ca-exchanged zeolite-X (NaCaAlSiO,x ≈ 38). We demonstrate sensitivities to lattice contraction and N adsorption sites in the structure, with both static gas loading and gas flow. A steady-state isotope transient kinetic analysis of N adsorption measured simultaneously with mass spectrometry is also demonstrated. In the experiment, the gas flow through a plugged-flow gas-solid contactor is switched between N215 and N214 isotopes at a temperature of 300 K and a constant pressure of 1 atm; the gas flow and mass spectrum are correlated with the structure factor determined from event-based neutron total scattering. Available flow conditions, sample considerations, and future applications are discussed.

No abstract