Inelastic neutron scattering (INS) is increasingly being used for the characterization of heterogeneous catalysts. As the technique is uniquely sensitive to hydrogen atoms, vibrational spectra can be obtained that emphasize a hydrogenous component or hydrogen-containing moieties adsorbed on to an inorganic support. However, due to sensitivity constraints, the technique typically requires large sample masses (∼10 g catalyst). A reaction system is hereby described that enables suitable quantities of heterogeneous catalysts to be appropriately activated and operated under steady-state conditions for extended periods of time prior to acquisition of the INS spectrum. In addition to ex situ studies, a cell is described which negates the need for a sample transfer stage between reaction testing and INS measurement. This cell can operate up to temperatures of 823 K and pressures up to 20 bar. The apparatus is also amenable to adsorption experiments at the gas-solid interface.
The archetype cubic chiral magnet MnSi is home to some of the most fascinating states in condensed matter such as skyrmions and a non-Fermi liquid behavior in conjunction with a topological Hall effect under hydrostatic pressure. Using small angle neutron scattering, we study the evolution of the helimagnetic, conical and skyrmionic correlations with increasing hydrostatic pressure. We show that the helical propagation vector smoothly reorients from 111 to 100 at intermediate pressures. At higher pressures, above the critical pressure, the long-range helimagnetic order disappears at zero magnetic field. Nevertheless, skyrmion lattices and conical spirals form under magnetic fields, in a part of the phase diagram where a topological Hall effect and a non-Fermi liquid behavior have been reported. These unexpected results shed light on the puzzling behavior of MnSi at high pressures and the mechanisms that destabilize the helimagnetic long-range order at the critical pressure.
An in situ cell that allows the electrical resistance of a sample pellet to be measured while performing neutron diffraction experiments has been developed at the ISIS pulsed neutron source. The sample is held between two spring loaded platinum electrodes embedded in a boron nitride clamp assembly with the resistance measured using the four-probe method. An outer quartz glass jacket allows the atmosphere within the sample enclosure to be controlled, and the entire device can be accommodated within a standard ISIS neutron furnace for measurements at temperatures up to 1270 K. The operation of this cell is illustrated using data for the structural, magnetic, and electrical properties of chalcopyrite CuFeS(2) collected over the temperature range of 398-873 K on the Polaris powder diffractometer at ISIS.
Abstract. A flow-through quartz gas cell, together with a gas flow control and monitoring system, has been designed and constructed at ISIS. This equipment allows neutron powder diffraction data to be collected on samples at temperatures up to around 1300 K when exposed to user chosen mixtures of O 2 , Ar, CO 2 , and CO. By exploiting the sensitivity of neutrons to the presence of light atoms such as oxygen, it is possible to probe the crystal structure of oxide materials as a function of oxygen partial pressures down to log
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