Experimental arrangements suitable for the acquisition of inelastic neutron scattering spectra of heterogeneous catalysts

Rev Sci Instrum. 2011 Mar;82(3):034101. doi: 10.1063/1.3553295.

Abstract

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.