A high precision gas flow cell for performing in situ neutron studies of local atomic structure in catalytic materials

Olds, Daniel; Page, Katharine; Paecklar, Arnold A.; Peterson, Peter F.; Liu, Jue; Rucker, Gerald; Ruiz-Rodriguez, Mariano; Olsen, Michael; Pawel, Michelle; Overbury, Steven H.; Neilson, James R.

doi:10.1063/1.4978287

Title: A high precision gas flow cell for performing in situ neutron studies of local atomic structure in catalytic materials

Journal Article · Fri Mar 17 00:00:00 EDT 2017 · Review of Scientific Instruments

DOI:https://doi.org/10.1063/1.4978287· OSTI ID:1376356

^[1];

^[2];

^[1]; Liu, Jue ^[1]; Rucker, Gerald ^[1];

^[1];

^[2]; Pawel, Michelle ^[1]; Overbury, Steven H. ^[1]; Neilson, James R. ^[2]

Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Colorado State Univ., Fort Collins, CO (United States)

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 N₂ by Ca-exchanged zeolite-X (Na_78–2xCa_xAl₇₈Si₁₄₄O₃₈₄,x ≈ 38). We demonstrate sensitivities to lattice contraction and N₂ adsorption sites in the structure, with both static gas loading and gas flow. A steady-state isotope transient kinetic analysis of N₂ 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 ¹⁵N₂ and ¹⁴N₂ 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. As a result, available flow conditions, sample considerations, and future applications are discussed.

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Research Organization:: Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: AC05-00OR22725; LDRD Seed #7735

OSTI ID:: 1376356

Alternate ID(s):: OSTI ID: 1373971

Journal Information:: Review of Scientific Instruments, Vol. 88, Issue 3; ISSN 0034-6748

Publisher:: American Institute of Physics (AIP)Copyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 6 works

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