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Title: AGES: Automated Gas Environment System for in situ neutron powder diffraction

Abstract

High fluxes available at modern neutron and synchrotron sources have opened up a wide variety of in situ and operando studies of real processes using scattering techniques. This has allowed the user community to follow chemistry in the beam, which often requires high temperatures, gas flow, etc. In this paper, we describe an integrated gas handling system for the general-purpose powder diffraction beamline Powgen at the Spallation Neutron Source. The Automated Gas Environment System (AGES) allows control of both gas flow and temperature (room temperature to 850 °C), while measuring the partial pressure of oxygen and following the effluent gas by mass spectrometry, concurrent with neutron powder diffraction, in order to follow the structural evolution of materials under these conditions. The versatility of AGES is illustrated by two examples of experiments conducted with the system. In solid oxide fuel cell electrode materials, oxygen transport pathways in double perovskites PrBaCo2O5+δ and NdBaCo2O5+δ were elucidated by neutron diffraction measurements under atmosphere with oxygen partial pressures (pO2) of 10–1 to 10–4 (achieved using mixtures of nitrogen and oxygen) and temperatures from 575 to 850 °C. In another example, the potential oxygen storage material La1–xSrxFeO3 was measured under alternating flows of 15% CH4 inmore » N2 and air (20% O2 in N2) at temperatures from 135 to 835 °C. As a result, from the oxygen stoichiometry, the optimal composition for oxygen storage was determined.« less

Authors:
ORCiD logo [1]; ORCiD logo [1]; ORCiD logo [1]; ORCiD logo [1]
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  1. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Publication Date:
Research Org.:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
OSTI Identifier:
1493150
Alternate Identifier(s):
OSTI ID: 1471796
Grant/Contract Number:  
AC05-00OR22725
Resource Type:
Accepted Manuscript
Journal Name:
Review of Scientific Instruments
Additional Journal Information:
Journal Volume: 89; Journal Issue: 9; Journal ID: ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)
Country of Publication:
United States
Language:
English
Subject:
47 OTHER INSTRUMENTATION

Citation Formats

Kirkham, Melanie J., Heroux, Luke, Ruiz-Rodriguez, Mariano, and Huq, Ashfia. AGES: Automated Gas Environment System for in situ neutron powder diffraction. United States: N. p., 2018. Web. doi:10.1063/1.5031432.
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Kirkham, Melanie J., Heroux, Luke, Ruiz-Rodriguez, Mariano, & Huq, Ashfia. AGES: Automated Gas Environment System for in situ neutron powder diffraction. United States. https://doi.org/10.1063/1.5031432
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Kirkham, Melanie J., Heroux, Luke, Ruiz-Rodriguez, Mariano, and Huq, Ashfia. Fri . "AGES: Automated Gas Environment System for in situ neutron powder diffraction". United States. https://doi.org/10.1063/1.5031432. https://www.osti.gov/servlets/purl/1493150.
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@article{osti_1493150,
title = {AGES: Automated Gas Environment System for in situ neutron powder diffraction},
author = {Kirkham, Melanie J. and Heroux, Luke and Ruiz-Rodriguez, Mariano and Huq, Ashfia},
abstractNote = {High fluxes available at modern neutron and synchrotron sources have opened up a wide variety of in situ and operando studies of real processes using scattering techniques. This has allowed the user community to follow chemistry in the beam, which often requires high temperatures, gas flow, etc. In this paper, we describe an integrated gas handling system for the general-purpose powder diffraction beamline Powgen at the Spallation Neutron Source. The Automated Gas Environment System (AGES) allows control of both gas flow and temperature (room temperature to 850 °C), while measuring the partial pressure of oxygen and following the effluent gas by mass spectrometry, concurrent with neutron powder diffraction, in order to follow the structural evolution of materials under these conditions. The versatility of AGES is illustrated by two examples of experiments conducted with the system. In solid oxide fuel cell electrode materials, oxygen transport pathways in double perovskites PrBaCo2O5+δ and NdBaCo2O5+δ were elucidated by neutron diffraction measurements under atmosphere with oxygen partial pressures (pO2) of 10–1 to 10–4 (achieved using mixtures of nitrogen and oxygen) and temperatures from 575 to 850 °C. In another example, the potential oxygen storage material La1–xSrxFeO3 was measured under alternating flows of 15% CH4 in N2 and air (20% O2 in N2) at temperatures from 135 to 835 °C. As a result, from the oxygen stoichiometry, the optimal composition for oxygen storage was determined.},
doi = {10.1063/1.5031432},
journal = {Review of Scientific Instruments},
number = 9,
volume = 89,
place = {United States},
year = {Fri Sep 21 00:00:00 EDT 2018},
month = {Fri Sep 21 00:00:00 EDT 2018}
}
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Journal Article:
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Publisher's Version of Record
https://doi.org/10.1063/1.5031432
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Cited by: 7 works
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Figures / Tables:

Figure 1 Figure 1: Overview schematic of AGES Automated Gas Environment System.
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Works referenced in this record:

Versatile in situ powder X-ray diffraction cells for solid–gas investigations
journal, October 2010

  • Jensen, Torben R.; Nielsen, Thomas K.; Filinchuk, Yaroslav
  • Journal of Applied Crystallography, Vol. 43, Issue 6
  • DOI: 10.1107/s0021889810038148

An in-situ neutron diffraction study of the crystal structure of PrBaCo2O5+δ at high temperature and controlled oxygen partial pressure
journal, November 2013

On apparatus for studying catalysts and catalytic processes using neutron scattering
journal, May 1999

  • Turner, J. F. C.; Done, R.; Dreyer, J.
  • Review of Scientific Instruments, Vol. 70, Issue 5
  • DOI: 10.1063/1.1149758

Visualizing oxygen anion transport pathways in NdBaCo2O5+δ by in situ neutron diffraction
journal, January 2013

  • Cox-Galhotra, Rosemary A.; Huq, Ashfia; Hodges, Jason P.
  • Journal of Materials Chemistry A, Vol. 1, Issue 9
  • DOI: 10.1039/c3ta01308a

Unravelling the low thermal expansion coefficient of cation-substituted YBaCo4O7+δ
journal, March 2016

Oxygen Storage Properties of La 1– x Sr x FeO 3−δ for Chemical-Looping Reactions—An In Situ Neutron and Synchrotron X-ray Study
journal, May 2016

Hydrogen gas sample environment for TOSCA
journal, November 2014

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