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

Journal Article · · Review of Scientific Instruments
DOI:https://doi.org/10.1063/1.5031432· OSTI ID:1493150

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.

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
OSTI ID:
1493150
Alternate ID(s):
OSTI ID: 1471796
Journal Information:
Review of Scientific Instruments, Vol. 89, Issue 9; ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)Copyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 7 works
Citation information provided by
Web of Science

References (8)

Versatile in situ powder X-ray diffraction cells for solid–gas investigations journal October 2010
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
In-Situ Time Resolved Synchrotron Powder Diffraction Studies of Syntheses and Chemical Reactions journal July 1996
Visualizing oxygen anion transport pathways in NdBaCo2O5+δ by in situ neutron diffraction journal January 2013
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

Figures / Tables (9)


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