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Title: Transmission in situ and operando high temperature X-ray powder diffraction in variable gaseous environments

Journal Article · · Review of Scientific Instruments
DOI:https://doi.org/10.1063/1.5001695· OSTI ID:1465703
ORCiD logo [1]; ORCiD logo [2];  [1];  [1];  [1];  [3];  [1]
  1. Technische Universität Berlin (Germany). Fachgebiet Keramische Werkstoffe / Chair of Advanced Ceramic Materials, Institut für Werkstoffwissenschaften- und Technologien
  2. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS)
  3. University of Innsbruck (Austria). Institute of Physical Chemistry

In this paper, we describe a device for time-resolved synchrotron-based in situ and operando X-ray powder diffraction measurements at elevated temperatures under controllable gaseous environments. The respective gaseous sample environment is realized via a gas-tight capillary-in-capillary design, where the gas flow is achieved through an open-end 0.5 mm capillary located inside a 0.7 mm capillary filled with a sample powder. Thermal mass flow controllers provide appropriate gas flows and computer-controlled on-the-fly gas mixing capabilities. The capillary system is centered inside an infrared heated, proportional integral differential-controlled capillary furnace allowing access to temperatures up to 1000 °C.

Research Organization:
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Sponsoring Organization:
USDOE Office of Science (SC)
Grant/Contract Number:
AC02-05CH11231
OSTI ID:
1465703
Journal Information:
Review of Scientific Instruments, Vol. 89, Issue 3; Related Information: © 2018 Author(s).; ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)Copyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 24 works
Citation information provided by
Web of Science

References (13)

Versatile in situ powder X-ray diffraction cells for solid–gas investigations journal October 2010
Back Cover: Formation of Intermetallic Compounds by Reactive Metal-Support Interaction: A Frequently Encountered Phenomenon in Catalysis (ChemCatChem 3/2015) journal February 2015
Compact low power infrared tube furnace for in situ X-ray powder diffraction journal January 2017
Absorption and Release of Carbon Dioxide with Various Metal Oxides and Hydroxides journal January 2007
Pressure acid leaching of nickel laterite ores: an in situ diffraction study of the mechanism and rate of reaction journal November 2005
Surface chemistry of pure tetragonal ZrO 2 and gas-phase dependence of the tetragonal-to-monoclinic ZrO 2 transformation journal January 2017
Iron Exsolution Phenomena in Lanthanum Strontium Ferrite SOFC Anodes journal May 2017
The Oxford-Diamond In Situ Cell for studying chemical reactions using time-resolved X-ray diffraction journal August 2012
Anion-mediated negative thermal expansion in lanthanum hexaboride journal October 2017
2D-Mapping of the Catalyst Structure Inside a Catalytic Microreactor at Work:  Partial Oxidation of Methane over Rh/Al 2 O 3 journal May 2006
Surface chemistry and stability of metastable corundum-type In 2 O 3 journal January 2017
Exsolution of Fe and SrO Nanorods and Nanoparticles from Lanthanum Strontium Ferrite La 0.6 Sr 0.4 FeO 3−δ Materials by Hydrogen Reduction journal September 2015
A Single‐Source Precursor Approach to Self‐Supported Nickel–Manganese‐Based Catalysts with Improved Stability for Effective Low‐Temperature Dry Reforming of Methane journal February 2016

Cited By (3)

On the structural stability of crystalline ceria phases in undoped and acceptor-doped ceria materials under in situ reduction conditions journal January 2019
Crystallographic and electronic evolution of lanthanum strontium ferrite (La 0.6 Sr 0.4 FeO 3−δ ) thin film and bulk model systems during iron exsolution journal January 2019
Reactive metal-support interaction in the Cu-In 2 O 3 system: intermetallic compound formation and its consequences for CO 2 -selective methanol steam reforming journal April 2019

Figures / Tables (5)


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