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

Abstract

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.

Authors:
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
Publication Date:
Research Org.:
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Sponsoring Org.:
USDOE Office of Science (SC)
OSTI Identifier:
1465703
Grant/Contract Number:  
AC02-05CH11231
Resource Type:
Accepted Manuscript
Journal Name:
Review of Scientific Instruments
Additional Journal Information:
Journal Volume: 89; Journal Issue: 3; Related Information: © 2018 Author(s).; Journal ID: ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)
Country of Publication:
United States
Language:
English
Subject:
47 OTHER INSTRUMENTATION; 36 MATERIALS SCIENCE

Citation Formats

Schlicker, Lukas, Doran, Andrew, Schneppmüller, Peter, Gili, Albert, Czasny, Mathias, Penner, Simon, and Gurlo, Aleksander. Transmission in situ and operando high temperature X-ray powder diffraction in variable gaseous environments. United States: N. p., 2018. Web. doi:10.1063/1.5001695.
Schlicker, Lukas, Doran, Andrew, Schneppmüller, Peter, Gili, Albert, Czasny, Mathias, Penner, Simon, & Gurlo, Aleksander. Transmission in situ and operando high temperature X-ray powder diffraction in variable gaseous environments. United States. https://doi.org/10.1063/1.5001695
Schlicker, Lukas, Doran, Andrew, Schneppmüller, Peter, Gili, Albert, Czasny, Mathias, Penner, Simon, and Gurlo, Aleksander. Tue . "Transmission in situ and operando high temperature X-ray powder diffraction in variable gaseous environments". United States. https://doi.org/10.1063/1.5001695. https://www.osti.gov/servlets/purl/1465703.
@article{osti_1465703,
title = {Transmission in situ and operando high temperature X-ray powder diffraction in variable gaseous environments},
author = {Schlicker, Lukas and Doran, Andrew and Schneppmüller, Peter and Gili, Albert and Czasny, Mathias and Penner, Simon and Gurlo, Aleksander},
abstractNote = {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.},
doi = {10.1063/1.5001695},
journal = {Review of Scientific Instruments},
number = 3,
volume = 89,
place = {United States},
year = {Tue Mar 06 00:00:00 EST 2018},
month = {Tue Mar 06 00:00:00 EST 2018}
}

Journal Article:
Free Publicly Available Full Text
Publisher's Version of Record

Citation Metrics:
Cited by: 24 works
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Figures / Tables:

Figure 1 Figure 1: Flow chart of the experimental setup (a) and a photograph of the capillary-in-capillary gas-injection setup and capillary furnace as installed at the beamline (b).

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Works referenced in this record:

Versatile in situ powder X-ray diffraction cells for solid–gas investigations
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Absorption and Release of Carbon Dioxide with Various Metal Oxides and Hydroxides
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2D-Mapping of the Catalyst Structure Inside a Catalytic Microreactor at Work:  Partial Oxidation of Methane over Rh/Al 2 O 3
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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
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Works referencing / citing this record:

On the structural stability of crystalline ceria phases in undoped and acceptor-doped ceria materials under in situ reduction conditions
journal, January 2019

  • Bekheet, Maged F.; Grünbacher, Matthias; Schlicker, Lukas
  • CrystEngComm, Vol. 21, Issue 1
  • DOI: 10.1039/c8ce01726c

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

  • Götsch, Thomas; Köpfle, Norbert; Grünbacher, Matthias
  • Physical Chemistry Chemical Physics, Vol. 21, Issue 7
  • DOI: 10.1039/c8cp07743f

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

  • Ploner, Kevin; Schlicker, Lukas; Gili, Albert
  • Science and Technology of Advanced Materials, Vol. 20, Issue 1
  • DOI: 10.1080/14686996.2019.1590127

Figures/Tables have been extracted from DOE-funded journal article accepted manuscripts.