Air-heated solid–gas reaction setup for in situ neutron powder diffraction

Jakob Voldum Ahlburg, Emmanuel Canévet, Mogens Christensen*

*Corresponding author for this work

Research output: Contribution to journalJournal articleResearchpeer-review

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Abstract

The design and function of a reduction furnace, specially designed for solid–gas in situ monochromatic angular dispersive neutron powder diffraction, is presented. The functionality is demonstrated by performing a reduction experiment of CoFe2O4 nanoparticles at the instrument DMC at SINQ. Heating is provided by an air gun, allowing the sample to reach temperatures in the range of 300–973 K within less than 5 min. The setup is based on a single-crystal sapphire tube with one end closed. A ϕ scan of the tube reveals its single-crystal nature, through strong single-crystal reflections, while the remaining background is very low, uniform and flat. CoFe2O4 was reduced using a time resolution of 8 min and a sample volume of ∼2 cm3. By means of sequential Rietveld refinement of the in situ neutron diffraction data, a two-step reduction mechanism was discovered: CoFe2O4 → Co0.33Fe0.67O → CoFe2. The setup offers high temperatures, fast temperature stability, large sample volumes and respectable time resolution. The setup has proven to be ideal to carry out investigations of advanced materials under realistic conditions. The ability to investigate real materials in real time under realistic conditions may be a significant advantage for scientific investigations as well as for industrial applications.

Original languageEnglish
JournalJournal of Applied Crystallography
Volume52
Issue number4
Pages (from-to)761-768
Number of pages8
ISSN0021-8898
DOIs
Publication statusPublished - 2019

Keywords

  • Exchange-spring magnets
  • In situ
  • Neutron powder diffraction
  • Single-crystal sapphire
  • Solid–gas reactions

Cite this

Ahlburg, Jakob Voldum ; Canévet, Emmanuel ; Christensen, Mogens. / Air-heated solid–gas reaction setup for in situ neutron powder diffraction. In: Journal of Applied Crystallography. 2019 ; Vol. 52, No. 4. pp. 761-768.
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abstract = "The design and function of a reduction furnace, specially designed for solid–gas in situ monochromatic angular dispersive neutron powder diffraction, is presented. The functionality is demonstrated by performing a reduction experiment of CoFe2O4 nanoparticles at the instrument DMC at SINQ. Heating is provided by an air gun, allowing the sample to reach temperatures in the range of 300–973 K within less than 5 min. The setup is based on a single-crystal sapphire tube with one end closed. A ϕ scan of the tube reveals its single-crystal nature, through strong single-crystal reflections, while the remaining background is very low, uniform and flat. CoFe2O4 was reduced using a time resolution of 8 min and a sample volume of ∼2 cm3. By means of sequential Rietveld refinement of the in situ neutron diffraction data, a two-step reduction mechanism was discovered: CoFe2O4 → Co0.33Fe0.67O → CoFe2. The setup offers high temperatures, fast temperature stability, large sample volumes and respectable time resolution. The setup has proven to be ideal to carry out investigations of advanced materials under realistic conditions. The ability to investigate real materials in real time under realistic conditions may be a significant advantage for scientific investigations as well as for industrial applications.",
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Air-heated solid–gas reaction setup for in situ neutron powder diffraction. / Ahlburg, Jakob Voldum; Canévet, Emmanuel; Christensen, Mogens.

In: Journal of Applied Crystallography, Vol. 52, No. 4, 2019, p. 761-768.

Research output: Contribution to journalJournal articleResearchpeer-review

TY - JOUR

T1 - Air-heated solid–gas reaction setup for in situ neutron powder diffraction

AU - Ahlburg, Jakob Voldum

AU - Canévet, Emmanuel

AU - Christensen, Mogens

PY - 2019

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N2 - The design and function of a reduction furnace, specially designed for solid–gas in situ monochromatic angular dispersive neutron powder diffraction, is presented. The functionality is demonstrated by performing a reduction experiment of CoFe2O4 nanoparticles at the instrument DMC at SINQ. Heating is provided by an air gun, allowing the sample to reach temperatures in the range of 300–973 K within less than 5 min. The setup is based on a single-crystal sapphire tube with one end closed. A ϕ scan of the tube reveals its single-crystal nature, through strong single-crystal reflections, while the remaining background is very low, uniform and flat. CoFe2O4 was reduced using a time resolution of 8 min and a sample volume of ∼2 cm3. By means of sequential Rietveld refinement of the in situ neutron diffraction data, a two-step reduction mechanism was discovered: CoFe2O4 → Co0.33Fe0.67O → CoFe2. The setup offers high temperatures, fast temperature stability, large sample volumes and respectable time resolution. The setup has proven to be ideal to carry out investigations of advanced materials under realistic conditions. The ability to investigate real materials in real time under realistic conditions may be a significant advantage for scientific investigations as well as for industrial applications.

AB - The design and function of a reduction furnace, specially designed for solid–gas in situ monochromatic angular dispersive neutron powder diffraction, is presented. The functionality is demonstrated by performing a reduction experiment of CoFe2O4 nanoparticles at the instrument DMC at SINQ. Heating is provided by an air gun, allowing the sample to reach temperatures in the range of 300–973 K within less than 5 min. The setup is based on a single-crystal sapphire tube with one end closed. A ϕ scan of the tube reveals its single-crystal nature, through strong single-crystal reflections, while the remaining background is very low, uniform and flat. CoFe2O4 was reduced using a time resolution of 8 min and a sample volume of ∼2 cm3. By means of sequential Rietveld refinement of the in situ neutron diffraction data, a two-step reduction mechanism was discovered: CoFe2O4 → Co0.33Fe0.67O → CoFe2. The setup offers high temperatures, fast temperature stability, large sample volumes and respectable time resolution. The setup has proven to be ideal to carry out investigations of advanced materials under realistic conditions. The ability to investigate real materials in real time under realistic conditions may be a significant advantage for scientific investigations as well as for industrial applications.

KW - Exchange-spring magnets

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KW - Single-crystal sapphire

KW - Solid–gas reactions

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