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

Jakob Voldum Ahlburg, Emmanuel Canevet, Mogens Christensen*

*Corresponding author for this work

Research output: Contribution to journal/Conference contribution in journal/Contribution to newspaperJournal articleResearchpeer-review


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 300-973K within less than 5min. The setup is based on a single-crystal sapphire tube with one end closed. A phi 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 8min and a sample volume of similar to 2cm(3). 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
Pages (from-to)761-768
Number of pages8
Publication statusPublished - Aug 2019


  • in situ
  • neutron powder diffraction
  • solid-gas reactions
  • single-crystal sapphire
  • exchange-spring magnets
  • CELL


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