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Related Concept Videos

Heterogeneous Catalysis01:22

Heterogeneous Catalysis

138
Heterogeneous catalysis involves a catalyst in a different phase from the reactants. It is a process where the catalyst and the reactants are in distinct phases, typically solid and gas or liquid.Most heterogeneous catalysts are metals, metal oxides, or acids. The list includes transition metals like iron (Fe), cobalt (Co), nickel (Ni), palladium (Pd), platinum (Pt), chromium (Cr), manganese (Mn), tungsten (W), silver (Ag), and copper (Cu). These metals possess partially vacant d orbitals that...
138

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In-situ X-ray diffraction activation study on an Fe/TiO2 pre-catalyst.

Matthew K Rayner1, David G Billing2, Neil J Coville1

  • 1DST/NRF Centre of Excellence in Catalysis and Molecular Science Institute, School of Chemistry, University of the Witwatersrand, Private Bag 3, PO Wits, 2050, South Africa.

Acta Crystallographica Section B, Structural Science, Crystal Engineering and Materials
|June 4, 2014
PubMed
Summary

This study used in situ powder X-ray diffraction (PXRD) to track iron on titania (Fe/TiO2) catalysts during oxidation and reduction. Optimal calcination at 450°C yields maximum hematite, while reduction conditions dictate iron oxide and metallic iron formation.

Keywords:
Rietveld analysisX-ray diffractionactivationcalcinationilmenitenon-ambient crystallographypseudobrookitetitania

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Area of Science:

  • Materials Science
  • Catalysis
  • Solid-State Chemistry

Background:

  • Titania-supported iron catalysts are crucial in various chemical processes.
  • Understanding structural transformations during catalyst preparation is key to performance.
  • Phase evolution of iron oxides on titania influences catalytic activity.

Purpose of the Study:

  • To monitor structural changes of 10% Fe/TiO2 pre-catalyst during calcination and activation using in situ powder X-ray diffraction (PXRD).
  • To determine optimal calcination conditions for maximizing hematite formation.
  • To investigate the effect of reduction atmospheres on the catalyst's phase composition.

Main Methods:

  • In situ powder X-ray diffraction (PXRD) with Rietveld quantitative phase analysis.
  • Controlled calcination (oxidation) experiments in the temperature range of 25-900°C.
  • In situ reduction experiments using varying hydrogen (H2) concentrations (5%, 10%, 100%) in nitrogen (N2).

Main Results:

  • Calcination at 450°C maximizes hematite concentration and yields optimal particle size.
  • Iron addition increases the temperature for the anatase to rutile phase transformation in TiO2.
  • Reduction with low H2 concentrations forms ilmenite (FeTiO3), consuming both anatase and rutile.
  • High H2 concentrations lead to magnetite (Fe3O4) and metallic iron (Fe(0)) formation.
  • Reducing atmospheres decrease the anatase to rutile transformation temperature.

Conclusions:

  • Optimal calcination temperature for 10% Fe/TiO2 pre-catalyst is 450°C, yielding maximum hematite.
  • The presence of iron influences TiO2 phase transformations and facilitates pseudobrookite formation.
  • Catalyst reduction pathways are dependent on hydrogen concentration, forming different iron oxide or metallic phases.
  • Pre-reduction calcination temperature impacts the ease of iron reduction, suggesting process optimization is possible.