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Evolution in the structure of akaganeite and hematite during hydrothermal growth: an in situ synchrotron X-ray diffraction analysis

Published online by Cambridge University Press:  10 September 2018

Kristina M. Peterson ,
Peter J. Heaney  and
Jeffrey E. Post
Kristina M. Peterson*
Affiliation:
Lyell Centre, Heriot Watt University, Edinburgh, UK
Peter J. Heaney
Affiliation:
Department of Geosciences, Pennsylvania State University, University Park, Pennsylvania 16802
Jeffrey E. Post
Affiliation:
Department of Mineral Sciences, Smithsonian Institution, Washington, District of Columbia 20560-0119
*
a)Author to whom correspondence should be addressed. Electronic mail: k.peterson@hw.ac.uk
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Abstract

Synchrotron X-ray diffraction was used to monitor the hydrothermal precipitation of akaganeite (β-FeOOH) and its transformation to hematite (Fe2O3) in situ. Akaganeite was the first phase to form and hematite was the final phase in our experiments with temperatures between 150 and 200 °C. Akaganeite was the only phase that formed at 100 °C. Rietveld analyses revealed that the akaganeite unit-cell volume contracted until the onset of dissolution, and subsequently expanded. This reversal at the onset of dissolution was associated with a substantial and rapid increase in occupancy of the Cl site, perhaps by OH− or Fe3+. Rietveld analyses supported the incipient formation of an OH-rich, Fe-deficient hematite phase in experiments between 150 and 200 °C. The inferred H concentrations of the first crystals were consistent with “hydrohematite.” With continued crystal growth, the Fe occupancies increased. Contraction in both a- and c-axes signaled the loss of hydroxyl groups and formation of a nearly stoichiometric hematite.

Keywords

TR-XRDakaganeitehematitehydrohematitehydrothermalRietveld refinements
Type
Technical Article
Information
Powder Diffraction , Volume 33 , Issue 4 , December 2018 , pp. 287 - 297
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Copyright
Copyright © International Centre for Diffraction Data 2018 

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