Imaging the continuous hydrothermal flow synthesis of nanoparticulate CeO2 at different supercritical water temperatures using in situ angle-dispersive diffraction

Journal article


Middelkoop, V, Tighe, CJ, Kellici, S, Gruar, RI, Perkins, JM, Jacques, SDM, Barnes, P and Darr, JA (2014). Imaging the continuous hydrothermal flow synthesis of nanoparticulate CeO2 at different supercritical water temperatures using in situ angle-dispersive diffraction. Journal of Supercritical Fluids. 87, pp. 118 - 128. https://doi.org/10.1016/j.supflu.2013.12.022
AuthorsMiddelkoop, V, Tighe, CJ, Kellici, S, Gruar, RI, Perkins, JM, Jacques, SDM, Barnes, P and Darr, JA
Abstract

In situ high-energy synchrotron X-ray diffraction, a non-destructive synchrotron-based technique was employed to probe inside the steel tubing of a continuous hydrothermal flow synthesis (CHFS) mixer to spatially map, for the first time, the superheated water crystallisation of nanocrystalline ceria (CeO2) at three different (superheated-water) temperatures representing three unique chemical environments within the reactor. Rapid hydrothermal co-precipitation at the three selected temperatures led to similarly sized ceria nanoparticles ranging from 3 to 7 nm. 2D maps of CeO 2 formation were constructed from the intensity and corresponding full width at half maximum (FWHM) values of the two most intense ceria reflections (111) and (002) for all three water inlet temperatures (350, 400 and 450 C at 24 MPa) and subsequent changes in the particle size distribution were analysed. The accompanying high-resolution transmission electron microscopy (HRTEM) and tomographic particle size maps have confirmed that the mean ceria particle size slightly increases with temperature. This X-ray tomographic imaging study amounted to a formidable technical and engineering challenge, nevertheless one that has been met; this represents a significant achievement in imaging science, given the dynamic nature and hostile environment of a working CHFS reactor. © 2014 Elsevier B.V.

Year2014
JournalJournal of Supercritical Fluids
Journal citation87, pp. 118 - 128
PublisherElsevier
ISSN0896-8446
Digital Object Identifier (DOI)https://doi.org/10.1016/j.supflu.2013.12.022
Publication dates
Print06 Jan 2014
Publication process dates
Deposited08 Jun 2017
Accepted27 Dec 2013
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