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
Authors | Middelkoop, V, Tighe, CJ, Kellici, S, Gruar, RI, Perkins, JM, Jacques, SDM, Barnes, P and Darr, JA |
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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. |
Year | 2014 |
Journal | Journal of Supercritical Fluids |
Journal citation | 87, pp. 118 - 128 |
Publisher | Elsevier |
ISSN | 0896-8446 |
Digital Object Identifier (DOI) | https://doi.org/10.1016/j.supflu.2013.12.022 |
Publication dates | |
06 Jan 2014 | |
Publication process dates | |
Deposited | 08 Jun 2017 |
Accepted | 27 Dec 2013 |
Accepted author manuscript | License File Access Level Open |
Supplemental file | License File Access Level Open |
https://openresearch.lsbu.ac.uk/item/8788q
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Accepted author manuscript
Middlekoop-et-al_2014.docx | ||
License: CC BY-NC-ND 4.0 | ||
File access level: Open |
Supplemental file
mmc1.docx | ||
License: CC BY 4.0 | ||
File access level: Open |
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