Thermally stable surfactant-free ceria nanocubes in silica aerogel

Francesco Caddeo, Alberto Casu, Danilo Loche, Lucy M. Morgan, Gavin Mountjoy, Colm O'Regan, Maria F. Casula, Shusaku Hayama, Anna Corrias, Andrea Falqui

Research output: Contribution to journalArticlepeer-review

3 Scopus citations


Surfactant-mediated chemical routes allow one to synthesize highly engineered shape- and size-controlled nanocrystals. However, the occurrence of capping agents on the surface of the nanocrystals is undesirable for selected applications. Here, a novel approach to the production of shape-controlled nanocrystals which exhibit high thermal stability is demonstrated. Ceria nanocubes obtained by surfactant-mediated synthesis are embedded inside a highly porous silica aerogel and thermally treated to remove the capping agent. Powder X-ray Diffraction and Scanning Transmission Electron Microscopy show the homogeneous dispersion of the nanocubes within the aerogel matrix. Remarkably, both the size and the shape of the ceria nanocubes are retained not only throughout the aerogel syntheses but also upon thermal treatments up to 900 °C, while avoiding their agglomeration. The reactivity of ceria is measured by in situ High-Energy Resolution Fluorescence Detected - X-ray Absorption Near Edge Spectroscopy at the Ce L3 edge, and shows the reversibility of redox cycles of ceria nanocubes when they are embedded in the aerogel. This demonstrates that the enhanced reactivity due to their prominent {1 0 0} crystal facets is preserved. In contrast, unsupported ceria nanocubes begin to agglomerate as soon as the capping agent decomposes, leading to a degradation of their reactivity already at 275 °C.
Original languageEnglish (US)
Pages (from-to)376-384
Number of pages9
JournalJournal of Colloid and Interface Science
StatePublished - Sep 22 2020

Bibliographical note

KAUST Repository Item: Exported on 2020-10-12
Acknowledgements: This work was supported by the British Council UK-Gulf Institutional Links grant (279183790) and by the Engineering and Physical Sciences Research Council (EPSRC) grants (EP/K50306X/1 and EP/1641783). The authors also wish to thank the Diamond Light Source for the award of beam time SP19013. The graphical abstract was produced by Heno Hwang, scientific illustrator at KAUST, who is gratefully acknowledged.


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