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Solid state NMR and X-ray studies of the structural evolution of nanocrystalline zirconia

Chadwick, Alan V., Strange, John H., Mountjoy, Gavin, Tucker, M.G., Smith, Mark E., Nield, V.M., Poplett, I.J.F. (2001) Solid state NMR and X-ray studies of the structural evolution of nanocrystalline zirconia. Chemistry of Materials, 13 (4). pp. 1219-1229. ISSN 0897-4756. (doi:10.1021/cm001152w) (Access to this publication is currently restricted. You may be able to access a copy if URLs are provided) (KAR id:9398)

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Abstract

A combination of X-ray techniques [diffraction and Zr K-edge absorption (EXAFS and XANES)] and multinuclear (H-1, C-13, O-17) solid-state NMR spectroscopy is employed to follow in detail the structural development of nanocrystalline zirconia. O-17 magic-angle spinning NMR spectroscopy of sol-gel produced undoped ZrO2 shows unequivocally that oxygen sites in the initial gel are monoclinic-like. This result is consistent with X-ray absorption measurements, which also suggest that the structures of the initial amorphous phases of doped and undoped samples produced by the hydroxide-precipitation and sol-gel methods are very similar. On crystallization, the local structure of the crystalline component is tetragonal, but a significant fraction of the sample remains disordered. Heating to higher temperatures results in conversion to monoclinic zirconia in undoped samples at room temperature. For sol-gel-produced ZrO2, C-13 NMR shows that loss of all of the organic fragments occurs prior to crystallization. The H-1 NMR experiments determined that the proton content remains significant until well above the crystallization temperature, so that the composition is not accurately described as ZrO2 until > 500 degreesC.

Item Type: Article
DOI/Identification number: 10.1021/cm001152w
Subjects: Q Science
Divisions: Divisions > Division of Natural Sciences > Physics and Astronomy
Depositing User: Alan Chadwick
Date Deposited: 09 Oct 2008 14:33 UTC
Last Modified: 16 Nov 2021 09:47 UTC
Resource URI: https://kar.kent.ac.uk/id/eprint/9398 (The current URI for this page, for reference purposes)

University of Kent Author Information

Chadwick, Alan V..

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Strange, John H..

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Mountjoy, Gavin.

Creator's ORCID: https://orcid.org/0000-0002-6495-2006
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