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Disordered lithium niobate rock-salt materials prepared by hydrothermal synthesis
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Modeshia, Deena R., Walton, Richard I., Mitchell, Martin R. and Ashbrook, Sharon E. (2010) Disordered lithium niobate rock-salt materials prepared by hydrothermal synthesis. Dalton Transactions, Vol.39 (No.26). pp. 6031-6036. doi:10.1039/c002190c ISSN 1477-9226.
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Official URL: http://dx.doi.org/10.1039/c002190c
Abstract
An investigation of the one-step hydrothermal crystallisation of lithium niobates reveals that reaction between Nb2O5 and aqueous LiOH at 240 degrees C yields materials with a disordered rock-salt structure where the metals are statistically distributed over the cation sites. This contrasts with the well-studied reaction between Nb2O5 and NaOH or KOH that produces ANbO(3) (A = Na, K) perovskites. Powder neutron diffraction shows that materials prepared at short reaction times and lower LiOH concentration (2.5 M) are lithium deficient and have a slight excess of niobium, but that at longer periods of reaction in 5 M LiOH, close to the ideal, stoichiometric Li0.75Nb0.25O composition is produced. Upon annealing this phase cleanly transforms into the known ordered rock-salt material Li3NbO4, a process we have followed using thermodiffractometry, which indicates that transformation begins at similar to 700 degrees C. Solid-state Nb-93 and Li-7 NMR of the disordered and ordered rock-salt phases shows that both contain single metal sites but there is clear evidence for local disorder in the disordered samples. For the ordered material, NMR parameters derived from experiment are also compared to those calculated using density functional theory and are shown to be in good agreement.
Item Type: | Journal Article | ||||
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Subjects: | Q Science > QD Chemistry | ||||
Divisions: | Faculty of Science, Engineering and Medicine > Science > Chemistry | ||||
Library of Congress Subject Headings (LCSH): | Lithium niobate, Thermochemistry, Crystallization, Crystal growth, Transition metal oxides -- Synthesis | ||||
Journal or Publication Title: | Dalton Transactions | ||||
Publisher: | Royal Society of Chemistry | ||||
ISSN: | 1477-9226 | ||||
Official Date: | 2010 | ||||
Dates: |
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Volume: | Vol.39 | ||||
Number: | No.26 | ||||
Number of Pages: | 6 | ||||
Page Range: | pp. 6031-6036 | ||||
DOI: | 10.1039/c002190c | ||||
Status: | Peer Reviewed | ||||
Publication Status: | Published | ||||
Funder: | Engineering and Physical Sciences Research Council (EPSRC) | ||||
Grant number: | EP/E041825 (EPSRC) |
Data sourced from Thomson Reuters' Web of Knowledge
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