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Application of magic-angle spinning NMR to examine the nature of protons in titanate nanotubes

Application of magic-angle spinning NMR to examine the nature of protons in titanate nanotubes
Application of magic-angle spinning NMR to examine the nature of protons in titanate nanotubes
Systematic MAS 1H-NMR studies of protonated titanate nanotubes (produced by alkaline hydrothermal treatment of TiO2 with NaOH) have revealed that there are several types of protons incorporated into their wall structure, including crystallographic water molecules and ion-exchangeable OH groups.

Each type (a) has a characteristic chemical shift and (b) disappears at a different rate during annealing in air. The evolution of protons in titanate nanotubes during crystallographic and morphological transformation in the sequence H2Ti3O7•xH2O, H2Ti3O7, H2Ti6O13, TiO2(B), TiO2(anatase) during calcination, at temperatures from 140 ºC to 500 ºC, has been studied using MAS NMR and Raman spectroscopies together with TGA, XRD and TEM techniques. The irreversible disappearance of ion-exchangeable OH groups has been observed, even under low temperature treatment.
dehydration, titanate, hydrogen, nanotubes, titania
0002-7863
2458-2465
Bavykin, Dmitry V.
1e9fabfc-d078-4585-876f-85ff33b7eed5
Carravetta, Marina
1b12fa96-4a6a-4689-ab3b-ccc68f1d7691
Kulak, Alexander N.
7dc57b4f-aae0-42a4-ae15-fd50ab6521c2
Walsh, Frank C.
309528e7-062e-439b-af40-9309bc91efb2
Bavykin, Dmitry V.
1e9fabfc-d078-4585-876f-85ff33b7eed5
Carravetta, Marina
1b12fa96-4a6a-4689-ab3b-ccc68f1d7691
Kulak, Alexander N.
7dc57b4f-aae0-42a4-ae15-fd50ab6521c2
Walsh, Frank C.
309528e7-062e-439b-af40-9309bc91efb2

Bavykin, Dmitry V., Carravetta, Marina, Kulak, Alexander N. and Walsh, Frank C. (2010) Application of magic-angle spinning NMR to examine the nature of protons in titanate nanotubes. Journal of the American Chemical Society, 22 (8), 2458-2465.

Record type: Article

Abstract

Systematic MAS 1H-NMR studies of protonated titanate nanotubes (produced by alkaline hydrothermal treatment of TiO2 with NaOH) have revealed that there are several types of protons incorporated into their wall structure, including crystallographic water molecules and ion-exchangeable OH groups.

Each type (a) has a characteristic chemical shift and (b) disappears at a different rate during annealing in air. The evolution of protons in titanate nanotubes during crystallographic and morphological transformation in the sequence H2Ti3O7•xH2O, H2Ti3O7, H2Ti6O13, TiO2(B), TiO2(anatase) during calcination, at temperatures from 140 ºC to 500 ºC, has been studied using MAS NMR and Raman spectroscopies together with TGA, XRD and TEM techniques. The irreversible disappearance of ion-exchangeable OH groups has been observed, even under low temperature treatment.

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More information

Published date: 23 March 2010
Keywords: dehydration, titanate, hydrogen, nanotubes, titania
Organisations: Engineering Mats & Surface Engineerg Gp

Identifiers

Local EPrints ID: 146195
URI: https://eprints.soton.ac.uk/id/eprint/146195
ISSN: 0002-7863
PURE UUID: 346974e0-8b0c-4cdc-9998-90b6c1271e32
ORCID for Marina Carravetta: ORCID iD orcid.org/0000-0002-6296-2104

Catalogue record

Date deposited: 21 Apr 2010 08:05
Last modified: 14 Jul 2018 00:34

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