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Revisiting the thermal decomposition of layered γ-titanium phosphate and structural elucidation of Its intermediate phases

Author:
García-Granda, SantiagoUniovi authority; Khaynakov, SergiyUniovi authority; Espina Álvarez, María AránzazuUniovi authority; García Menéndez, José RubénUniovi authority; Castro Castro, Germán Rafael; Rocha, João Carlos Matias Celestino Gomes da; Mafra, Luís Miguel Monteiro
Publication date:
2010
Publisher version:
http://dx.doi.org/10.1021/ic901254j
Citación:
Inorganic Chemistry, 49(6), p. 2630-2638 (2010); doi:10.1021/ic901254j
Descripción física:
p. 2630-2638
Abstract:

The thermal transformations of γ-titanium phosphate, Ti(PO4)(H2PO4)·2H2O, have been studied by thermal analyses (thermogravimetry (TG) and differential thermal analysis (DTA)) and variable-temperature 31P magic-angle spinning (MAS)/CPMAS and 2D 31P−31P spin-exchange NMR. The structure of this material has been refined from synchrotron powder X-ray diffraction data (monoclinic, P21, a = 5.1811(2) Å, b = 6.3479(2) Å, c = 23.725(2) Å, β = 102.57(1)°). Vyazovkin’s model-free kinetic algorithms have been applied to determine the apparent activation energy to both dehydration and dehydroxylation of γ-titanium phosphate. In these processes, several overlapped steps have been detected. Structural models for Ti(PO4)(H2PO4)·H2O and Ti(PO4)(H2P2O7)0.5 intermediate layered phases have been proposed.

The thermal transformations of γ-titanium phosphate, Ti(PO4)(H2PO4)·2H2O, have been studied by thermal analyses (thermogravimetry (TG) and differential thermal analysis (DTA)) and variable-temperature 31P magic-angle spinning (MAS)/CPMAS and 2D 31P−31P spin-exchange NMR. The structure of this material has been refined from synchrotron powder X-ray diffraction data (monoclinic, P21, a = 5.1811(2) Å, b = 6.3479(2) Å, c = 23.725(2) Å, β = 102.57(1)°). Vyazovkin’s model-free kinetic algorithms have been applied to determine the apparent activation energy to both dehydration and dehydroxylation of γ-titanium phosphate. In these processes, several overlapped steps have been detected. Structural models for Ti(PO4)(H2PO4)·H2O and Ti(PO4)(H2P2O7)0.5 intermediate layered phases have been proposed.

URI:
http://hdl.handle.net/10651/7945
ISSN:
0020-1669
Identificador local:

20100130

DOI:
10.1021/ic901254j
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