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Structural characterization of titanium-oxo-polymers synthesized in the presence of protons or complexing ligands as inhibitors

Structural characterization of titanium-oxo-polymers synthesized in the presence of protons or complexing ligands as inhibitors

Authors :
Clément Sanchez
François Ribot
P.-V. Bellot
Juliette Blanchard
Arlette Trokiner
Laboratoire de Chimie de la Matière Condensée de Paris (site Paris VI) (LCMCP (site Paris VI))
Université Pierre et Marie Curie - Paris 6 (UPMC)-Collège de France (CdF (institution))-Ecole Nationale Supérieure de Chimie de Paris - Chimie ParisTech-PSL (ENSCP)
Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)
Matériaux Hybrides et Nanomatériaux (LCMCP-MHN)
Laboratoire de Chimie de la Matière Condensée de Paris (LCMCP)
Institut de Chimie du CNRS (INC)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS)
Novel Advanced Nano-Objects (LCMCP-NANO)
Institut de Chimie du CNRS (INC)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS)-Laboratoire de Chimie de la Matière Condensée de Paris (LCMCP)
Institut de Chimie du CNRS (INC)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS)
Physique et mécanique des milieux hétérogenes (UMR 7636) (PMMH)
Ecole Superieure de Physique et de Chimie Industrielles de la Ville de Paris (ESPCI Paris)
Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS)-Université de Paris (UP)
Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS)-Université Paris Cité (UPCité)
Source :
Journal of Non-Crystalline Solids, Journal of Non-Crystalline Solids, Elsevier, 2000, 265 (1-2), pp.83-97. ⟨10.1016/S0022-3093(99)00885-6⟩, Journal of Non-Crystalline Solids, 2000, 265 (1-2), pp.83-97. ⟨10.1016/S0022-3093(99)00885-6⟩
Publication Year :
2000
Publisher :
HAL CCSD, 2000.

Abstract

The structure of sol–gel synthesized titanium oxo-polymers has been investigated using solid and liquid state 17O NMR and small angle X-ray scattering (SAXS). The growth of the titanium oxo-polymers has been controlled to produce sols and gels by adjusting two main parameters: the hydrolysis ratio H=[H2O]/[Ti] and the inhibitor ratio p=[H+]/[Ti] or a=[ acacH ]/[ Ti ] ( acacH = acetylacetone ) . The combination of 17O NMR and SAXS techniques has allowed us to determine the structure of the oxo-polymers at a local and a semi local scale. The proposed model for the structure of these oxo-polymers is based on the condensation of sub-units with a mean composition Ti(OZ)x(OH)yO2 − (x + y)/2 (OZ=Acac+OBun) and having a gyration radius of about 20–25 A. These sub-units are made with a titanium-oxo core built with μ2-O, μ3-O, μ4-O bridges and their surface is capped by the residual ligands OZ. Increasing the hydrolysis ratio H or decreasing the inhibitor ratio (p or a), mainly results in an increase of the size and the fractal dimension of the oxo-polymers, while the size and the mean composition of titanium oxo-core constituting the sub-units are apparently not modified.

Details

Language :
English
ISSN :
00223093
Database :
OpenAIRE
Journal :
Journal of Non-Crystalline Solids, Journal of Non-Crystalline Solids, Elsevier, 2000, 265 (1-2), pp.83-97. ⟨10.1016/S0022-3093(99)00885-6⟩, Journal of Non-Crystalline Solids, 2000, 265 (1-2), pp.83-97. ⟨10.1016/S0022-3093(99)00885-6⟩
Accession number :
edsair.doi.dedup.....c31c2988364c854ac38911613f589f60
Full Text :
https://doi.org/10.1016/S0022-3093(99)00885-6⟩