New process of preparation, structure, and physicochemical investigations of the new titanyl phosphate Ti{sub 2}O(H{sub 2}O)(PO{sub 4}){sub 2}
- LCMS, UFR Sciences des Materiaux Solides, Faculte des Sciences Ben M'Sik, Casablanca (Morocco)
- Institut de chimie de la matiere condensee de Bordeaux (ICMCB-CNRS UPR 9048), Universite de Bordeaux 1, 87 Av. Dr. Schweitzer, 33608 Pessac (France)
- Laboratoire Leon Brillouin, Saclay (France)
New titanyl phosphate Ti{sub 2}O(H{sub 2}O)(PO{sub 4}){sub 2} has been prepared and characterized by X-ray and neutron diffraction, nuclear magnetic resonance, infrared and Raman spectroscopies and thermogravimetric analysis. The crystal structure has been solved from neutron powder diffraction data at 300 K by Rietveld method in P2{sub 1} space group. The refinement led to satisfactory profile factors (R{sub p}=2.7%, R{sub wp}=3.2%) and crystal structure model indicators (R{sub B}=5.8%, R{sub F}=3.2%). The cell is monoclinic with a=7.3735 A, b=7.0405 A, c=7.6609 A and {beta}=121.48{sup o}, Z=4. The structure can be described as a three-dimensional framework built up by chains of [TiO{sub 5}(OH{sub 2})] octahedra with alternative short bonds [Ti{sub (1)}-O{sub (12)}; Ti{sub (2)}-O{sub (12)}, 1.88-1.84 A] and long ones [Ti{sub (1)}-O{sub W}; Ti{sub (2)}-O{sub W}, 2.25-2.23 A] along c-axis and connected via [PO{sub 4}] tetrahedra. Oxygen atom denoted O{sub (12)} is only linked to two titanium atoms and Oxygen atom denoted O{sub W} is linked to two titanium atoms and two hydrogen atoms. O{sub (12)} and O{sub W} are not linked to P atoms and justify the titanyl phosphate formulation Ti{sub 2}O(H{sub 2}O)(PO{sub 4}){sub 2}. The infrared and Raman spectra presents peaks due to vibrations of Ti-O, P-O and O-H bonds. The {sup 31}P MAS NMR spectrum reveals two {sup 31}P resonance lines, in agreement with the structure which showed two crystallographic sites for phosphorus. The thermogravimetric analysis show that Ti{sub 2}O(H{sub 2}O)(PO{sub 4}){sub 2} is thermally stable until 400 deg. C. Above this temperature, it losses water and decomposes to Ti{sub 5}O{sub 4}(PO{sub 4}){sub 4} and TiP{sub 2}O{sub 7}. - Graphical abstract: The structure of TiHP can be described as a TiOPO{sub 4} framework constituted by chains of tilted corner-sharing [TiO{sub 6}] octahedra and cross linked by [PO{sub 4}] tetrahedra with empty cavities in the framework.
- OSTI ID:
- 21049502
- Journal Information:
- Journal of Solid State Chemistry, Vol. 180, Issue 10; Other Information: DOI: 10.1016/j.jssc.2007.07.028; PII: S0022-4596(07)00305-2; Copyright (c) 2007 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved; Country of input: International Atomic Energy Agency (IAEA); ISSN 0022-4596
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
CRYSTALLOGRAPHY
HYDROGEN
INDICATORS
MONOCLINIC LATTICES
NEUTRON DIFFRACTION
NMR SPECTRA
NUCLEAR MAGNETIC RESONANCE
PHOSPHATES
PHOSPHORUS
RAMAN SPECTRA
RAMAN SPECTROSCOPY
SPACE GROUPS
SYNTHESIS
THERMAL GRAVIMETRIC ANALYSIS
TITANIUM COMPOUNDS
WATER
X-RAY DIFFRACTION