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Title: Synthesis, structure refinement and characterisation of a new oxyphosphate Mg{sub 0.50}TiO(PO{sub 4})

Abstract

A new titanium oxyphosphate Mg{sub 0.50}TiO(PO{sub 4}) has been synthesized and characterized by several physical techniques: X-ray diffraction, {sup 31}P MAS-NMR, Raman diffusion, infrared absorption and diffuse reflectance spectroscopy. It crystallizes in the monoclinic system with unit cell parameters: a = 7.367(9), b = 7.385(8), c = 7.373(9) A, {beta} = 120.23(1), with the space group P2{sub 1}/c (no. 14), Z = 4. The crystal structure has been refined by the Rietveld method using X-ray powder diffraction. The conventional R indices obtained are R {sub wp} = 0.138, R {sub p} = 0.096 and R {sub B} = 0.0459. The structure of Mg{sub 0.50}TiO(PO{sub 4}) consists of infinite chains of corner-shared [TiO{sub 6}] octahedra parallel to the c-axis, crosslinked by corner-shared [PO{sub 4}] tetrahedra. These infinite chains have alternating short (1.74 A) and long (2.26 A) Ti-O bonds and are similar to those found in titanium oxyphosphate M{sup II} {sub 0.50}TiO(PO{sub 4}) (M{sup 2+} = Fe{sup 2+}, Co{sup 2+}, Ni{sup 2+}, Cu{sup 2+}, Zn{sup 2+}). The magnesium atom is located in an antiprism between two [TiO{sub 6}] octahedra. {sup 31}P MAS NMR showed only a single {sup 31}P resonance line, in a good agreement with the crystal structure. Raman andmore » IR spectra show strong bands respectively at 765 and 815 cm{sup -1}, attributed to the vibration of -Ti-O-Ti-O- bonds in the infinite chains. The gap due to the Oxygen-Titanium(IV) charge transfer is 3.37 eV.« less

Authors:
 [1];  [2];  [3];  [4];  [4];  [4];  [5]
  1. LCMS, UFR Sciences des Materiaux Solides, Faculte des Sciences Ben M' Sik, Casablanca (Morocco). E-mail: s.benmokhtar@univh2m.ac.ma
  2. LCMS, UFR Sciences des Materiaux Solides, Faculte des Sciences Ben M' Sik, Casablanca (Morocco)
  3. Departement de Chimie, Faculte des Sciences, Ain Chock, Casablanca (Morocco)
  4. Institut de chimie de la matiere condensee de Bordeaux (ICMCB-CNRS UPR 9048), 87, av. du Dr. A. Schweitzer, 33608 Pessac (France)
  5. Department of Chemistry, University of Pretoria, 0002 Pretoria (South Africa)
Publication Date:
OSTI Identifier:
21000637
Resource Type:
Journal Article
Resource Relation:
Journal Name: Materials Research Bulletin; Journal Volume: 42; Journal Issue: 5; Other Information: DOI: 10.1016/j.materresbull.2006.08.020; PII: S0025-5408(06)00346-1; Copyright (c) 2006 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; CHEMICAL PREPARATION; COBALT IONS; COPPER IONS; CROSS-LINKING; INFRARED SPECTRA; IRON IONS; MAGNESIUM; MONOCLINIC LATTICES; NICKEL IONS; NUCLEAR MAGNETIC RESONANCE; PHOSPHATES; PHOSPHORUS 31; SPACE GROUPS; SPECTROSCOPY; TITANIUM; X-RAY DIFFRACTION; ZINC IONS

Citation Formats

Benmokhtar, S., El Jazouli, A., Krimi, S., Chaminade, J.P., Gravereau, P., Menetrier, M., and Waal, D. de. Synthesis, structure refinement and characterisation of a new oxyphosphate Mg{sub 0.50}TiO(PO{sub 4}). United States: N. p., 2007. Web. doi:10.1016/j.materresbull.2006.08.020.
Benmokhtar, S., El Jazouli, A., Krimi, S., Chaminade, J.P., Gravereau, P., Menetrier, M., & Waal, D. de. Synthesis, structure refinement and characterisation of a new oxyphosphate Mg{sub 0.50}TiO(PO{sub 4}). United States. doi:10.1016/j.materresbull.2006.08.020.
Benmokhtar, S., El Jazouli, A., Krimi, S., Chaminade, J.P., Gravereau, P., Menetrier, M., and Waal, D. de. Thu . "Synthesis, structure refinement and characterisation of a new oxyphosphate Mg{sub 0.50}TiO(PO{sub 4})". United States. doi:10.1016/j.materresbull.2006.08.020.
@article{osti_21000637,
title = {Synthesis, structure refinement and characterisation of a new oxyphosphate Mg{sub 0.50}TiO(PO{sub 4})},
author = {Benmokhtar, S. and El Jazouli, A. and Krimi, S. and Chaminade, J.P. and Gravereau, P. and Menetrier, M. and Waal, D. de},
abstractNote = {A new titanium oxyphosphate Mg{sub 0.50}TiO(PO{sub 4}) has been synthesized and characterized by several physical techniques: X-ray diffraction, {sup 31}P MAS-NMR, Raman diffusion, infrared absorption and diffuse reflectance spectroscopy. It crystallizes in the monoclinic system with unit cell parameters: a = 7.367(9), b = 7.385(8), c = 7.373(9) A, {beta} = 120.23(1), with the space group P2{sub 1}/c (no. 14), Z = 4. The crystal structure has been refined by the Rietveld method using X-ray powder diffraction. The conventional R indices obtained are R {sub wp} = 0.138, R {sub p} = 0.096 and R {sub B} = 0.0459. The structure of Mg{sub 0.50}TiO(PO{sub 4}) consists of infinite chains of corner-shared [TiO{sub 6}] octahedra parallel to the c-axis, crosslinked by corner-shared [PO{sub 4}] tetrahedra. These infinite chains have alternating short (1.74 A) and long (2.26 A) Ti-O bonds and are similar to those found in titanium oxyphosphate M{sup II} {sub 0.50}TiO(PO{sub 4}) (M{sup 2+} = Fe{sup 2+}, Co{sup 2+}, Ni{sup 2+}, Cu{sup 2+}, Zn{sup 2+}). The magnesium atom is located in an antiprism between two [TiO{sub 6}] octahedra. {sup 31}P MAS NMR showed only a single {sup 31}P resonance line, in a good agreement with the crystal structure. Raman and IR spectra show strong bands respectively at 765 and 815 cm{sup -1}, attributed to the vibration of -Ti-O-Ti-O- bonds in the infinite chains. The gap due to the Oxygen-Titanium(IV) charge transfer is 3.37 eV.},
doi = {10.1016/j.materresbull.2006.08.020},
journal = {Materials Research Bulletin},
number = 5,
volume = 42,
place = {United States},
year = {Thu May 03 00:00:00 EDT 2007},
month = {Thu May 03 00:00:00 EDT 2007}
}