Journal of Chemical Crystallography

, Volume 40, Issue 4, pp 323–327 | Cite as

Structural Characterization of Na0.96Ho9.04(SiO4)6Cl0.02O1.98 Apatite Prepared by Mechanical Milling

  • Ivonne Rosales
  • Eligio Orozco
  • Lauro Bucio
  • Maria E. Fuentes
  • Luis Fuentes
Original Paper
First Online:
Received:
Accepted:

Abstract

In this paper we report the synthesis and structural characterization of Na0.96Ho9.04(SiO4)6Cl0.02O1.98 apatite prepared by mechanical milling at room temperature, in which well crystallized sample was obtained after heating the sample at 1123 K. The crystal structure study was carried out by synchrotron radiation diffraction. This apatite crystallizes in the hexagonal space group P6 3 /m (No. 176) with cell parameters a = 9.3444(1) Å, c = 6.7611(1) Å, unit cell volume of 511.27(1) Å3 and Z = 1. As in other rare-earth orthosilicate apatites, it was found that sodium cations are mixed with holmium occupying the 4f position at the center of tricapped trigonal prisms; while holmium fully occupies the 6h position at the center of a seven-coordinated polyhedron. No vacancies are present in the two crystallographic sites available for holmium atoms. The chemical composition was established by wavelength dispersive spectroscopy.

Graphical Abstract

The title compound, Na0.96Ho9.04(SiO4)6Cl0.02O1.98 was synthesized by mechanical milling at room temperature and well crystallinity was obtained after heating the sample at 1123 K. X-ray powder diffraction analysis reveals that sodium cations in the crystal structure, are mixed with holmium occupying one of the crystallographic sites.

Keywords

Synchrotron radiation Oxychloroapatite Mechanochemical synthesis WDS microanalysis 
This is a preview of subscription content, log in to check access.

Notes

Acknowledgments

Portions of this research were carried out at the Stanford Synchrotron Radiation Lightsource, a national user facility operated by Stanford University on behalf of the U.S. Department of Energy, Office of Basic Energy Sciences. The authors acknowledge to Manuel Aguilar for the conventional X-ray diffraction measurements at Instituto de Física and Carlos Linares by the WDS measurements at the Laboratorio Universitario de Petrología, both laboratories at Universidad Nacional Autónoma de México; and Angel Osornio by his technical support. I. Rosales acknowledges the postdoctoral fellowship of Consejo Nacional de Ciencia y Tecnologia (CONACyT) and projects CONACYT SEP 81700, CONACyT SEP-2004-C01-47652, and DGAPA-PAPIIT IN118106-3.

References

  1. 1.
    Emirdag-Eanes M, Pennington WT, Kolis JW (2004) J Alloys Compd 366:76CrossRefGoogle Scholar
  2. 2.
    Redhammer GJ, Roth G (2003) Acta Cryst C 59:i120CrossRefGoogle Scholar
  3. 3.
    Higuchi M, Masubuchi Y, Nakayama S, Kikkawa S, Kodaira K (2004) Solid State Ionics 174:73CrossRefGoogle Scholar
  4. 4.
    Masubuchi Y, Higuchi M, Takeda T, Kikkawa S (2006) Solid State Ionics 177:263CrossRefGoogle Scholar
  5. 5.
    Tao S, Irving JTS (2001) Mater Res Bull 36:1245CrossRefGoogle Scholar
  6. 6.
    Rodríguez-Reyna E, Fuentes AF, Maczka M, Lanuza J, Boulahya K, Amador U (2006) J Solid State Chem 179:522CrossRefGoogle Scholar
  7. 7.
    Fuentes AF, Rodríguez-Reyna E, Martínez-González LG, Maczka M, Lanuza J, Amador U (2006) Solid State Ionics 177:1869CrossRefGoogle Scholar
  8. 8.
    Veilleux D, Barthelemy N, Trombe JC, Verelst M (2001) J Mater Sci 36:2245CrossRefGoogle Scholar
  9. 9.
    Vijayalakshmi U, Rajeswari S (2006) Tends Biomater Artif Organs 19:57Google Scholar
  10. 10.
  11. 11.
    Gunawardane RP, Howie RA, Glasser FP (1982) Acta Cryst B 38:1564CrossRefGoogle Scholar
  12. 12.
    Gualtieri AFJ (2000) J Appl Cryst 33:267CrossRefGoogle Scholar
  13. 13.
    Beall GW, Milligan WO, Wolcott HAJ (1977) Inorg Nucl Chem 39:65CrossRefGoogle Scholar
  14. 14.
    Rodríguez-Carvajal J FULLPROF (version July 2006) http://www.ill.eu/sites/fullprof/php/reference.html
  15. 15.
    Thompson P, Cox DE, Hastings JB (1987) J Appl Cryst 20:79CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media, LLC 2009

Authors and Affiliations

  • Ivonne Rosales
    • 1
  • Eligio Orozco
    • 1
  • Lauro Bucio
    • 1
  • Maria E. Fuentes
    • 2
  • Luis Fuentes
    • 3
  1. 1.Instituto de FísicaUniversidad Nacional Autónoma de México, Ciudad UniversitariaMéxico D.F.México
  2. 2.Facultad de QuímicaUniversidad Autónoma de ChihuahuaChihuahuaMéxico
  3. 3.Centro de Investigación en Materiales AvanzadosChihuahuaMéxico

Personalised recommendations