Advertisement

Synthesis of tetracalcium phosphate from mechanochemically activated reactants and assessment as a component of bone cements

  • H. E. Romeo
  • M. A. Fanovich
Article

Abstract

The aim of this work was to gain a better understanding about the synthesis of tetracalcium phosphate (TTCP, Ca4(PO4)2O) through a solid-state reaction from mechanochemically activated CaCO3–(NH4)2HPO4 mixtures. The evolution of the reaction was followed by DTA, XRD, FTIR and SEM techniques. An enhanced reactivity of the mixtures was detected as the mechanochemical treatment times increased. This effect was related to both the loss of crystallinity of the reactants and the production of defects on their surfaces. 6 h of mechanochemical processing at 1190 rpm, followed by 3 h of thermal treatment at 1500°C, were enough to obtain pure TTCP. The crystallinity and purity of the obtained TTCP were checked by XRD and FTIR. The morphologic characteristics were analyzed by SEM and BET analysis. The behavior of synthesized TTCP powder in combination with commercial dicalcium phosphate anhydrous (DCPA, CaHPO4), as the solid phase of bone cements, was tested. Both the combination of different particle sizes of TTCP and DCPA and the effect of different kinds of accelerator agents (disodium hydrogen phosphate, tartaric acid, citric acid and oxalic acid) on setting time and degree of conversion to hydroxyapatite (HA, Ca10(PO4)6(OH)2) were evaluated. The combination of TTCP (0.32 m2/g) with DCPA (1.52 m2/g), in a 1/1 molar ratio, showed the shortest setting times and high conversions to HA when an oxalic acid solution (5% volume fraction) was used as the liquid phase of the formulation. Results obtained from this work demonstrated that synthesized TTCP shows promising behavior as a component of bone cements, exhibiting not only a smaller particle size than that usually reported but also a low degree of crystallinity, all of which increases the reactivity of the obtained TTCP. This study provided a very efficient method for synthesizing pure TTCP through a modified solid-state reaction from mechanochemically activated reactants, employing very short times of thermal treatment in comparison with the conventional processes.

Keywords

Calcium Phosphate Cement Mechanochemical Activation Mechanochemical Treatment Oxalic Acid Solution DCPA 
These keywords were added by machine and not by the authors. This process is experimental and the keywords may be updated as the learning algorithm improves.

Notes

Acknowledgements

The financial support of the following institutions is gratefully acknowledged: National Research Council (CONICET, Argentina), National Agency for the Promotion of Science and Technology (ANPCyT, Argentina, PICT 12-14593), University of Mar del Plata and Fundación Antorchas (Argentina).

References

  1. 1.
    B.W. Brown, L.C. Chow, Dental Restorative Cement Paste. US Patent No. 4.518.430, 1985Google Scholar
  2. 2.
    S. Matsuya, S. Takagi, L.C. Chow, J. Mater. Sci: Mater. Med. 11, 305 (2000)CrossRefGoogle Scholar
  3. 3.
    L.E. Carey, H.H.K. Xu, C.G. Simon, S. Takagi, L.C. Chow, Biomaterials 26, 5002 (2005)CrossRefGoogle Scholar
  4. 4.
    H.H.K. Xu, L.E. Carey, C.G. Simon Jr., S. Takagi, L.C. Chow, Dent. Mat. 23, 433 (2007)CrossRefGoogle Scholar
  5. 5.
    Y. Fukase, E.D. Eanes, S. Takagi, L.C. Chow, W.E. Brown, J. Dent. Res. 69, 1852 (1990)Google Scholar
  6. 6.
    H.H.K. Xu, C.G. Simon Jr, Biomaterials 26, 1337 (2005)CrossRefGoogle Scholar
  7. 7.
    H.H.K. Xu, J.B. Quinn, Biomaterials 23, 193 (2002)CrossRefGoogle Scholar
  8. 8.
    M. Bohner, U. Gbureck, J.E. Barralet, Biomaterials 26, 6423 (2005)CrossRefGoogle Scholar
  9. 9.
    L.C. Chow, M. Marcovic, S.A. Frukhtbeyn, S. Takagi, Biomaterials 26, 393 (2005)CrossRefGoogle Scholar
  10. 10.
    C. Liu, H. Shao, F. Chen, H. Zheng, Biomaterials 24, 4103 (2003)CrossRefGoogle Scholar
  11. 11.
    S. Serraj, P. Boudeville, B. Pauvert, A. Terol, J. Biomed. Mat. Res. 55, 566 (2001)CrossRefGoogle Scholar
  12. 12.
    S. Serraj, P. Boudeville, A. Terol, J. Mater. Sci: Mater. Med. 12, 45 (2001)CrossRefGoogle Scholar
  13. 13.
    C.L. Camiré, U. Gbureck, W. Hirsiger, M. Bohner, Biomaterials 26, 2787 (2005)CrossRefGoogle Scholar
  14. 14.
    M.P. Ginebra, F.C.M. Driessens, J.A. Planell, Biomaterials 25, 3453 (2004)CrossRefGoogle Scholar
  15. 15.
    Y. Sargin, M. Kizilyalli, C. Telli, H. Güler, J. Eur. Ceram. Soc. 17, 963 (1997)CrossRefGoogle Scholar
  16. 16.
    V.V. Samuskevich, N.K. Belous, L.N. Samuskevich, J. Inorg. Mat. 39, 520 (2003)CrossRefGoogle Scholar
  17. 17.
    J.E. Barralet, L. Grover, T. Gaunt, A.J. Wright, I.R. Gibson, Biomaterials 23, 3063 (2002)CrossRefGoogle Scholar
  18. 18.
    A. Hoshikawa, N. Fukui, A. Fukuda, T. Sawamura, M. Hattori, K. Nakamura, H. Oda, Biomaterials 24, 4967 (2003)CrossRefGoogle Scholar
  19. 19.
    D. Guo, K. Xu, X. Zhao, Y. Han, Biomaterials 26, 4073 (2005)CrossRefGoogle Scholar
  20. 20.
    U. Gbureck, J.E. Barralet, M. Hofmann, R. Thull, J. Am. Ceram. Soc. 87, 311 (2004)CrossRefGoogle Scholar
  21. 21.
    U. Gbureck, M.P. Hofmann, J.E. Barralet, J. Am. Ceram. Soc. 88, 1327 (2005)CrossRefGoogle Scholar
  22. 22.
    A.W. Weeber, H. Bakker, Condens Matter 153, 93 (1988)CrossRefGoogle Scholar
  23. 23.
    R.C. Weast (ed.), Handbook of Chemistry and Physics (CRC Press, Boca Raton, FL, USA, 1976)Google Scholar
  24. 24.
    A. Slosarczyk, C. Paluszkiewicz, M. Gawlicki, Z. Paszkiewicz, Ceram. Int. 23, 297 (1997)CrossRefGoogle Scholar
  25. 25.
    U. Posset, E. Locklin, R. Thull, W. Kiefer, J. Biomed. Mater. Res. 40, 640 (1998)CrossRefGoogle Scholar
  26. 26.
    I. Martin, P.W. Brown, Adv. Cem. Res. 5, 115 (1993)Google Scholar
  27. 27.
    L.L. Hench, Handbook of Bioactive Ceramics, vol. II (CRC Press, Boca Raton, USA, 1990)Google Scholar
  28. 28.
    C.S. Liu, W. Shen, J. Mater. Sci.: Mater. Med. 8, 803 (1997)CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media, LLC 2008

Authors and Affiliations

  1. 1.Institute of Materials Science and Technology (INTEMA)University of Mar del Plata and National Research Council (CONICET)Mar del PlataArgentina

Personalised recommendations