Abstract
The structural changes that occur during the transformation of a Ca-deficient apatite, prepared by a wet chemical method, to β-TCP were investigated. X-ray diffraction (XRD) analysis of as-prepared samples and samples calcined at temperatures between 500 and 1100 °C showed that the transformation occurs over the temperature range 710–740 °C, under non-equilibrium conditions. The change in crystallite size with increasing calcination/sintering temperature was studied by XRD using the Scherrer formula. Fourier transform infra-red (FTIR) analysis indicated considerable structural change in samples above and below this temperature range. Changes were observed in the hydroxyl, carbonate and phosphate bands as the calcination temperature was increased from 500 to 1100 °C. Even once a single β-TCP phase is obtained at 740 °C there remains a considerable amount of structural change at temperatures between 740 and 1100 °C. This effect was illustrated by an unusual change in the lattice parameters of the β-TCP structure and significant changes in the phosphate bands of the FTIR spectra as the calcination temperature was increased. The results obtained in this study show that the combined experimental techniques of XRD and FTIR are excellent complimentary methods for characterizing structural changes that occur during phase transformations.
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References
F. C. M. Driessens, in “Bioceramics of calcium phosphate”, edited by K. de Groot (CRC Press, Boca Raton, 1983) p. 1–32.
A. M. Gatti, D. Zaffe and G. P. Poli, Biomaterials 11 (1990) 513.
M. Akao, H. Aoki, K. Katoand A. Sato, J. Mater. Sci. 17 (1982) 343.
M. Jarcho, R. L. Salsbury, M. B. Thomas and R. H. Doremus, ibid. 14 (1979) 142.
R. Famery, N. Richard and P. Boch, Ceram. Inter. 20 (1994) 327.
E. R. Kreidler and F. A. Hummel, Inorg. Chem. 6 (1967) 884.
L. Yubao, C. P. A. T. Klein, S. Van De Meer and K. De Groot, J. Mater. Sci.: Mater. Med. 5 (1994) 263.
J. J. Prieto Valdés, J. Ortiz López, G. Rueda Morales, G. Pacheco Malagon and V. Prieto Gortcheva, ibid. 8 (1997) 297.
A. Mortier, J. Lemaitre and P. G. Rouxhet, Thermochemica Acta 143 (1989) 265.
A. Mortier, J. Lemaitre, L. Rodrique and P. G. Rouxhet, J. Solid State Chem. 78 (1989) 215.
A. C. Larson, R. B. Von Dreele and M. Lujan JR, GSAS—Generalized Crystal Structure Analysis System, Neutron Scattering Center, Los Alamos National Laboratory, California (1990).
M. I. Kay, R. A. Young and A. S. Posner, Nature 204 (1964) 1050.
B. Dickens, L. W. Schroeder and W. E. Brown, J. Solid State Chem. 10 (1974) 232.
PDF Card no. 9–432, ICDD, Newton Square, Pennsylvania, USA.
PDF Card no. 9–169, ICDD, Newton Square, Pennsylvania, USA.
I. R. Gibson, M. Akao, S. M. Best and W. Bonfield in “Bioceramics 9”, edited by T. Kokubo, T. Nakamura and F. Miyaji (University Press, UK, 1996) p. 173.
I. Rehman and W. Bonfield, J. Mater. Sci.: Mater. Med. 8 (1997) 1.
L. Yubao, PhD Thesis, University of Leiden, Netherlands (1994).
R. Z. Legeros, J. P. Legeros, G. Daculsi and R. Kijkowska, in “Encyclopedic Handbook of Biomaterials and Bioengineering”, edited by D. L. Wise, D. J. Trantolo, D. E. Altobelli, M. J. Yaszemski, J. D. Gresser and E. R. Schwartz (Marcel Dekker, Inc., 1995) p. 1429.
K. Ishikawa, P. Ducheyne and S. Radin, J. Mater. Sci.: Mater. Med. 4 (1993) 165.
P. N. De Aza, C. Santos, A. Pazo, S. De Aza, R. Cusco and L. Artus, Chem. Mater. 9 (1997) 912.
D. G. A. Nelson and J. D. B. Featherstone, Calc. Tiss. Int. 34 (1982) 69.
H. Elfeki, C. Rey and M. Vignoles, ibid. 49 (1991) 269.
R. Z. Legeros, G. Kijkowska, J. P. Legeros, T. Abergas and H. Bleiwas, J. Dent. Res. 66 (1987) 190.
J. C. Elliott, D. W. Holcomb and R. A. Young, Calc. Tiss. Int. 37 (1985) 372.
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Gibson, I.R., Rehman, I., Best, S.M. et al. Characterization of the transformation from calcium-deficient apatite to β-tricalcium phosphate. Journal of Materials Science: Materials in Medicine 11, 533–539 (2000). https://doi.org/10.1023/A:1008961816208
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DOI: https://doi.org/10.1023/A:1008961816208