Characterization of the transformation from calcium-deficient apatite to β-tricalcium phosphate

Gibson, I.R. and Rehman, I. and Best, S.M. and Bonfield, W. (2000) Characterization of the transformation from calcium-deficient apatite to β-tricalcium phosphate. Journal of Materials Science: Materials in Medicine, 11 (12). pp. 799-804. ISSN 0957-4530

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 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. © 2000 Kluwer Academic Publishers. 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 crystalline 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 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.