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

The structural changes that occur during the transformation of a Ca-deficient apatite, prepared by a wet chemical method, to beta-TCp were investigated. X-ray diffraction (XRD) analysis of as-prepared samples and samples calcined at temperatures between 500 and 1100 degrees C showed that the transformation occurs over the temperature range 710-740 degrees 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 degrees C. Even once a single beta-TCP phase is obtained at 740 degrees C there remains a considerable amount of structural change at temperatures between 740 and 1100 degrees C. This effect was illustrated by an unusual change in the lattice parameters of the beta-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.