TY - JOUR

T1 - Characterization of the transformation from calcium-deficient apatite to β-tricalcium phosphate

AU - Gibson, I.R.

AU - Rehman, I.

AU - Best, S.M.

AU - Bonfield, W.

PY - 2000

Y1 - 2000

N2 - 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.

AB - 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.

KW - Biocompatibility

KW - Calcination

KW - Crystal lattices

KW - Fourier transform infrared spectroscopy

KW - Lattice constants

KW - Phase transitions

KW - Sintering

KW - Thermal effects

KW - Wetting

KW - X ray diffraction analysis

KW - Calcium deficient apatite

KW - Crystallite size

KW - Scherrer formula

KW - Structural changes

KW - Wet chemical method

KW - Calcium compounds

KW - apatite

KW - calcium phosphate

KW - article

KW - conformational transition

KW - crystal structure

KW - Fourier transformation

KW - priority journal

KW - temperature dependence

KW - ultraviolet spectroscopy

KW - X ray diffraction

U2 - 10.1023/A:1008905613182

DO - 10.1023/A:1008905613182

M3 - Journal article

VL - 11

SP - 799

EP - 804

JO - Journal of Materials Science: Materials in Medicine

JF - Journal of Materials Science: Materials in Medicine

SN - 0957-4530

IS - 12

ER -