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α-tricalcium phosphate synthesis from amorphous calcium phosphate: structural characterization and hydraulic reactivity

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Abstract

In the present study, amorphous tricalcium phosphate (TCP) has been synthetized by a wet route to obtain low temperature α-TCP at 650 °C (LT-αTCP) and compare its structural, physical–chemical and thermal properties with those of α-TCP obtained by the conventional solid-state reaction method at 1400 °C (HT-αTCP). Even if no significant differences were observed concerning the values of lattice parameters measured by Rietveld refinement, LT-αTCP presented lower crystallinity and higher crystal strains than HT-αTCP. The reactivity in water of the α-TCP obtained by the two different routes was assessed. Both raw samples appeared relatively inert in solution and did not favour the nucleation of calcium deficient apatite (CDA); the LT-αTCP and HT-αTCP were converted into apatite only after milling. The mechanical process leads to a decrease in crystallinity and the formation of an amorphous phase, which is supported in this work by Raman spectroscopy. The faster rate of conversion of milled LT-αTCP compared to HT-αTCP can be assigned to its higher specific surface area, lower crystallinity and higher residual crystal strain; these favour the dissolution of the α-TCP phase. Finally, the setting properties of α-TCP-based bone cements were compared regarding their synthesis route. Although the synthesis route does not significantly affect the setting times, the kinetic of conversion into CDA was faster for LT-αTCP than for HT-αTCP. Thus, the modulation of the dissolution rate of α-TCP-based cement determined by the preparation route and the grinding process allows control of the overall setting reaction.

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Acknowledgements

M.P.G. acknowledges the support provided by the Spanish Government through Project MAT2015-65601-R (MINECO/FEDER, UE), and the “Generalitat de Catalunya” for the 2017 SGR11-65 and the Icrea Academia Award. M.E. acknowledges the Serra Hunter Fellowship. This project was supported by Inca-Cancéropôle GSO under the DOXOSARCOME project.

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Authors and Affiliations

  1. CIRIMAT, Université de Toulouse, CNRS, Université Toulouse 3 Paul Sabatier, INP-ENSIACET, 4 allée Emile Monso, 31030, Toulouse cedex 4, France

    T. Martinez, C. Charvillat, O. Marsan, C. Rey & S. Sarda

  2. Biomaterials, Biomechanics and Tissue Engineering Group, Department of Materials Science and Engineering, Universitat Politècnica de Catalunya, Av. Eduard Maristany 10-14, 08019, Barcelona, Spain

    M. Espanol & M. P. Ginebra

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Martinez, T., Espanol, M., Charvillat, C. et al. α-tricalcium phosphate synthesis from amorphous calcium phosphate: structural characterization and hydraulic reactivity. J Mater Sci 56, 13509–13523 (2021). https://doi.org/10.1007/s10853-021-06161-0

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