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Spray-drying-derived amorphous calcium phosphate: a multi-scale characterization

  • Ceramics
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Abstract

Amorphous calcium orthophosphates (ACP) are bioactive compounds presenting high interest as bone substitute. However, the synthesis of such metastable products requires special attention as they can rapidly evolve into a crystalline phase during the elaboration process. The resulting increased stability generally leads to less bioactive reactive materials. Among the various strategies developed to obtain stable form of ACP, the use of spray drying is an effective and reproducible route. Compared to previous works, this study aims to demonstrate for the first time the feasibility of ACP elaboration by spray drying directly from a single solution of selected precursors. Moreover, structuration of the spray-dried powders was determined at different length scales, demonstrating a hierarchical organization from nanometric clusters to particles aggregates. These complementary analyses highlighted a thorough mechanism of particles formation during processing. The effect of the initial composition of the solution was observed, and it was demonstrated that there is a correlation with the purity of the final product that may be modulated. In addition, ACP powders were found to be highly reactive in aqueous medium and their fast transformation into low crystalline apatite suggests a good suitability for biomedical use.

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Acknowledgements

The authors would like to acknowledge Marianne Clerc-Imperor for helpful discussions about SAXS results, Gwénaëlle Guittier (LGC) for N2 adsorption measurements and Cédric Charvillat (CIRIMAT) for XRD and TGA-TDA measurements. They also want to thank Alessandro Pugliara and Teresa Hungria (Centre de MicroCaractérisation Raimond Castaing UMS 3623) and Stéphanie Balor (METi) for the TEM analyses. The FERMaT Federation FR3089, Université de Toulouse, CNRS, is acknowledged too for providing small-angle X-ray scattering laboratory facility.

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Authors and Affiliations

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

    Sylvain Le Grill, Jeremy Soulie, Olivier Marsan, Cédric Charvillat, Ghislaine Bertrand, Christian Rey & Fabien Brouillet

  2. LCC, UPR 8241 CNRS, Université de Toulouse, 205 route de Narbonne, Toulouse, France

    Yannick Coppel

  3. LGC, CNRS, Université de Toulouse, 118 route de Narbonne Bâtiment 2R1, Toulouse, France

    Pierre Roblin

  4. CEMES, CNRS, Université de Toulouse, 29 Rue Jeanne Marvig, Toulouse, France

    Pierre Lecante

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  1. Sylvain Le Grill
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Le Grill, S., Soulie, J., Coppel, Y. et al. Spray-drying-derived amorphous calcium phosphate: a multi-scale characterization. J Mater Sci 56, 1189–1202 (2021). https://doi.org/10.1007/s10853-020-05396-7

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