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The influence of phosphorus precursors on the synthesis and bioactivity of SiO2–CaO–P2O5 sol–gel glasses and glass–ceramics

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Abstract

Bioactive glasses and glass–ceramics of the SiO2–CaO–P2O5 system were synthesised by means of a sol–gel method using different phosphorus precursors according to their respective rates of hydrolysis—triethylphosphate (OP(OC2H5)3), phosphoric acid (H3PO4) and a solution prepared by dissolving phosphorus oxide (P2O5) in ethanol. The resulting materials were characterised by differential scanning calorimetry and thermogravimetry, X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy coupled with energy dispersive X-ray spectroscopy and by in vitro bioactivity tests in acellular simulated body fluid. The different precursors significantly affected the main steps of the synthesis, beginning with the time required for gel formation. The most striking influence of these precursors was observed during the thermal treatments at 700–1,200 °C that were used to convert the gels into glasses and glass–ceramics. The samples exhibited very different mineralisation behaviours; especially those prepared using the phosphoric acid, which had a reduced onset temperature of crystallisation and an increased resistance to devitrification. However, all resulting materials were bioactive. The in vitro bioactivity of these materials was strongly affected by the heat treatment temperature. In general, their bioactivity decreased with increasing treatment temperature. For crystallised samples obtained above 900 °C, the bioactivity was favoured by the presence of two crystalline phases: wollastonite (CaSiO3) and tricalcium phosphate (α-Ca3(PO4)2).

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Acknowledgments

We extend our appreciation to Dr. Aluísio A. Cabral Júnior, from the Instituto Federal de Educação, Ciência e Tecnologia do Maranhão, Brazil, for the DSC and TG analyses and to Dr. Olga S. Dymshits, from NITIOM State Optical Institute, Russian Federation, for the valuable instructions and discussions. We also thank the Brazilian funding agencies Fundação de Amparo à Pesquisa do Estado de São Paulo—FAPESP (2007/08179-9) and Coordenação de Aperfeiçoamento de Pessoal de Nível Superior—CAPES for the financial support used to accomplish of this research project.

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  1. Grupo de Pesquisas em Nanotecnologia e Nanomateriais, Centro Federal de Educação Tecnológica de Minas Gerais, Campus Timóteo, Av. Amazonas 1193, Vale Verde, Timóteo, MG, 35183-006, Brazil

    Renato Luiz Siqueira

  2. Laboratório de Materiais Vítreos, Departamento de Engenharia de Materiais, Universidade Federal de São Carlos, Rod. Washington Luís km 235, CP 676, São Carlos, SP, 13565-905, Brazil

    Renato Luiz Siqueira & Edgar Dutra Zanotto

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Correspondence to Renato Luiz Siqueira.

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Siqueira, R.L., Zanotto, E.D. The influence of phosphorus precursors on the synthesis and bioactivity of SiO2–CaO–P2O5 sol–gel glasses and glass–ceramics. J Mater Sci: Mater Med 24, 365–379 (2013). https://doi.org/10.1007/s10856-012-4797-x

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