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The effect of cyclic heat treatment on the physicochemical properties of bio hydroxyapatite from bovine bone

  • Biomaterials Synthesis and Characterization
  • Original Research
  • Published:
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Abstract

This paper focus on physicochemical changes in bio-hydroxyapatite (BIO-HAp) from bovine femur obtained by calcination at high temperatures: 520–620 (each 20 °C) at 7.4 °C/min and from 700 to 1100 °C (each 100 °C) at three heating rates: 7.4, 9.9, and 11.1 °C/min. BIO-HAp samples were obtained using a multi-step process: cleaning, milling, hydrothermal process, calcination in an air atmosphere, and cooling in furnace air. Inductively Couple Plasma (ICP) showed that the presence of Mg, K, S, Ba, Zn, and Na, is not affected by the annealing temperature and heating rate. While Scanning Electron Microscopy (SEM) images showed the continuous growth of the HAp crystals during the calcination process due to the coalescence phenomenon, and the Full Width at the Half Maximum for the X-ray patterns for temperatures up to 700 is affected by the annealing temperature and the heating rate. Through X-ray diffraction, thermal, and calorimetric analysis (TGA-DSC), a partial dehydroxylation of hydroxyapatite was found in samples calcined up to 900 °C for the three heating rates. Also, Ca/P molar ratio decreased for samples calcined up to 900 °C as a result of the dehydroxylation process. NaCaPO4, CaCO3, Ca3(PO4)2, MgO, and Ca(H2PO4)2 are some phases identified by X-ray diffraction; some of them are part of the bone and others were formed during the calcination process as a function of annealing temperature and heating rate, as it is the case for MgO.

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Acknowledgements

S. M. Londoño-Restrepo thanks the Consejo Nacional de Ciencia y Tecnologıa (CONACYT-Mexico) for the financial support of her Ph.D. thesis, and PAPIIT project number IN112317 for the financial support of this investigation as well. The authors would like to thank Dr. Genoveva Hernandez-Padrón for her technical support for the Raman experiments, Dra. Beatriz Millan Malo and M. Alicia del Real for technical support, and Carolina Muñoz from CGEO-UNAM for the ICP determinations. Authors thank Alexandra Morin Dube for the technical English revision of this article.

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Authors and Affiliations

  1. Posgrado en Ciencia e Ingeniería de Materiales, Centro de Física Aplicada y Tecnología Avanzada, Universidad Nacional Autónoma de México, Campus Juriquilla, Querétaro, c.p. 76230, Mexico

    S. M. Londoño-Restrepo

  2. Licenciatura en Tecnología, Centro de Física Aplicada y Tecnología Avanzada, Universidad Nacional Autónoma de México, Campus Juriquilla, Querétaro, c.p. 76230, Mexico

    R. Jeronimo-Cruz

  3. Benemérita Universidad Autónoma de Puebla, Centro Universitario de Vinculación y Transferencia de Tecnología, Ciudad Universitaria, Puebla, c.p. 72570, Mexico

    E. Rubio-Rosas

  4. Departamento de Nanotecnología, Centro de Física Aplicada y Tecnología Avanzada, Universidad Nacional Autónoma de México, Campus Juriquilla, Querétaro, c.p. 76230, Mexico

    M. E. Rodriguez-García

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  1. S. M. Londoño-Restrepo
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  3. E. Rubio-Rosas
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Correspondence to M. E. Rodriguez-García.

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Londoño-Restrepo, S.M., Jeronimo-Cruz, R., Rubio-Rosas, E. et al. The effect of cyclic heat treatment on the physicochemical properties of bio hydroxyapatite from bovine bone. J Mater Sci: Mater Med 29, 52 (2018). https://doi.org/10.1007/s10856-018-6061-5

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