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Thermal crystallization of amorphous calcium phosphate combined with citrate and fluoride doping: a novel route to produce hydroxyapatite bioceramics

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2021
Manuscript_revised.pdf (2.428Mb)
Authors
Degli Esposti, Lorenzo
Marković, Smilja
Ignjatović, Nenad
Panseri, Silvia
Montesi, Monica
Adamiano, Alessio
Fosca, Marco
Rau, Julietta V.
Uskoković, Vuk
Iafisco, Michele
Article (Accepted Version)
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Abstract
Amorphous calcium phosphate (ACP) is a material of high interest for dentistry, orthopedics, and other biomedical sectors. Being intrinsically metastable, the process of transformation of ACP into a crystalline phase upon heating is of high relevance for the development of innovative bioceramics. Here we have first studied the thermal behavior of a citrate-stabilized ACP (Cit-ACP) also doped with fluoride ions (Cit-FACP) prepared at three different nominal Cit/Ca ratios (i.e. 4, 2, 1) by differential thermal analysis. Next, the physico-chemical features of the crystalline products as well as the in vitro cell response to the materials were investigated. A citrate and fluoride free ACP sample was also tested as the blank. We have found that the activation energy of crystallization of Cit-(F)ACP samples is lower in comparison to the blank ACP and this is influenced by the nominal Cit/Ca molar ratio. Interestingly, we have discovered that the thermal treatment of Cit-(F)ACP at 800 °C yiel...ds hydroxyapatite (HA) or fluorapatite (FHA) as the main products differently from blank ACP that, like most of the ACPs reported in the literature, yields β-tricalcium phosphate. This was attributed to the Ca/P ratio of Cit-(F)ACP, which is similar to HA. A study of the crystalline products has revealed that all the (F)HA samples were non-cytotoxic, and retained carbonate ions in the crystal structure despite the heat treatment that should have induced decarbonation. The morphology of the products is influenced by the nominal Cit/Ca ratio and the presence of fluoride, ranging from spherical nanoparticles to micrometric hexagonal rods. Overall, our results prove that the thermal crystallization of Cit-(F)ACP is markedly different from classic ACP based materials and the thermal treatment of Cit-(F)ACP represents an attractive route for producing pure bioactive HA ceramics.

Keywords:
calcium phosphate / amorphous materials / doping / citrate / fluoride / hydroxyapatite / bioceramics
Source:
Journal of Materials Chemistry B, 2021, 9, 24, 4832-4845
Publisher:
  • Royal Society of Chemistry
Funding / projects:
  • Ministry of Health (Bando Ricerca Finalizzata 2016, no. GR-2016-02364704)
Note:
  • This is the peer-reviewed version of the article: Degli Esposti Lorenzo, Marković Smilja, Ignjatović Nenad, Panseri Silvia, Montesi Monica, Adamiano Alessio, Fosca Marco, Rau Julietta V., Uskoković Vuk, Iafisco Michele, "Thermal crystallization of amorphous calcium phosphate combined with citrate and fluoride doping: a novel route to produce hydroxyapatite bioceramics" Journal of Materials Chemistry B, 9, no. 24 (2021):4832-4845, https://doi.org/10.1039/D1TB00601K
  • Supplementary information: https://hdl.handle.net/21.15107/rcub_dais_11642
Related info:
  • Version of
    https://hdl.handle.net/21.15107/rcub_dais_11639
  • Version of
    http://dx.doi.org/10.1039/D1TB00601K
  • Referenced by
    https://hdl.handle.net/21.15107/rcub_dais_11642

DOI: 10.1039/D1TB00601K

ISSN: 2050-750X; 2050-7518

WoS: 000651135000001

[ Google Scholar ]
4
Handle
https://hdl.handle.net/21.15107/rcub_dais_11640
URI
https://dais.sanu.ac.rs/123456789/11640
Collections
  • ИТН САНУ - Општа колекција / ITS SASA - General collection
Institution/Community
Институт техничких наука САНУ / Institute of Technical Sciences of SASA
TY  - JOUR
AU  - Degli Esposti, Lorenzo
AU  - Marković, Smilja
AU  - Ignjatović, Nenad
AU  - Panseri, Silvia
AU  - Montesi, Monica
AU  - Adamiano, Alessio
AU  - Fosca, Marco
AU  - Rau, Julietta V.
AU  - Uskoković, Vuk
AU  - Iafisco, Michele
PY  - 2021
UR  - https://dais.sanu.ac.rs/123456789/11640
AB  - Amorphous calcium phosphate (ACP) is a material of high interest for dentistry, orthopedics, and other biomedical sectors. Being intrinsically metastable, the process of transformation of ACP into a crystalline phase upon heating is of high relevance for the development of innovative bioceramics. Here we have first studied the thermal behavior of a citrate-stabilized ACP (Cit-ACP) also doped with fluoride ions (Cit-FACP) prepared at three different nominal Cit/Ca ratios (i.e. 4, 2, 1) by differential thermal analysis. Next, the physico-chemical features of the crystalline products as well as the in vitro cell response to the materials were investigated. A citrate and fluoride free ACP sample was also tested as the blank. We have found that the activation energy of crystallization of Cit-(F)ACP samples is lower in comparison to the blank ACP and this is influenced by the nominal Cit/Ca molar ratio. Interestingly, we have discovered that the thermal treatment of Cit-(F)ACP at 800 °C yields hydroxyapatite (HA) or fluorapatite (FHA) as the main products differently from blank ACP that, like most of the ACPs reported in the literature, yields β-tricalcium phosphate. This was attributed to the Ca/P ratio of Cit-(F)ACP, which is similar to HA. A study of the crystalline products has revealed that all the (F)HA samples were non-cytotoxic, and retained carbonate ions in the crystal structure despite the heat treatment that should have induced decarbonation. The morphology of the products is influenced by the nominal Cit/Ca ratio and the presence of fluoride, ranging from spherical nanoparticles to micrometric hexagonal rods. Overall, our results prove that the thermal crystallization of Cit-(F)ACP is markedly different from classic ACP based materials and the thermal treatment of Cit-(F)ACP represents an attractive route for producing pure bioactive HA ceramics.
PB  - Royal Society of Chemistry
T2  - Journal of Materials Chemistry B
T1  - Thermal crystallization of amorphous calcium phosphate combined with citrate and fluoride doping: a novel route to produce hydroxyapatite bioceramics
SP  - 4832
EP  - 4845
VL  - 9
IS  - 24
DO  - 10.1039/D1TB00601K
UR  - https://hdl.handle.net/21.15107/rcub_dais_11640
ER  - 
@article{
author = "Degli Esposti, Lorenzo and Marković, Smilja and Ignjatović, Nenad and Panseri, Silvia and Montesi, Monica and Adamiano, Alessio and Fosca, Marco and Rau, Julietta V. and Uskoković, Vuk and Iafisco, Michele",
year = "2021",
abstract = "Amorphous calcium phosphate (ACP) is a material of high interest for dentistry, orthopedics, and other biomedical sectors. Being intrinsically metastable, the process of transformation of ACP into a crystalline phase upon heating is of high relevance for the development of innovative bioceramics. Here we have first studied the thermal behavior of a citrate-stabilized ACP (Cit-ACP) also doped with fluoride ions (Cit-FACP) prepared at three different nominal Cit/Ca ratios (i.e. 4, 2, 1) by differential thermal analysis. Next, the physico-chemical features of the crystalline products as well as the in vitro cell response to the materials were investigated. A citrate and fluoride free ACP sample was also tested as the blank. We have found that the activation energy of crystallization of Cit-(F)ACP samples is lower in comparison to the blank ACP and this is influenced by the nominal Cit/Ca molar ratio. Interestingly, we have discovered that the thermal treatment of Cit-(F)ACP at 800 °C yields hydroxyapatite (HA) or fluorapatite (FHA) as the main products differently from blank ACP that, like most of the ACPs reported in the literature, yields β-tricalcium phosphate. This was attributed to the Ca/P ratio of Cit-(F)ACP, which is similar to HA. A study of the crystalline products has revealed that all the (F)HA samples were non-cytotoxic, and retained carbonate ions in the crystal structure despite the heat treatment that should have induced decarbonation. The morphology of the products is influenced by the nominal Cit/Ca ratio and the presence of fluoride, ranging from spherical nanoparticles to micrometric hexagonal rods. Overall, our results prove that the thermal crystallization of Cit-(F)ACP is markedly different from classic ACP based materials and the thermal treatment of Cit-(F)ACP represents an attractive route for producing pure bioactive HA ceramics.",
publisher = "Royal Society of Chemistry",
journal = "Journal of Materials Chemistry B",
title = "Thermal crystallization of amorphous calcium phosphate combined with citrate and fluoride doping: a novel route to produce hydroxyapatite bioceramics",
pages = "4832-4845",
volume = "9",
number = "24",
doi = "10.1039/D1TB00601K",
url = "https://hdl.handle.net/21.15107/rcub_dais_11640"
}
Degli Esposti, L., Marković, S., Ignjatović, N., Panseri, S., Montesi, M., Adamiano, A., Fosca, M., Rau, J. V., Uskoković, V.,& Iafisco, M.. (2021). Thermal crystallization of amorphous calcium phosphate combined with citrate and fluoride doping: a novel route to produce hydroxyapatite bioceramics. in Journal of Materials Chemistry B
Royal Society of Chemistry., 9(24), 4832-4845.
https://doi.org/10.1039/D1TB00601K
https://hdl.handle.net/21.15107/rcub_dais_11640
Degli Esposti L, Marković S, Ignjatović N, Panseri S, Montesi M, Adamiano A, Fosca M, Rau JV, Uskoković V, Iafisco M. Thermal crystallization of amorphous calcium phosphate combined with citrate and fluoride doping: a novel route to produce hydroxyapatite bioceramics. in Journal of Materials Chemistry B. 2021;9(24):4832-4845.
doi:10.1039/D1TB00601K
https://hdl.handle.net/21.15107/rcub_dais_11640 .
Degli Esposti, Lorenzo, Marković, Smilja, Ignjatović, Nenad, Panseri, Silvia, Montesi, Monica, Adamiano, Alessio, Fosca, Marco, Rau, Julietta V., Uskoković, Vuk, Iafisco, Michele, "Thermal crystallization of amorphous calcium phosphate combined with citrate and fluoride doping: a novel route to produce hydroxyapatite bioceramics" in Journal of Materials Chemistry B, 9, no. 24 (2021):4832-4845,
https://doi.org/10.1039/D1TB00601K .,
https://hdl.handle.net/21.15107/rcub_dais_11640 .

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