Abstract
The synthesis of calcium hydroxyapatite powder (Ca-HA) from orthophosphoric acid or from potassium dihydrogen orthophosphate and calcium carbonate was carried out under moderate conditions. A better dissolution of calcium carbonate and a complete precipitation of the orthophosphate species were obtained with orthophosphoric acid, indicating that it may be of interest as a phosphate source compared with potassium dihydrogen orthophosphate. The influence of calcination treatment on the physico-chemical properties of the solids is discussed in this paper. Different characterization techniques such as specific surface area (S BET), true density, particle size distribution, thermo-mechanical analysis, simultaneous thermogravimetry and differential scanning calorimetry analysis, X-ray diffraction and infrared were performed to understand the phase changes during thermal treatment. Specific surface area decreased while true density and particle size increased with the rise in the calcination temperature, due to the sintering of particles and the chemical reactions occurring at high temperatures. Mixtures of well-crystallized Ca-HA and tricalcium phosphate (TCP) or well-crystallized Ca-HA, CaO, and TCP were obtained after calcination at 800–1,000 °C of the solid products starting from orthophosphoric acid or potassium dihydrogen orthophosphate, respectively.
Similar content being viewed by others
References
Habraken WJEM, Wolke JGC, Jansen JA. Ceramic composites as matrices and scaffolds for drug delivery in tissue engineering. Adv Drug Deliv Rev. 2007;59:234–48.
Saha SK, Banerjee A, Banerjee S, Bose S. Synthesis of nanocrystalline hydroxyapatite using surfactant template systems: role of templates in controlling morphology. Mater Sci Eng C. 2009;29:2294–301.
Baillez S, Nzihou A, Bernache-Assolant D, Champion E, Sharrock P. Removal of aqueous lead ions by hydroxyapatites: equilibria and kinetic processes. J Hazard Mater. 2007;A139:443–6.
Bianco A, Cacciotti I, Lombardi M, Montanaro L, Gusmano G. Thermal stability and sintering behaviour of hydroxyapatite nanopowders. J Therm Anal Calorim. 2007;88:237–43.
De Campos M, Muller FA, Bressiani AHA, Bressiani JC, Greil P. Sonochemical synthesis of calcium phosphate powders. J Mater Sci Mater Med. 2007;18:669–75.
Zyman ZZ, Tkachenko MV, Polevodin DV. Preparation and characterization of biphasic calcium phosphate ceramics of desired composition. J Mater Sci Mater Med. 2008;19:2819–25.
Saeki T. A new type of CO2 gas sensor comprising porous hydroxyapatite ceramics. Sens Actuators. 1998;15:145–51.
Boukha Z, Kacimi M, Pereira MFR, Faria JL, Figueiredo JL, Ziyad M. Methane dry reforming on Ni loaded hydroxyapatite and fluoroapatite. Appl Catal A. 2007;317:299–309.
Khachani M, Kacimi M, Ensuque A, Piquemal JY, Connan C, Bozon-Verduraz F, Ziyad M. Iron–calcium–hydroxyapatite catalysts: iron speciation and comparative performances in butan-2-ol conversion and propane oxidative dehydrogenation. Appl Catal A. 2010;388:113–23.
Pham Minh D, Sebei H, Nzihou A, Sharrock P. Apatitic calcium phosphates: synthesis, characterization and reactivity in the removal of lead(II) from aqueous solution. Chem Eng J. 2012;198–199:180–90.
Kim DW, Cho IS, Kim JY, Jang HL, Han GS, Ryu HS, Shin H, Jung HS, Kim H, Hong KS. Simple large-scale synthesis of hydroxyapatite nanoparticles: in situ observation of crystallization process. Langmuir. 2010;26:384–8.
Elliott JC. Structure and chemistry of the apatites and other calcium orthophosphates. In: Studies in inorganic chemistry, vol 18. Amsterdam: Elsevier; 1994.
El Feki H, Khattech I, Jemal M, Rey C. Décomposition thermique d’hydroxyapatites carbonatées sodées. Thermochim Acta. 1994;237:99–110.
Tônsuaadu K, Peld M, Leskela T, Mannonen R, Niinisto L, Veiderma M. A thermoanalytical study of synthetic carbonate-containing apatites. Thermochim Acta. 1995;256:55–65.
Wilson RM, Elliott JC, Dowker SEP, Smith RI. Rietveld structure refinement of precipitated carbonate apatite using neutron diffraction data. Biomaterials. 2004;25:2205–13.
Yao F, LeGeros JP, LeGeros RZ. Simultaneous incorporation of carbonate and fluoride in synthetic apatites: effect on crystallographic and physico-chemical properties. Acta Biomater. 2009;5:2169–77.
Landin M, Rowe RC, York P. Particle size effects on the dehydration of dicalcium phosphate dihydrate powders. Int J Pharm. 1994;104:271–5.
Yoğurtcuoğlu E, Uçurum M. Surface modification of calcite by wet-stirred ball milling and its properties. Powder Technol. 2011;214:47–53.
Vagenas NV, Gatsouli A, Kontoyannis CG. Quantitative analysis of synthetic calcium carbonate polymorphs using FT-IR spectroscopy. Talanta. 2003;59:831–6.
Gunasekaran S, Anbalagan G. Spectroscopic study of phase transitions in natural calcite mineral. Spectrochim Acta. 2008;A69:1246–51.
Karlinsey RL, Mackey AC, Walker ER, Frederick KE. Preparation, characterization and in vitro efficacy of an acid-modified β-TCP material for dental hard-tissue remineralization. Acta Biomater. 2010;6:969–78.
Coelho PG, Coimbra ME, Ribeiro C, Fancio E, Higa O, Suzuki M, Marincola M. Physico/chemical characterization and preliminary human histology assessment of a β-TCP particulate material for bone augmentation. Mater Sci Eng C. 2009;29:2085–91.
Koumoulidis GC, Trapalis CC, Vaimakis TC. Sintering of hydroxyapatite lath-like powders. J Therm Anal Calorim. 2006;84:165–74.
Bailliez S, Nzihou A. The kinetics of surface area reduction during isothermal sintering of hydroxyapatite adsorbent. Chem Eng J. 2004;98:141–52.
Arifuzzaman SM, Rohani S. Experimental study of brushite precipitation. J Cryst Growth. 2004;267:624–34.
Stulajterova R, Medvecky L. Effect of calcium ions on transformation brushite to hydroxyapatite in aqueous solutions. Colloids Surf A. 2008;316:104–9.
Jinawath S, Sujaridworakun P. Fabrication of porous calcium phosphates. Mater Sci Eng C. 2002;22:41–6.
Frost RL, Palmer SJ. Thermal stability of the ‘cave’ mineral brushite CaHPO4·2H2O—mechanism of formation and decomposition. Thermochim Acta. 2011;521:14–7.
Mitsionis AI, Vaimakis TC. A calorimetric study of the temperature effect on calcium phosphate precipitation. J Therm Anal Calorim. 2010;99:785–9.
Zawrah MF, Shaw L. Liquid-phase sintering of SiC in presence of CaO. Ceram Int. 2004;30:721–5.
Acknowledgements
The authors gratefully acknowledge the support from Dr. Nathalie Lyczko, Mr. Philippe Accart, Mr. Denis Marty, and Ms. Christine Rolland at the centre RAPSODEE for different measurements.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Pham Minh, D., Galera Martínez, M., Nzihou, A. et al. Thermal behavior of apatitic calcium phosphates synthesized from calcium carbonate and orthophosphoric acid or potassium dihydrogen orthophosphate. J Therm Anal Calorim 112, 1145–1155 (2013). https://doi.org/10.1007/s10973-012-2695-6
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10973-012-2695-6