Parameters affecting the synthesis of β-tricalcium phosphate powder using a wet precipitation method

R. Othman; Z. Mustafa; P.T. Kien; N.F. Ishak; A. Shaaban; A.F. Mohd Noor

doi:10.15282/jmes.11.4.2017.22.0288

Authors

R. Othman Advanced Manufacturing Centre, Faculty of Manufacturing Engineering, Universiti Teknikal Malaysia Melaka, 76100 Durian Tunggal, Malacca, Malaysia
Z. Mustafa Advanced Manufacturing Centre, Faculty of Manufacturing Engineering, Universiti Teknikal Malaysia Melaka, 76100 Durian Tunggal, Malacca, Malaysia
P.T. Kien School of Materials & Mineral Resources Engineering, Universiti Sains Malaysia, Engineering Campus, 14300 Nibong Tebal, Penang, Malaysia
N.F. Ishak Advanced Manufacturing Centre, Faculty of Manufacturing Engineering, Universiti Teknikal Malaysia Melaka, 76100 Durian Tunggal, Malacca, Malaysia
A. Shaaban School of Materials & Mineral Resources Engineering, Universiti Sains Malaysia, Engineering Campus, 14300 Nibong Tebal, Penang, Malaysia
A.F. Mohd Noor School of Materials & Mineral Resources Engineering, Universiti Sains Malaysia, Engineering Campus, 14300 Nibong Tebal, Penang, Malaysia

DOI:

https://doi.org/10.15282/jmes.11.4.2017.22.0288

Keywords:

Hydroxyapatite; monetite; tricalcium phosphate; calcination.

Abstract

In this work, precursor materials that are normally used to directly synthesise hydroxyapatite (HA) were adopted to obtain tricalcium phosphate (TCP). Calcium hydroxide, (Ca(OH)₂), and phosphoric acid, (H₃PO₄), with a Ca/P ratio of 1.5, were mixed as the precursor materials. The mixture was stirred at various stirring speeds ranging from 0 to 400 rpm, over a range of stirring durations of 1 to 4 hours. Upon completion of the reaction, the as-prepared powders were calcined at different temperatures ranging from 500^oC-1300^oC for a soaking duration that was varied between 1-4 hours. Differential scanning calorimetry (DSC) and thermogravimetry (TG) were used for thermal analyses to ascertain the calcination temperatures, whilst x-ray diffraction (XRD) was utilised to determine the phases formed before and after calcination. Field emission scanning electron microscopy (FESEM) was used to monitor the morphological changes at different calcination temperatures. Based on the XRD results, the phases formed were dependent on the processing parameters employed. This work has successfully ascertained that the most optimum parameters to synthesise singlephase β-TCP are a stirring speed of 200 rpm, a calcination temperature of 900°C, a calcination soaking duration of 2 hours and a mixing duration of 1 hour. Microstructural observation conducted on the β-TCP powders obtained at calcination temperatures of 900°C to 1300°C showed an aggregated structure of particles with massive grain growth as the temperature was raised up to 1300 °C.

References

Šupová M. Substituted hydroxyapatites for biomedical applications: A review. Ceramics International. 2015;41:9203-31.

Dorozhkin SV. Calcium orthophosphate bioceramics. Ceramics International. 2015;41:13913-66.

Lee S-J, Yoon Y-S, Lee M-H, Oh N-S. Highly sinterable β-tricalcium phosphate synthesized from eggshells. Materials Letters. 2007;61:1279-82.

Choi D, Kumta PN. Mechano-chemical synthesis and characterization of nanostructured β-TCP powder. Materials Science and Engineering: C. 2007;27:377-81.

Yoshida K, Kobayashi M, Hyuga H, Kondo N, Kita H, Hashimoto K, et al. Reaction sintering of β-tricalcium phosphates and their mechanical properties. Journal of the European Ceramic Society. 2007;27:3215-20.

Koç N, Timuçin M, Korkusuz F. Fabrication and characterization of porous tricalcium phosphate ceramics. Ceramics International. 2004;30:205-11.

Valletregi M. Synthesis of ?-tricalcium phosphate in layered or powdered forms for biomedical applications. Solid State Ionics. 2004;172:445-9.

Zou C, Weng W, Deng X, Cheng K, Liu X, Du P, et al. Preparation and characterization of porous -tricalcium phosphate/collagen composites with an integrated structure. Biomaterials. 2005;26:5276-84.

Kwon S-H, Jun Y-K, Hong S-H, Kim H-E. Synthesis and dissolution behavior of β-TCP and HA/β-TCP composite powders. Journal of the European Ceramic Society. 2003;23:1039-45.

Cheang P, Khor KA. Thermal spraying of hydroxyapatite (HA) coatings: Effects of powder feedstock. Journal of Materials Processing Technology. 1995;48:429-36.

Afshar A, Ghorbani M, Ehsani N, Saeri MR, Sorrell CC. Some important factors in the wet precipitation process of hydroxyapatite. Materials & Design. 2003;24:197-202.

Saeri MR, Afshar A, Ghorbani M, Ehsani N, Sorrell CC. The wet precipitation process of hydroxyapatite. Materials Letters. 2003;57:4064-9.

Nagai H, Nishimura Y. Hydroxyapatite, ceramic material and process for preparing thereof: Google Patents; 1985.

Schmidt PC, Herzog R. Calcium phosphates in pharmaceutical tableting: 1. Physico-pharmaceutical properties. Pharmacy World & Science. 1993;15:105-15.

Feng W, Mu-sen L, Yu-peng L, Yong-xin Q. A simple sol–gel technique for preparing hydroxyapatite nanopowders. Materials Letters. 2005;59:916-9.

Xiao XF, Liu RF, Zheng YZ. Characterization of hydroxyapatite/titania composite coatings codeposited by a hydrothermal–electrochemical method on titanium. Surface and Coatings Technology. 2006;200:4406-13.

Kalita SJ, Bhardwaj A, Bhatt HA. Nanocrystalline calcium phosphate ceramics in biomedical engineering. Materials Science and Engineering: C. 2007;27:441-9.

Monma H, Goto M. Behavior of the alpha - beta phase transformation in tricalcium phosphate. Journal of the Ceramic Association, Japan. 1983;91:473-5.

Champion E. Sintering of calcium phosphate bioceramics. Acta Biomaterialia. 2013;9:5855-75.

Nikaido T, Tsuru K, Munar M, Maruta M, Matsuya S, Nakamura S, et al. Fabrication of β-TCP foam: Effects of magnesium oxide as phase stabilizer on its properties. Ceramics International. 2015;41:14245-50.

Li HC, Wang DG, Chen CZ, Weng F, Shi H. Influence of different amount of Na 2 O additive on the structure, mechanical properties and degradability of bioactive wollastonite. Ceramics International. 2016;42:1439-45.

Latifi SM, Fathi M, Varshosaz J, Ghochaghi N. Simultaneous structural and surface modifications of nanophase hydroxyapatite for improving its dissolution and bioactivity. Ceramics International. 2016;42:6355-9.