Parameters affecting the synthesis of β-tricalcium phosphate powder using a wet precipitation method
DOI:
https://doi.org/10.15282/jmes.11.4.2017.22.0288Keywords:
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 500oC-1300oC 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.
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