Fabrication of alpha tricalcium phosphate by wet milling method
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Date
2016-06
Authors
Ahmad Ikmal Mohd Radzi
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Abstract
Wet milling method has been employed to fabricate α-TCP. Parameters varied in this experiment are milling time, sintering temperature, and soaking time. Precursor used in the synthesize process are calcium hydrogenphosphate dihydrate (CaHPO4.2H2O) and calcium carbonate (CaCO3) with molar ratio of 2:1 to obtain 1.5 Ca/P of initial ratio. Both material mixed and milled for 12 hours and 24 hours by using planetary mill. Particle Size Analyser (PSA) shows that particle size of mixture milled at 24 hours is finer and smaller than 12 hours mill which is 4.38μm rather than 11.9μm. The mixture was dried overnight at 80⁰C and powder form is obtained after crushing and grinding the dried mixture. Sample was pressed into cylinder block form and sintered at 1200⁰C and 1400⁰C with soaking time of 2 hours and 4 hours. All samples were quenched into room temperature to retain the polymorph of α-TCP. However, X-ray diffraction (XRD) analysis indicated that single phase β-TCP was obtained at 1200⁰C while α-TCP was obtained at 1400⁰C. Density-porosity measurement and diametral tensile strength (DTS) have been performed to study the mechanical properties of α-TCP. It is found that higher soaking time offered least porosity and contribute to higher strength of samples. Morphology of samples was observed by using scanning electron microscopy (SEM). SEM morphology shows that α-TCP block obtained from 24 hours milling time and sintered at 1400⁰C has a dense structure with minimum porosity of 2.71%.