Structure reinforcement of porous hydroxyapatite pellets using sodium carbonate as sintering aid: Microstructure, secondary phases and mechanical properties

Abstract

Porous HAP pellets suitable for loading therapeutic agents were prepared using microcrystalline cellulose (MCC) as pore former and sodium carbonate as sintering aid (SAID). The effect of sintering temperature on the microstructure, mechanical properties and disintegration of pellets prepared at different SAID content was studied. Pellets were characterized by SEM, image analysis, porosimetry and surface area. Secondary phases were identified by PXRD, ATR-FTIR and Raman spectroscopy. Increasing the sintering temperature decreased the diameter, porosity, surface area and friability of the pellets but increased the pore size, tensile strength and disintegration time. The effect of SAID was dependent on sintering temperature. With 5% SAID, a secondary β-tricalcium phosphate (β-TCP) phase was formed, indicated by FTIR peak at 980 cm−1 and characteristic PXRD reflections, whereas with 10%, a secondary B-type carbonated hydroxyapatite phase (CHA) formed, indicated by FTIR peaks at 878 and 1450 cm−1, a broad Raman peak in the region 1020 to 1050 cm−1 and PXRD reflections. Pellets prepared with SAID showed high strength and also porosity. The biphasic HAP/β-TCP pellets exhibited remarkably great strength (4.39 MPa) at the high sintering temperature, while still retaining 43.9% porosity. Relationships were established between the mechanical properties or disintegration time of the porous pellets and the microstructural parameters.