Effects of Temperature on the Physicochemical Properties of Bioinspired, Synthetic, and Biogenic Hydroxyapatites Calcinated under the Same Thermal Conditions

Abstract

The paper studies the changes in physicochemical properties of three types of hydroxyapatite (HAp): HAp-HB (from bovine sources), HAp-SC (chemically synthesized), and bioinspired HAp-SE (synthesized using eggshells) calcined under identical thermally controlled conditions from room temperature to 400, 500, 600, 650, 680, 700, 720, 750, 800, and 900 °C in furnace air. The thermogravimetric analysis (TGA) indicated distinct thermal transitions and coalescence phenomena at different temperatures for these samples due to their sources and mineral composition differences. Inductively coupled plasma (ICP) showed that HAp-H (human), HAp-HB (bovine), and HAp-SE (bioinspired) have similar Ca, P, and Mg contents. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) revealed that the coalescence phenomena increased in the crystallite size as the temperature increased. X-Ray diffraction (XRD) patterns revealed partial phase changes in the bioinspired sample (HAp-SE) and crystallite growth in all samples, resulting in full width at the half maximum (FWHM) and peak position alterations. Fourier-transform infrared spectroscopy (FTIR) showed that HAp-SE exhibited a partial phase change due to dehydroxylation and the presence of functional groups (PO43−, OH, and CO32−) with varying vibrational modes influenced by the obtained method and calcination temperature. Raman spectra of the HAp-SE samples exhibited fluorescence at 400 °C and revealed vibrational modes of surface P-O. It observed the bands of the internal phosphates of the crystal lattice and shifts in the band positions at higher temperatures indicated phosphorus interacting with carbon and oxygen, triggering dehydroxylation.