In situ study of hydroxyapatite from cattle during a controlled calcination process using HT-XRD

In situ High-Temperature X-ray diffraction (HT-XRD) from 400 to 900 °C was carried out to obtain patterns of bio hydroxyapatite every 20 °C during calcination processes at heating rates of 3, 6, and 9 °C/min to determine changes in its structural parameters as well as in its thermal expansion coefficient (TEC) for a and c lattice parameters. Additionally, High-Resolution Transmission Electron microscopy (HR-TEM) demonstrates that this HAp has an ordered nano like plate crystalline structure. The raw sample exhibits broad X-ray peaks originated by its nano size, and after calcination at about 700 °C, these become narrowed due to crystal growth. The calculation of the TEC as a function of the temperature for this hydroxyapatite shows a nonlinear increment for the a and c lattice parameters. Lattice thermal expansion occurs as water and organic matter are lost as the coalescence of HAp crystals take place; furthermore, as the heating rate increases, so does the lattice volume. Thermal analyses confirm that crystal growth is a process that starts after the bone sample has lost all its organic material and then bio-hydroxyapatite size changes from nano to micro-scale. A simulation using the PDF-4 software confirmed the nanometric size of the hydroxyapatite.