Synthesis of calcium phosphate-based composite nanopowders by mechanochemical process and subsequent thermal treatment

One-step mechanochemical process followed by thermal treatment has been used to produce calcium phosphate-based composite nanopowders. Effects of milling and subsequent heat treatment on the phase transition as well as structural features were investigated. The products were characterized by powder X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and transmission electron microscopy (TEM) techniques. The results revealed that the dominant phases after mechanical activation were hydroxyapatite, anatase (TiO₂), and periclase (MgO), while after thermal annealing process at 700 °C hydroxyapatite along with geikielite (MgTiO₃) and periclase (MgO) were the major phases. In addition, decomposition of hydroxyapatite to tricalcium phosphate (β-TCP) occurred after heat treatment in the range 900–1100 °C which resulted in the formation of tricalcium phosphate-based composite nanopowders. Evaluation of structural features of the samples calculated by X-ray diffraction profiles analysis indicated that the average crystallite size of hydroxyapatite after 10 h of milling and subsequent heat treatment at 700 °C were about 21 and 34 nm, respectively. TEM and SEM studies exhibited that the considerable morphological changes at temperatures ≥900 °C had to be ascribed not only to grain growth, but also for the transformation of hydroxyapatite to β-TCP.