Synthesis and characterization of pure and nanosized hydroxyapatite bioceramics

Synthetic nanosized hydroxyapatite (HA) particles (<120 nm) were prepared using a co-precipitation technique by adopting two different routes - one from an aqueous solution of calcium nitrate tetrahydrate and diammonium hydrogen phosphate at pH 10 and the other by using calcium hydroxide and phosphoric acid as precursors at pH 8.5 and reaction temperature of 50 degrees C. The lattice parameters of HA nanopowder were analogous to reference [Joint Committee on Powdered Diffraction Standards (JCPDS)] pattern no. 09-432. No decomposition of HA into other phases was observed even after heating at 1000 degrees C in air for 1 h. This observation revealed the high-temperature stability of the HA nanopowder obtained using co-precipitation route. The effects of preliminary Ca/P molar ratio, precipitation, pH and temperature on the evolution of phase and crystallinity of the nanopowder were systematically examined and optimized. The product was evaluated by techniques such as X-ray-diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) and Raman spectroscopy analyses. The chemical structural analysis of the as-prepared HA sample was performed using X-ray photoelectron spectroscopy (XPS). After heat treatment at 1000 degrees C for 1 h and ageing for 15 h, the product was obtained as a phase- pure, highly crystalline HA nanorods.