Characterization of hydroxyapatite powders prepared by ultrasonic spray-pyrolysis technique

Abstract

The hydroxyapatite (HAp) powder was prepared by the ultrasonic spray-pyrolysis technique; the characterization of the resulting powders was performed. Five kinds of the starting solutions with the Ca/P ratio of 1.67 were prepared by mixing Ca(NO₃)₂, (NH₄)₂HPO₄ and HNO₃; the concentrations of Ca²⁺ and PO₄ ³⁻ were in the ranges of 0.10 to 0.90 mol · dm⁻³ and 0.06 to 0.54 mol · dm⁻³, respectively. These solutions were sprayed into the heating zone to prepare the HAp powders. The heating zone was composed of two electric furnaces; the lower furnace was used for the evaporation of the solvent from the droplets (300–500°C) and the upper furnace for the pyrolysis of the precipitated metal salts (750–900°C). The easily sinterable HAp powder was prepared by spray-pyrolysing the solution with Ca²⁺ (0.50 mol · dm⁻³) and PO₄ ³⁻ (0.30 mol · dm⁻³) at the temperatures of 800°C (the upper furnaces) and 400°C (the lower furnaces). The resulting powder was composed of the spherical particles with diameters of ∼1 μm or below. Even without the calcination and grinding operations, the relative densities of the compacts fired at 1150 and 1200°C for 5 h attained maxima ∼95%. The microstructure of the sintered compacts appeared to be uniform; the average grain size was ∼3 μm. The activation energies for the grain growth of the sintered HAp compacts were 120 to 147 kJ · mol⁻¹ · K⁻¹.