Novel route for rapid sol-gel synthesis of hydroxyapatite, avoiding ageing and using fast drying with a 50-fold to 200-fold reduction in process time

• DOI: 10.1016/j.msec.2016.09.054
• Publication Date: 2016-09-30T20:19:15Z
• Authors: Basam A.E. Ben-Arfa; Isabel M. Miranda...; José M.F. Ferreira; Robert C. Pullar
• Keywords: Durapatite; Time Factors; X-Ray Diffraction; Materials Testing; Spectroscopy, Fourier Transform Infrared; Microscopy, Electron, Scanning; Biocompatibility; Hydroxyapatite; Nano-synthesis; Nanoparticles; Sol-gel; β-TCP; Durapatite; Materials Testing; Microscopy, Electron, Scanning; Powders; Spectroscopy, Fourier Transform Infrared; Time Factors; X-Ray Diffraction; Desiccation; 02 engineering and technology; Desiccation; Powders; 0210 nano-technology

We have developed an innovative, rapid sol-gel method of producing hydroxyapatite nanopowders that avoids the conventional lengthy ageing and drying processes (over a week), being 200 times quicker in comparison to conventional aqueous sol-gel preparation, and 50 times quicker than ethanol based sol-gel synthesis. Two different sets of experimental conditions, in terms of pH value (5.5 and 7.5), synthesis temperature (45 and 90°C), drying temperature (60 and 80°C) and calcination temperature (400 and 700°C) were explored. The products were characterised by X-ray diffraction (XRD) Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and specific surface area (SSA) measurements. Pure hydroxyapatite (Ca10(PO4)6(OH)2, HAp) was obtained for the powders synthesised at pH7.5 and calcined at 400°C, while biphasic mixtures of HAp/β-tricalcium phosphate (β-Ca3(PO4)2, TCP) were produced at pH5.5 and (pH7.5 at elevated temperature). The novel rapid drying was up to 200 times faster than conventional drying, only needing 1h with no prior ageing step, and favoured the formation of smaller/finer nanopowders, while producing pure HAp or phase mixtures virtually identical to those obtained from the slow conventional drying method, despite the absence of a slow ageing process. The products of this novel rapid process were actually shown to have smaller crystallite sizes and larger SSA, which should result in increased bioactivity.