Transformations in Sol-Gel Synthesized Nanoscale Hydroxyapatite Calcined Under Different Temperatures and Time Conditions

Abstract

Nano-hydroxyapatite (HAP) has been synthesized using sol-gel technique. Calcium nitrate tetrahydrate and potassium dihydrogen phosphate were used as precursors for calcium and phosphorus, respectively. A detailed study on its transformation during calcination at two crucial temperatures has been undertaken. The synthesized nanopowder was calcined at 600 and 800 °C for different time periods. The results revealed that the obtained powders after calcining at 600 and 800 °C are composed of hydroxyapatite nanoparticles. The nano-HAP powders were characterized by x-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy, thermal gravimetric analysis (TGA), and BET surface area analyzer techniques. The results indicate that crystallite size as well as crystallinity of synthesized HAP nanopowders increase with increase in calcination temperature as well as calcination time, but the effect of temperature is more prominent as compared to that of calcination time. TEM micrograph revealed the presence of majority of HAP powder particles as agglomerates and a few as individual particles. It also revealed that HAP produced after sintering at 600 °C is 26-45 nm in size, which is well in agreement with the crystallite size calculated using XRD data. TGA study showed the thermal stability of the as-synthesized nano-HAP powder. The BET surface area decreased with increase in calcination temperature and time. The results clearly demonstrate the significant role of calcination parameters on the characteristics of nano-HAP powders.