A comparison of pretreatments on hydroxyapatite formation on Ti by biomimetic method

Abstract

In this study, hydroxyapatite coating on titanium material substrate was successfully performed by using biomimetic method. Titanium plates immersed in 1.5 SBF at pH 7.4 and 37 °C were analyzed at the end of the first, second, and fourth weeks. At the end of the first week, the immersion process was continued with the sample exposed to the optimum selected surface pretreatment. Three different treatments have been applied to determine the optimum surface treatment: each substrate immersed into NaOH, HCl, and NaOH + HCl solutions before heat treatment at 600 °C for 1 h and immersed in NaOH solution was selected the optimum surface treatment. The presence of biphasic hydroxyapatite (HA, Ca5(PO4)3(OH)) and tricalcium phosphate (TCP, Ca3(PO4)2) on Ti surfaces were confirmed by XRD. SEM studies showed that denser HA coating which have nano-sphere-like morphology formed on Ti pretreated with NaOH solution at the end of first week than other hydroxyapatite (HA)-coated Ti pretreated with NaCl and NaOH + NaCl solutions and coating thickness increased by increasing immersion time. The HA coating thickness of the samples immersed in optimum pretreatment solution was found as 178 and 340 μm for at the end of second and fourth weeks, respectively. The particle size analysis of the biphasic HA powders scraped from the coating layer on the substrate before and after sintering was carried out by Zetasizer and it showed that HA powders have 0.58 μm average particle size and their particle size distribution has less dimensional dispersion after sintering. Energy-dispersive X-ray spectroscopy (EDS) analysis revealed that the Ca/P ratio in HA powders was near to 1.5. Raman and Fourier transform-infrared spectroscopy (FTIR) results combined with the X-ray diffraction (XRD) indicated the presence of biphasic hydroxyapatite after biomimetic coating process and increment in crystallinity of the powders after sintering. It was found that HA nucleation on Ti pretreated with NaOH solution was higher than Ti pretreated with other solutions which is confirmed by electrochemical impedance spectroscopy (EIS).