A comparison of pretreatments on hydroxyapatite formation on Ti by biomimetic method
- 45 Downloads
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).
KeywordsBiomaterials Hydroxyapatite Titanium Biomimetic coating Simulated body fluid
This work was supported by the Scientific Research Projects Commission of Sakarya University (Project number: 2016-01-08-051). The authors express their thanks to Rectorate of Sakarya University for providing financial support. The authors also thank to experts Fuat Kayis and Murat Kazanci for performing XRD and SEM-EDS studies and special appreciation are extended to technicians Ersan Demir and Erkut Taş of Sakarya University for assisting with experimental studies.
- 1.I.V. Pylypchuk, P.P. Gorbyk, A.L. Petranovska, O.M. Korduban, P.E. Markovsky, O.M. Ivasyshyn, Formation of biomimetic hydroxyapatite coatings on the surface of titanium and Ti-containing alloys: Ti-6Al-4V and Ti-Zr-Nb, In: Grumezescu, A. (ed.) Surf. Chem. Nanobiomaterials Appl. Nanobiomaterials, William Andrew, 2016: pp. 193–229. doi: https://doi.org/10.1016/B978-0-323-42861-3.00007-8
- 4.Jensen, S.S., Yeo, A., Dard, M., Hunziker, E., Schenk, R., Buser, D.: Evaluation of a novel biphasic calcium phosphate in standardized bone defects. A histologic and histomorphometric study in the mandibles of minipigs. Clin Oral Implants Res. 18, 752–760 (2007). https://doi.org/10.1111/j.1600-0501.2007.01417.x CrossRefGoogle Scholar
- 5.Arts, J.J.C., Walschot, L.H.B., Verdonschot, N., Schreurs, B.W., Buma, P.: Biological activity of tri-calciumphosphate/hydroxyl-apatite granules mixed with impacted morsellized bone graft. A study in rabbits. J. Biomed. Mater. Res. - Part B Appl. Biomater. 81, 476–485 (2007). https://doi.org/10.1002/jbm.b.30687 CrossRefGoogle Scholar
- 6.Ben-Arfa Basam, A.E., Salvado, I.M.M., Ferreira, J.M.F., Pullar, R.C.: 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. Mater. Sci. Eng. C. 70, 796–804 (2016). https://doi.org/10.1016/j.msec.2016.09.054 CrossRefGoogle Scholar
- 8.Descamps, M., Boilet, L., Moreau, G., Tricoteaux, A., Lu, J., Leriche, A., Lardot, V., Cambier, F.: Processing and properties of biphasic calcium phosphates bioceramics obtained by pressureless sintering and hot isostatic pressing. J Eur Ceram Soc. 33, 1263–1270 (2013). https://doi.org/10.1016/j.jeurceramsoc.2012.12.020 CrossRefGoogle Scholar
- 9.Mohammed, H.I., Abdel-Fattah, W.I., El-Sayed, E.S.M., Talaat, M.S., Sallam, A.S.M., Faerber, J., Pourroy, G., Roland, T., Carradò, A.: Influence of heat treatment on Ti6Al4V for biomimetic biolayer. Bioinspired, Biomim Nanobiomaterials. 1, 173–182 (2012). https://doi.org/10.1680/bbn.12.00003 CrossRefGoogle Scholar
- 12.Bracci, B., Torricelli, P., Panzavolta, S., Boanini, E., Giardino, R., Bigi, A.: Effect of Mg2+, Sr2+, and Mn2+ on the chemico-physical and in vitro biological properties of calcium phosphate biomimetic coatings. J Inorg Biochem. 103, 1666–1674 (2009). https://doi.org/10.1016/j.jinorgbio.2009.09.009 CrossRefGoogle Scholar
- 14.Bigi, A., Fini, M., Bracci, B., Boanini, E., Torricelli, P., Giavaresi, G., Aldini, N.N., Facchini, A., Sbaiz, F., Giardino, R.: The response of bone to nanocrystalline hydroxyapatite-coated Ti13Nb11Zr alloy in an animal model. Biomaterials. 29, 1730–1736 (2008). https://doi.org/10.1016/j.biomaterials.2007.12.011 CrossRefGoogle Scholar
- 16.Kokubo, T., Takadama, H.: How useful is SBF in predicting in vivo bone bioactivity? Biomaterials. 27, 2907–2915 (2006). https://doi.org/10.1016/j.biomaterials.2006.01.017 CrossRefGoogle Scholar
- 25.Lukić, M., Stojanović, Z., Škapin, S.D., Maček-Kržmanc, M., Mitrić, M., Marković, S., Uskoković, D.: Dense fine-grained biphasic calcium phosphate (BCP) bioceramics designed by two-step sintering. J Eur Ceram Soc. 31, 19–27 (2011). https://doi.org/10.1016/j.jeurceramsoc.2010.09.006 CrossRefGoogle Scholar
- 29.Harris, J., Mey, I., Hajir, M., Mondeshki, M., Wolf, S.E.: Pseudomorphic transformation of amorphous calcium carbonate films follows spherulitic growth mechanisms and can give rise to crystal lattice tilting. CrystEngComm. 17, 6831–6837 (2015). https://doi.org/10.1039/C5CE00441A CrossRefGoogle Scholar