Characterization of Apatite Glass-Ceramic Coatings on Ti-6Al-4V Substrate by Sol-Gel Method for Medical Application

Document Type : Original Articles


1 Ferdowsi university of mashhad

2 par-e-tavous


A single- and double-layer apatite-anorthite glass-ceramic coating was produced by dip coating sol-gel method on Ti-6Al-4V substrate. Heat treatment was performed at 800­°C. DTA analysis was performed to determine the appropriate heat treatment temperatures. XRD analysis confirmed the intended crystalline compounds; and the morphology of the coated layer was investigated using a SEM. Hardness and roughness of each layer was measured by micro hardness test and AFM, respectively. SEM micrographs confirm the adhesion and uniformity of the first apatite layer. Micro hardness of the second (top) layer showed an increase compared to the first layer. The roughness of the coatings is in the appropriate limit for dental applications.


. Jun S.-H., et al., "A bioactive coating of a silica xerogel/chitosan hybrid on titanium by a room temperature sol–gel process", Acta Biomaterialia, Vol. 6, pp. 302-307, (2010).
2. Wu C., et al., "Novel sphene coatings on Ti–6Al–4V for orthopedic implants using sol–gel method", Acta Biomaterialia, Vol. 4, pp. 569-576, (2008).
3. Duran A., et al., "Sol–gel coatings for protection and bioactivation of metals used in orthopaedic devices", Journal of Materials Chemistry, Vol. 14, pp. 2282-2290, (2004).
4. Catauro M., Papale F., Bollino F., "Coatings of titanium substrates with xCaO•(1− x) SiO 2 sol–gel materials: characterization, bioactivity and biocompatibility evaluation", Materials Science and Engineering C, Vol. 58, pp. 846-851, (2016).
5. Bibby J. K., et. al., "Fluorapatite-mullite glass sputter coated Ti6Al4V for biomedical applications", Journal of Materials Science: Materials in Medicine, Vol. 16, pp. 379-385, (2005).
6. Ong, Joo L., and Daniel CN Chan, "Hydroxyapatite and their use as coatings in dental implants: a review", Critical Reviews in Biomedical Engineering, Vol. 28(5-6), pp.667-707, (2000).
7.Tadashi K., Yamaguchi S., "Novel bioactive titanate layers formed on Ti metal and its alloys by chemical treatments", Materials, Vol. 3, pp. 48-63, (2009).
8. Velten D., et. al., "Preparation of TiO2 layers on cp‐Ti and Ti6Al4V by thermal and anodic oxidation and by sol‐gel coating techniques and their characterization", Journal of Biomedical Materials Research, Vol. 59, pp. 18-28, (2002).
9. Catauro M., et al., "Silica–polyethylene glycol hybrids synthesized by sol–gel: Biocompatibility improvement of titanium implants by coating", Materials Science and Engineering C, Vol. 55, pp. 118-125, (2015).
10. Catauro, Michelina, Flavia Bollino, and Ferdinando Papale, "Surface modifications of titanium implants by coating with bioactive and biocompatible poly (ε-caprolactone)/SiO2 hybrids synthesized via sol–gel", Arabian Journal of Chemistry, Vol. 4(7), (2015).
11. Bansiddhi, Ampika,"Processing and properties of porous nickel titanium", ProQuest Dissertations and Theses; Thesis (Ph.D.), No. AAI3331084; ISBN: 9780549883265, Northwestern University, (2008).
12. Wang X., et. al., "Fabrication and corrosion resistance of calcium phosphate glass-ceramic coated Mg alloy via a PEG assisted sol–gel method", Ceramics International, Vol. 40, pp. 3389-3398, (2014).
13. Bhola R., et. al., "Corrosion in titanium dental implants/prostheses–a review", Trends in Biomaterials and Artificial Organs, Vol. 25, pp. 34-46, (2011).
14. Holmberg, Kenneth, and Allan Matthews, "Coatings tribology: properties, mechanisms, techniques and applications in surface engineering", Elsevier Science; 2 edition , Amsterdam ; London, Vol. 56. Pp. 142-162, (2009).
15. Sato T., et. al., "Preparation of TiO2–Na2O glass by sol–gel method and structural characterization", Journal of Non-Crystalline Solids, Vol. 353, pp. 2832-2836, (2007).
16. Durgalakshmi D., Ajay R., Balakumar S., "Stacked Bioglass/TiO2 nanocoatings on titanium substrate for enhanced osseointegration and its electrochemical corrosion studies", Applied Surface Science, Vol. 349, pp. 561-569, (2015).
17. Ge F., et. al., "Preparation and drug release behavior of TiO2 nanorod films with incorporating mesoporous bioactive glass", Thin Solid Films, Vol. 584, pp. 2-8, (2015).
18. Delben J.R.J., et. al., "Bioactive glass prepared by sol–gel emulsion", Journal of Non-Crystalline Solids, Vol. 361 pp. 119-123, (2013).
19. Luz, Gisela M., and João F. Mano, "Preparation and characterization of bioactive glass nanoparticles prepared by sol–gel for biomedical applications", Nanotechnology, Vol. 22.49, pp. 494014, (2011).
20. Kumar, Anil, and Sevi Murugavel, "Influence of textural properties on biomineralization behavior of mesoporous bioactive glasses", Biomedical glasses, Vol. 1.1, pp. 12-19, (2015).
21. Abbasi Z., et. al., "Bioactive glasses in dentistry: a review", Journal of Dental Biomaterials, Vol. 2, pp. 1-9, (2015).
22. Bahniuk, Markian S., et al., "Bioactive glass 45S5 powders: effect of synthesis route and resultant surface chemistry and crystallinity on protein adsorption from human plasma", Biointerphases, Vol. 7.1, pp. 41, (2012).
23. Zhong J., Greenspan D.C., "Processing and properties of sol–gel bioactive glasses", Journal of Biomedical Materials Research, Vol. 53, pp. 694-701, (2000).
24. Mezahi F., et. al., "Reactivity kinetics of 52S4 glass in the quaternary system SiO2–CaO–Na2O–P2O5: Influence of the synthesis process: Melting versus sol–gel", Journal of Non-Crystalline Solids, Vol. 361, pp. 111-118, (2013).
25. Nychka, John A., et al., "Dissolution of bioactive glasses: The effects of crystallinity coupled with stress", Jom, Vol. 61.9, pp. 45-51, (2009).
26. Bellucci D., et. al., "Sol–gel derived bioactive glasses with low tendency to crystallize: Synthesis, post-sintering bioactivity and possible application for the production of porous scaffolds", Materials Science and Engineering C, Vol. 43, pp. 573-586, (2014).
27. Chen X., et. al., "Investigation on bio-mineralization of melt and sol–gel derived bioactive glasses", Applied Surface Science, Vol. 255, pp. 562-564, (2008).
28. Padilla S., et. al., "The influence of the phosphorus content on the bioactivity of sol–gel glass ceramics", Biomaterials, Vol. 26, pp. 475-483, (2005).
29. Chatzistavrou X., et. al., "Sol–gel based fabrication of novel glass-ceramics and composites for dental applications", Materials Science and Engineering C, Vol. 30, pp. 730-739, (2010).
30. Cai S., et. al., "Microstructural characteristics and crystallization of CaO–P2O5–Na2O–ZnO glass ceramics prepared by sol–gel method", Journal of Non-crystalline Solids, Vol. 355, pp. 273-279, (2009).
31. Shu C., et. al., "Dissolution behavior and bioactivity study of glass ceramic scaffolds in the system of CaO–P2O5–Na2O–ZnO prepared by sol–gel technique", Materials Science and Engineering C, Vol. 30, pp. 105-111, (2010).
32. Agathopoulos S., et. al., "The fluorapatite–anorthite system in biomedicine", Biomaterials, Vol. 24, pp. 1317-1331, (2003).
33. Khater, G. A. et al., "Spodumene- Nepheline- Anorthite Glass Ceramics for Dental Applications", Journal of Applied Sciences Research, Vol. 9 (1), pp. 821-825, (2013).
34. Wei, Daqing, and Yu Zhou, "Bioactive Microarc Oxidized TiO2-based Coatings for Biomedical Implication", Asian Pacific Conference for Materials and Mechanics,Yokohama, Japan, (2011).
35. Wren A.W., et. al., "A preliminary investigation into the structure, solubility and biocompatibility of solgel SiO2–CaO–Ga2O3 glass-ceramics", Materials Chemistry and Physics, Vol. 148, pp. 416-425, (2014).
36. Nayak A.K., "Hydroxyapatite synthesis methodologies: an overview", International Journal of ChemTech Research, Vol. 2, pp. 903-907, (2010).
37. Roach P., et. al., "Modern biomaterials: a review—bulk properties and implications of surface modifications", Journal of Materials Science Materials in Medicine, Vol. 18, pp. 1263-1277, (2007).
38. Attia Y., "Sol-gel processing and applications", Springer Science & Business Media, (2012).
39. Izquierdo-Barba I., Salinas A. J., Vallet-Regi M., "In vitro calcium phosphate layer formation on sol-gel glasses of the CaO-SiO2 system", Journal of Biomedical Materials Research, Vol. 47, pp. 243-250, (1999).
40. Sopyan I., Naqshbandi A., "Zinc-doped biphasic calcium phosphate nanopowders synthesized via sol-gel method", Indian Journal of Chemistry Section a-Inorganic Bio-Inorganic Physical Theoretical & Analytical Chemistry, Vol. 53, pp. 152-158, (2014).
41. Braem A., et. al., "Biofunctionalization of porous titanium coatings through sol–gel impregnation with a bioactive glass–ceramic", Materials Science and Engineering C, Vol. 32, pp. 2292-2298, (2012).
42. Nabian N., et al., "Quenched/unquenched nanobioactive glass-ceramics: Synthesis and in vitro bioactivity evaluation in Ringer's solution with BSA", Chemical Industry and Chemical Engineering Quarterly/CICEQ, Vol. 19, pp. 231-239, (2013).
43. Olmo N., et. al., "Bioactive sol–gel glasses with and without a hydroxycarbonate apatite layer as substrates for osteoblast cell adhesion and proliferation", Biomaterials, Vol. 24, pp. 3383-3393, (2003).
44. Lakshmi, R., and S. Sasikumar, "Influence of needle-like morphology on the bioactivity of nanocrystalline wollastonite–an in vitro study", International journal of nanomedicine, Vol. 10(Suppl 1, pp. 129-136, (2015).
45. Luyckx S., Love A., "The relationship between the abrasion resistance and the hardness of WC-Co alloys", Journal of the South African Institute of Mining and Metallurgy, Vol. 104, pp. 579-582, (2004).
46. Emamian, Ali, "A Study on Wear Resistance, Hardness and Impact Behaviour of Carburized Fe-Based Powder Metallurgy Parts for Automotive Applications", Materials Sciences and Applications, Vol. 3(08), pp.519, (2012).
47. Oshida Y., et. al., "Dental implant systems", International Journal of Molecular Sciences, Vol. 11, pp. 1580-1678, (2010).