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Optimisation of the enamelling of an apatite–mullite glass–ceramic coating on Ti6Al4V

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Abstract

Apatite–mullite glass–ceramics (AMGCs) are under investigation as a potential alternative to hydroxyapatite (HA) as a coating for cementless fixation of orthopaedic implants. These materials have tailorable mechanical and chemical properties that make them attractive for use as bioactive coatings. Here, AMGC coatings on Ti6Al4V were investigated to determine an improved heat treatment regime using a systematic examination of the different inputs: composition of glass, nucleation hold and crystallisation hold. An upper limit to the heat treatment temperature was determined by the \(\alpha\,+\,\beta\,\longrightarrow\,\beta\) of Ti6Al4V at 970°C. The glass composition was modified to produce different crystallisation temperatures and sintering characteristics. A glass was found that is fully crystalline below 970°C and has good sinterability. The effects of different heat treatment time and temperature combinations on the coating and substrate morphologies were examined and the most suitable combination determined. This sample was further investigated and was found to have qualitatively good adhesion and evidence of an interfacial reaction region between the coating and substrate indicating that a chemical reaction had occurred. Oxygen infiltration into the substrate was quantified and the new route was shown to result in a 63% reduction in penetration depth.

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Notes

  1. Stanton and Vanhumbeeck [23] first described a successful route for enamelling AMGC to Ti6Al4V. The following protocol was used: G187 was sedimented on Ti6Al4V in the same manner as used here then heated from room temperature at 10 K min−1 to 670°C (the ONT for G187 [23]); held for 60 min; 670–960°C at 10 K min−1; held for 90 min; cool to ambient at 10 K min−1.

References

  1. Akahori T, Niinomi M, Fukunaga K, Inagaki I. Effects of microstructure on the short fatigue crack initiation and propagation characteristics of biomedical α/β titanium alloys. Metall Mater Trans A. 2000;31A(8):1949–1958.

    Article  CAS  Google Scholar 

  2. Bigerelle M, Anselme K, Nol B, Ruderman I, Hardouin P, Iost A. Improvement in the morphology of Ti-based surfaces: a new process to increase in vitro human osteoblast response. Biomaterials. 2002;23(7):1563–1577.

    Article  CAS  Google Scholar 

  3. Boivineau M, Cagran C, Doytier D, Eyraud V, Nadal M, Wilthan B, Pottlacher G. Thermophysical properties of solid and liquid Ti–6Al–4V (TA6V) alloy. Int J Thermophys. 2006;27(2):507–529.

    CAS  Google Scholar 

  4. Bowen R. Adhesive bonding of various materials to hard tooth tissues IV. Bonding to dentin, enamel, and fluorapatite improved by the use of a surface-active comonomer. J Dent Res. 1965;44(5):906–911.

    Article  CAS  Google Scholar 

  5. Clifford A, Hill R. Apatite–mullite glass–ceramics. J Non-cryst Solids. 1996;196(1–3):346–351.

    Article  CAS  Google Scholar 

  6. Cross M, Parish E. A hydroxyapatite-coated total knee replacement PROSPECTIVE ANALYSIS OF 1000 PATIENTS. J Bone Joint Surg Br. 2005;87(8):1073–1076.

    Article  CAS  Google Scholar 

  7. Deligianni DD, Katsala ND, Koutsoukos PG, Missirlis YF. Effect of surface roughness of hydroxyapatite on human bone marrow cell adhesion, proliferation, differentiation and detachment strength. Biomaterials. 2001;22(1):87–96.

    Article  CAS  Google Scholar 

  8. Freeman C, Brooks I, Johnson A, Hatton P, Hill R, Stanton K. Crystallization modifies osteoconductivity in an apatite–mullite glass–ceramic. J Mater Sci Mater Med. 2003;14:985–990.

    Article  CAS  Google Scholar 

  9. Frosch K, Barvencik F, Viereck V, Lohmann C, Dresing K, Breme J, Brunner E, Sturmer K. Growth behavior, matrix production, and gene expression of human osteoblasts in defined cylindrical titanium channels. J Biomed Mater Res A. 2004;68A(2):325–334.

    Article  CAS  Google Scholar 

  10. Gomez-Vega J, Saiz E, Tomsia A. Glass-based coatings for titanium implant alloys. J Biomed Mater Res. 1999;46(4):549–559.

    Article  CAS  Google Scholar 

  11. Gomez-Vega J, Saiz E, Tomsia A, Marshall G, Marshall S. Bioactive glass coatings with hydroxyapatite and bioglass particles on Ti-based implants 1. Processing. Biomaterials. 2000;21(2):105–111.

    Article  CAS  Google Scholar 

  12. Haverty D, Tofail S, Stanton K, McMonagle J. Structure and stability of hydroxyapatite: density functional calculation and Rietveld analysis. Phys Rev B. 2005;71(9):94–103.

    Article  Google Scholar 

  13. Kasuga T, Nogami M, Niinomi M. Preparation of calcium phosphate glass–ceramics and their coating on titanium alloys. Key Eng Mater. 2001;192–195:223–226.

    Article  Google Scholar 

  14. Kingery W, Bowen H, Uhlmann D. Introduction to ceramics (ed.). New York: Wiley; 1976.

    Google Scholar 

  15. Kinloch A. Adhesion and adhesives. London: Chapman and Hall; 1987.

    Google Scholar 

  16. Long M, Rack H. Titanium alloys in total joint replacement—a materials science perspective. Biomaterials. 1998;19(18):1621–1639.

    Article  CAS  Google Scholar 

  17. Lopez-Esteban S, Saiz E, Fujino S, Oku T, Suganuma K, Tomsia A. Bioactive glass coatings for orthopedic metallic implants. J Eur Ceram Soc. 2003;23(15):2921–2930.

    Article  CAS  Google Scholar 

  18. Marotta A, Buri A, Branda F. Nucleation in glass and differential thermal analysis. J Mater Sci. 1981;16(2):341–344.

    Article  CAS  Google Scholar 

  19. O’Flynn K, Stanton K. Nucleation and early stage crystallization of fluorapatite in apatite–mullite glass–ceramics. Cryst Growth Des. 2010;10(3):1111–1117.

    Article  Google Scholar 

  20. Park D, Della Valle C, Quigley L, Moric M, Rosenberg A, Galante J. Revision of the acetabular component without cement. A concise follow-up, at twenty to twenty-four years, of a previous report. J Bone Joint Surg. 2009;91(2):350–355.

    Article  Google Scholar 

  21. Sha W, Guo Z. Phase evolution of Ti–6Al–4V during continuous heating. J Alloys Compd. 1999;290(1–2):3–7.

    Article  Google Scholar 

  22. Stanton K, Hill R. The role of fluorine in the devitrification of SiO2–Al2O3–P2O5–CaO–CaF2 glasses. J Mater Sci. 2000;35:1–6.

    Article  Google Scholar 

  23. Stanton K, Vanhumbeeck J. Bioactive apatite–mullite glass–ceramic coatings on titanium substrates. Adv Sci Technol. 2006;45:1275–1280.

    Article  CAS  Google Scholar 

  24. Stanton K, O’Flynn K, Newcombe S. TEM study of the reaction interface between an apatite–mullite glass–ceramic and Ti6Al4V. Key Eng Mater. 2007;361–363:269–272.

    Google Scholar 

  25. Stanton K, O’Flynn K, Nakahara S, Vanhumbeeck J, Delucca J, Hooghan B. Study of the interfacial reactions between a bioactive apatite–mullite glass–ceramic coating and titanium substrates using high angle annular dark field transmission electron microscopy. J Mater Sci Mater Med. 2009;20(4):851–857.

    Article  CAS  Google Scholar 

  26. Stanton K, O’Flynn K, Kiernan S, Menuge J, Hill R. Spherulitic crystallization of apatite–mullite glass–ceramics: mechanisms of formation and implications for fracture properties. J Non-cryst Solids. 2010;356(35–36):1802–1813.

    Article  CAS  Google Scholar 

  27. Tai C, Cross M. Five-to 12-year follow-up of a hydroxyapatite-coated, cementless total knee replacement in young, active patients. J Bone Joint Surg Br. 2006;88(9):1158–1163.

    Article  CAS  Google Scholar 

  28. Trentani L, Pelillo F, Pavesi F, Ceciliani L, Cetta G, Forlino A. Evaluation of the TiMo12Zr6Fe2 alloy for orthopaedic implants: in vitro biocompatibility study by using primary human fibroblasts and osteoblasts. Biomaterials. 2002;23(14):2863–2869.

    Article  CAS  Google Scholar 

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Acknowledgements

Part funding was provided by the Irish Research Council for Science, Engineering and Technology: funded by the National Development Plan. The authors also acknowledge the support from the UCD Nano Imaging and Material Analysis Centre (NIMAC) funded by Science Foundation Ireland (SFI).

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  1. School of Mechanical and Materials Engineering, University College Dublin, Belfield, Dublin 4, Ireland

    Kevin P. O’Flynn & Kenneth T. Stanton

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  1. Kevin P. O’Flynn
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  2. Kenneth T. Stanton
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Correspondence to Kenneth T. Stanton.

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O’Flynn, K.P., Stanton, K.T. Optimisation of the enamelling of an apatite–mullite glass–ceramic coating on Ti6Al4V. J Mater Sci: Mater Med 22, 2035–2044 (2011). https://doi.org/10.1007/s10856-011-4392-6

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  • DOI: https://doi.org/10.1007/s10856-011-4392-6

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