Abstract
Sterilization is one of the last stages prior to the implantation of a biomaterial. Therefore, the method should be chosen carefully as this is determinant not to compromise the properties of the material. In this context, three sterilization processes were evaluated as to their effect on the properties of a silane hybrid coating: steam autoclave, ethylene oxide, and hydrogen peroxide plasma. The coating was obtained from a sol consisting of alkoxysilane Tetraethoxysilane and organoalcoxysilane Methyltriethoxysilane (MTES), applied to the Ti6Al4V substrate, to increase its corrosion resistance and biocompatibility. After sterilization, the samples were characterized by scanning electron microscopy, atomic force microscopy, profilometry, wetabillity, and Fourier transform infrared spectroscopy. The electrochemical behavior was monitored by open circuit potential and potentiodynamic polarization curves. The cytocompatibility was evaluated by adhesion, viability, and morphological alterations in the MG-63 cells. The results showed that the protective behavior of the hybrid coating was compromised regardless of the sterilization method. However, the steam autoclave caused more morphological changes on the silane hybrid coating as well as on the Ti6Al4V substrate than the other two sterilization methods. Although the sterilized hybrid coating did not show cytotoxicity, the hybrid coating sterilized by hydrogen peroxide plasma showed a higher percentage of viable cells. The ethylene oxide presented the lowest percentage of viability and the highest cell death rate.
Similar content being viewed by others
References
J.H. Park, R.O. Navarrete, R.E. Baier, A.E. Meyer, R. Tannenbaum, B.D. Boyan, and Z. Schwartz: Effect of cleaning and sterilization on titanium implant surface properties and cellular response. Acta Biomater. 8, 1966 (2012).
M.A. Vetten, C.S. Yah, T. Singh, and M. Gulumian: Challenges facing sterilization and depyrogenation of nanoparticles: Effects on structural stability and biomedical applications. Nanomedicine 10, 1391 (2014).
X.L. Liu, W.R. Zhou, Y.H. Wu, Y. Chen, and Y.F. Zheng: Effect of sterilization process on surface characteristics and biocompatibility of pure Mg and MgCa alloys. Mater. Sci. Eng., C 33, 4144 (2013).
Q.Q. Qiu, W.Q. Sun, and J. Connor: Sterilization of Biomaterials of Synthetic and Biological Origin (Elsevier, Branchburg, New Jersey, 2011); p. 127.
M. Savaris, V. Dos Santos, and R.N. Brandalise: Influence of different sterilization processes on the properties of commercial poly(lactic acid). Mater. Sci. Eng., C 69, 661 (2016).
A.J. Wilson and S. Nayak: Disinfection, sterilization and disposables. Anaesthesia Intensive Care Med. 14, 423 (2013).
J. Chen, J. Wang, and H. Yuan: Morphology and performances of the anodic oxide films on Ti6Al4V alloy formed in alkaline-silicate electrolyte with aminopropyl silane addition under low potential. Appl. Surf. Sci. 284, 900 (2013).
F. Yu, O. Addison, and A.J. Davenport: A synergistic effect of albumin and H2O2 accelerates corrosion of Ti6Al4V. Acta Biomater. 26, 355 (2015).
E. Vasilescu, P. Drob, D. Raducanu, J.M.C. Moreno, M. Popa, and J.C.M. Rosca: Effect of thermo-mechanical processing on the corrosion resistance of Ti6Al4V alloys in biofluids. Corros. Sci. 51, 2885 (2009).
N. Somsanith, T.S.N. Narayanan, Y.K. Kim, I.S. Park, T.S. Bae, and M.H. Lee: Surface medication of Ti–15Mo alloy by thermal oxidation: Evaluation of surface characteristics and corrosion resistance in Ringer’s solution. Appl. Surf. Sci. 356, 1117 (2015).
J. Zhao, M. Milanova, M.M.C.G. Warmoeskerken, and V. Dutschk: Surface modification of TiO2 nanoparticles with silane coupling agents. Colloids Surf., A 413, 273 (2012).
R.A. Surmenev, M.A. Surmeneva, and A.A. Ivanova: Significance of calcium phosphate coatings for the enhancement of new bone osteogenesis—A review. Acta Biomater. 10, 557 (2014).
J. Xie and B.L. Luan: Microstructural and electrochemical characterization of hydroxyapatite-coated Ti6Al4V alloy for medical implants. J. Mater. Res. 23, 768 (2008).
D. Ke, S.F. Robertson, W.S. Dernell, A. Bandyopadhyay, and S. Bose: Effects of MgO and SiO2 on plasma-sprayed hydroxyapatite coating: An in vivo study in rat distal femoral defects. Appl. Mater. Interfaces 9, 25731 (2017).
R.I.M. Asri, W.S.W. Harun, M.A. Hassan, S.A.C. Ghani, and Z. Buyong: A review of hydroxyapatite-based coating techniques: Sol–gel and electrochemical depositions on biocompatible metals. J. Mech. Behav. Biomed. Mater. 57, 95 (2016).
P. Choudhury and D.C. Agrawal: Sol–gel derived hydroxyapatite coatings on titanium substrates. Surf. Coat. Technol. 206, 360 (2011).
M.J. Juan-Díaz, M. Martínez-Ibáñez, I. Lara-Sáez, S. da Silva, R. Izquierdo, M. Gurruchaga, I. Goñi, and J. Suay: Development of hybrid sol–gel coatings for the improvement of metallic biomaterials performance. Prog. Org. Coat. 96, 42 (2016).
P. Dubruel, E. Vanderleyden, M. Bergadà, I.D. Paepe, H. Chen, S. Kuypers, J. Luyten, J. Schrooten, L.V. Hoorebeke, and E. Schacht: Comparative study of silanisation reactions for the biofunctionalisation of Ti-surfaces. Surf. Sci. 600, 2562 (2006).
S.A. Omar, J. Ballare, and S.M. Ceré: Protection and functionalization of AISI 316L stainless for orthopedic implants: Hybrid coating and sol gel glasses by spray to promote bioactivity. Electrochim. Acta 203, 309 (2016).
J. Ballarre, R. Seltzer, E. Mendoza, J.C. Orellano, Y.W. Mai, C. García, and S.M. Ceré: Morphologic and nanomechanical characterization of bone tissue growth around bioactive sol–gel coatings containing wollastonite particles applied on stainless steel implants. Mater. Sci. Eng., C 31, 545 (2011).
D. Wang and G.P. Bierwagen: Sol–gel coatings on metals for corrosion protection. Prog. Org. Coat. 64, 327 (2009).
A. Zomorodian, F. Brusciotti, A. Fernandes, M.J. Moura, J.C.S. Fernandes, and M.F. Montemor: Anti-corrosion performance of a new silane coating for corrosion protection of AZ31 magnesium alloy in Hank’s solution. Surf. Coat. Technol. 206, 4368 (2012).
N. Hojjati, R. Mozaffarinia, S.R. Hamed, and E. Paimozd: Sol–gel processing of hybrid nanocomposite protective coatings using experimental design. Prog. Org. Coat. 76, 293 (2013).
C.Y. Zheng, F.L. Nie, Y.F. Zheng, Y. Cheng, S.C. Wei, and R.Z. Valiev: Enhanced corrosion resistance and cellular behavior of ultrafine-grained biomedical NiTi alloy with a novel SrO–SiO2–TiO2 sol–gel coating. Appl. Surf. Sci. 257, 5913 (2011).
X. Liu, Z. Yue, T. Romeo, J. Weber, T. Scheuermann, S. Moulton, and G. Wallace: Biofunctionalized anti-corrosive silane coatings for magnesium alloys. Acta Biomater. 9, 8671 (2013).
I. Junkar, M. Kulkarni, and B. Drašler: Influence of various sterilization procedures on TiO2 nanotubes used for biomedical devices. Bioelectrochemistry 109, 79 (2016).
M. Hirano, T. Kozuka, and Y. Asano: Effect of sterilization and water rinsing on cell adhesion to titanium surfaces. Appl. Surf. Sci. 311, 498 (2014).
S. Oh, K.S.B. Rammer, K.S. Moon, J.M. Bae, and S. Jins: Influence of sterilization methods on cell behavior and functionality of osteoblasts cultured on TiO2 nanotubes. Mater. Sci. Eng., C 31, 873 (2011).
W. Walke, Z. Paszenda, T. Pustelny, M.K. Ziemniak, and M. Basiaga: Evaluation of physicochemical properties of SiO2-coated stainless steel after sterilization. Mater. Sci. Eng., C 63, 155 (2016).
J.C. Almeida, L. Joana, V.F.M. Helena, M.A.M. Fernanda, and I.M. Alvado: Evaluating structural and microstructural changes of PDMS–SiO2 hybrid materials after sterilization by gamma irradiation. Mater. Sci. Eng., C 48, 354 (2015).
C. García, S. Ceré, and A. Durán: Bioactive coatings prepared by sol–gel on stainless steel 316L. J. Non-Cryst. Solids 348, 218 (2004).
J. Ballarre, D.A. López, W.H. Schreiner, A. Durán, and S.M. Ceré: Protective hybrid sol–gel coatings containing bioactive particles on surgical grade stainless steel: Surface characterization. Appl. Surf. Sci. 253, 7260 (2007).
J. Ballarre, I. Manjubala, W.H. Schreiner, J.C. Orellano, F. Peter, and S. Ceré: Improving the osteointegration and bone–implant interface by incorporation of bioactive particles in sol–gel coatings of stainless steel implants. Acta Biomater. 6, 1601 (2010).
A. Rodríguez-Cano, P. Cintas, M.C. Fernández-Calderón, M.A. Pacha-olivenza, L. Crespo, M.L. González-Martín, and R. Babiano: Controlled silanization–amination reactions on the Ti6Al4V surface for biomedical applications. Colloids Surf., B 106, 248 (2013).
G.T. Smith: Industrial Metrology (Faculty of Technology, Springer, London, 2002); pp. 24–356.
T. Kokubo and H. Takadama: How useful is SBF in predicting in vivo bone bioactivity? Biomaterials 27, 2907 (2006).
J. Ballarre, D.A. López, N.C. Rosero, A. Durán, M. Aparicio, and S.M. Ceré: Electrochemical evaluation of multilayer silica–metacrylate hybrid sol–gel coatings containing bioactive particles on surgical grade stainless steel. Surf. Coat. Technol. 203, 80 (2008).
T. Mosmann: Rapid colorimetric assay for cellular growth and survival: Application to proliferation and cytotoxicity assays. J. Immunol. Methods 65, 55 (1983).
M.C. Alley, A.S. Dominic, M. Anne, L.M. Miriam, J.C. Maciej, L.F. Donald, J.A. Betty, G.M. Joseph, H.S. Robert, and R.B. Michael: Feasibility of drug screening with panels of human tumor cell lines using a microculture tetrazolium assay. Cancer Res. 48, 589 (1988).
A. Nersesyan, M. Kundi, K. Atefie, R. Schulte-hermann, and S. Knasmuller: Effect of staining procedures on the results of micronucleus assays with exfoliated oral mucosa cells. Cancer Epidemiol., Biomarkers Prev. 15, 1835 (2006).
E.K.K. Baldin, S.R. Kunst, L.V.R. Beltrami, T.M. Lemos, A.C.B. Quevedo, M.G.S. Ferreira, P.R.R. Santos, V.H.V. Sarmento, and C.F. Malfatti: Ammonium molybdate added in hybrid films applied on tinplate: Effect of the concentration in the corrosion inhibition action. Thin Solid Films 600, 146 (2016).
M. Wang, Y. Wang, Y. Chen, and H. Gu: Improving endothelialization on 316L stainless steel through wettability controllable coating by sol–gel technology. Appl. Surf. Sci. 268, 73 (2013).
P. Innocenzi, M.O. Abdirashid, and M.I. Guglielm: Structure and properties of sol–gel coatings from methyltriethoxysilane and tetraethoxysilane. J. Sol-Gel Sci. Technol. 3, 47 (1994).
S.R. Kunst, L.V.R. Beltrami, H.R.P. Cardoso, J.A. Santana, V.H.V. Sarmento, I.L. Müller, and C.F. Malfatti: Characterization of siloxane–poly(methyl methacrylate) hybrid films obtained on a tinplate substrate modified by the addition of organic and inorganic acids. Mater. Res. 18, 151 (2015).
J.A. Gan and C.C. Berndt: Plasma surface modification of metallic biomaterials. Surf. Coat. Modif. Met. Biomater. 1, 103 (2015).
G. Müller, H. Benkhai, R. Matthes, B. Finke, W. Friedrichs, N. Geist, W. Langel, and A. Kramer: Poly(hexamethylene biguanide) adsorption on hydrogen peroxide treated Ti–Al–V alloys and effects on wettability, antimicrobial efficacy and cytotoxicity. Biomaterials 35, 5261 (2014).
M. Pegueroles, F.J. Gil, J.A. Planell, and C. Aparicio: The influence of blasting and sterilization on static and time-related wettability and surface-energy properties of titanium surfaces. Surf. Coat. Technol. 202, 3470 (2008).
C.C.R. Wang, M.C. Hsieh, and T.M. Lee: Effects of nanometric roughness on surface properties and fibroblast’s initial cytocompatibilities of Ti6AI4V. Biointerphases 6, 87 (2011).
R. Galante, D. Ghisleni, P. Paradiso, V.D. Alves, T.J.A. Pinto, R. Colaço, and A.P. Serro: Sterilization of silicone-based hydrogels for biomedical application using ozone gas: Comparison with conventional techniques. Mater. Sci. Eng., C 78, 389 (2017).
M.L. Lee, H.L. Kim, C.H. Kim, S.H. Lee, J.K. Kim, S.J. Lee, and J.C. Park: Effects of low temperature hydrogen peroxide gas on sterilization and cytocompatibility of porous poly(D,L-lactic-co-glycolic acid) scaffolds. Surf. Coat. Technol. 202, 5762 (2008).
S. Fleith, A. Ponche, R. Bareille, J. Amédée, and M. Nardin: Effect of several sterilisation techniques on homogeneous self assembled monolayers. Colloids Surf., B 44, 15 (2005).
G.R. Holyak, S. Wang, Y. Liu, and T.D. Bunch: Toxic effects of ethylene oxide residues on bovine embryos. Toxicol. In Vitro 108, 33 (1996).
R. França, A.M. Doris, T.D. Samani, C.L. Tien, M.A. Mateescu, L. Yahia, and E. Sacher: The effect of ethylene oxide sterilization on the surface chemistry and in vitro cytotoxicity of several kinds of chitosan. J. Biomed. Mater. Res., Part B 101, 1444 (2013).
C. Yavuz, S.N.B. Oliaei, and O.S. Celikta: Sterilization of PMMA microfluidic chips by various techniques and investigation of material characteristic. J. Supercrit. Fluids 107, 114 (2016).
A.L.R. Ribeiro, P. Hammer, L.G. Vaz, and L.A. Rocha: Are new TiNbZr alloys potential substitutes of the Ti6Al4V alloy for dental applications? An electrochemical corrosion study. Biomed. Mater. 8, 65005 (2013).
M.M. López, J. Fauré, M.I.E. Cabrera, and M.E.C. García: Structural characterization and electrochemical behavior of 45S5 bioglass coating on Ti6Al4V alloy for dental applications. Mater. Sci. Eng., B 206, 30 (2016).
J. Szewczenko, P.M. Grygiel, W. Walke, K. Nowinska, J. Granieczny, M. Kaczmarek, and J. Marciniak: Corrosion resistance of Ti6Al4V alloy in modified SBF environments. Key Eng. Mater. 687, 79 (2015).
M. Kiel-Jamrozik, J. Szewczenko, M. Basiaga, and K. Nowińska: Technological capabilities of surface layers formation on implant made of Ti–6Al–4V ELI alloy. Acta Bioeng. Biomech. 17, 31 (2016).
Z. Paszenda, W. Walke, and S. Jadacka: Electrochemical investigations of Ti6Al4V and Ti6Al7Nb alloys used on implants in bone surgery. J. Achiev. Mater. Manuf. Eng. 38, 24 (2010).
M. Basiaga, W. Walke, Z. Paszenda, and A. Kajzer: The effect of EO and steam sterilization on the mechanical and electrochemical properties of titanium grade 4. Mater. Tehnol. 50, 153 (2016).
C. García, S. Ceré, and A. Durán: Bioactive coatings deposited on titanium alloys. J. Non-Cryst. Solids 352, 3488 (2006).
Á. Györgyey, K. Ungvári, and G. Kecskeméti: Attachment and proliferation of human osteoblast-like cells (MG-63) on laser-ablated titanium implant material. Mater. Sci. Eng., C 33, 4251 (2013).
F. Likibi, B. Jiang, and B. Li: Biomimetic nanocoating promotes osteoblast cell adhesion on biomedical implants. J. Mater. Res. 23, 3222 (2008).
C. Wirth, B. Grosgogeat, N. Jaffrezic-Renault, and L. Ponsonnet: Biomaterial surface properties modulate in vitro rat calvaria osteoblasts response: Roughness and or chemistry? Mater. Sci. Eng., C 28, 990 (2008).
R.A. Gittens, T. McLachlan, R. Olivares-Navarrete, Y. Cai, S. Berner, R. Tannenbaum, Z. Schwartz, K.H. Sandhage, and B.D. Boyan: The effects of combined micron/submicron-scale surface roughness and nanoscale features on cell proliferation and differentiation. Biomaterials 32, 3395 (2011).
B.S. Moon, S. Kim, H.E. Kim, and T.S. Jang: Hierarchical micro-nano structured Ti6Al4V surface topography via two-step etching process for enhanced hydrophilicity and osteoblastic responses. Mater. Sci. Eng., C 73, 90 (2017).
L. Zhao, S. Mei, and W. Wang: The role of sterilization in the cytocompatibility of titania nanotubes. Biomaterials 31, 2055 (2010).
J.Y. Martin, Z. Schwartz, T.W. Hummert, D.M. Schraub, J. Simpson, J.R.J. Lankford, D.D. Dean, D.L. Cochran, and B.D. Boyan: Effect of titanium surface roughness on proliferation, differentiation, and protein synthesis of human osteoblast-like cells (MG-63). J. Biomed. Mater. Res. 29, 389 (1995).
S. Sharma, S. Bano, and A.S. Ghosh: Silk fibroin nanoparticles support in vitro sustained antibiotic release and osteogenesis on titanium surface. Nanomedicine 12, 1193 (2016).
ACKNOWLEDGMENTS
The authors would like to express their gratitude to CNPq (Project PVE 401211/2014-2), CAPES, UFRGS, UCS, Esterilizare RS/Brazil and hospital Pompéia RS/Brazil for the investment and support in this research.
Author information
Authors and Affiliations
Corresponding author
Supplementary Material
Rights and permissions
About this article
Cite this article
Baldin, E.K.K., Garcia, C., Henriques, J.A.P. et al. Effect of sterilization processes on the properties of a silane hybrid coating applied to Ti6Al4V alloy. Journal of Materials Research 33, 161–177 (2018). https://doi.org/10.1557/jmr.2017.429
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1557/jmr.2017.429