Microtensile Bond Strength and Failure Type Analysis of Self-Etch Adhesive Systems on Superficial and Deep Dentin After Long-term Water Storage


  • Pinar Cevik Gazi University faculty of dentistry https://orcid.org/0000-0003-1970-7543
  • Arzu Zeynep Yildirim
  • Zafer Artvin Research Scientist, Middle East Technical University - Department of Micro and Nanotechnology - Ankara - Turkey
  • Mutlu Özcan University of Zurich - Center for Dental and Oral Medicine - Division of Dental Biomaterials - Zurich - Switzerland




Objective: The aim of this study was to evaluate and compare the microtensile bond strengths of four current adhesive materials that contain different monomers at deep and superficial dentin. Material and Methods: Forty non-carious human third molars (n = 5) were used in the study. Specimens were divided into two main groups according to dentin thickness as superficial and deep dentin. Groups were further divided into four subgroups in terms of the adhesive systems used: Nova Compo B Plus (NCBP), Nova Compo B (NCB), Futurabond M (FB) and Clearfil S3 Bond Plus (CS3). All specimens were bonded to resin composite and stored in 37 °C water for 9-months. Teeth were sectioned into 3 x 3 mm x 1mm thick beams. Microtensile bond strength test was carried out by using a universal testing device (1 mm/min). After fracture, failure types were observed using an optical microscope and the fractured dentin surfaces were observed by a scanning electron microscopy (SEM). One-way ANOVA and Tukey tests were used to compare the adhesive system in each dentin group. An unpaired T-test was used to compare the dentin thickness in each adhesive material. Results: As compared to deep dentin, superficial dentin showed higher µTBS values in groups NCBP, FB and CS, as opposed to group NCB. Only NCB revealed higher bond strength at deep dentin layers when compared to superficial dentin. In the superficial dentin group, NCBP showed the highest bond strength value, while NCB showed the lowest bond strength. In the deep dentin group, while NCB showed the highest bond strength value, NCBP revealed the lowest bond strength value after 9-months storage. While 4-META and 10-MDP monomer combination (NCBP) resulted in the highest bond strength value among the adhesive systems in the superficial dentin group, the monomer combination (NCB) resulted in the highest bond strength in deep dentin group. Conclusions: Microtensile bond strength performance are affected by both the type of monomer in the adhesive combination and the depth of the dentin.


Adhesive system; dentin thickness; hydrophobic monomer; microtensile bond strength; scanning electron microscopy.

Author Biography

Pinar Cevik, Gazi University faculty of dentistry



Pashley DH, Carvalho RM. Dentine permeability and dentine adhesion. J Dent. 1997;25:355-72.

Matsui N, Takagaki T, Sadr A, Ikeda M, Ichinose S, Nikaido T, Tagami J. The role of MDP in a bonding resin of a two-step self-etching adhesive system. Dent Mater J. 2015;34:227-33.

Nakabayashi N, Kojima K, Masuhara E. The promotion of adhesion by the infiltration of monomers into tooth substrates. J Biomed Mater Res. 1982;16:265-73.

Nakabayashi N, Nakamura M, Yasuda M. Hybrid layer as a dentin-bonding mechanism. J Esthet Dent. 1991;3:133-38.

Takahashi M, Nakajima M, Hosaka K, Ikeda M, Foxton RM, Tagami J. Long-term evaluation of water sorption and ultimate tensile strength of HEMA-containing/-free one-step self-etch adhesives. J Dent. 2011;39:506-12.

Dhanpal P, Yiu CK, King NM, Tay FR, Hiraishi N. Effect of temperature on water sorption and solubility of dental adhesive resins. J Dent. 2009;37:122-32.

Reis AF, Giannini M, Pereira PN. Influence of water-storage time on the sorption and solubility behavior of current adhesives and primer/adhesive mixtures. Oper Dent. 2007;32:53-9.

Hosaka K, Tagami J, Nishitani Y, et al. Effect of wet vs. dry testing on the mechanical properties of hydrophilic self-etching primer polymers. Eur J Oral Sci. 2007;115:239-45.

Hosaka K, Nakajima M, Takahashi M, Itoh S, Ikeda M, Tagami J, Pashley DH. Relationship between mechanical properties of one-step self etch adhesives and water sorption. Dent Mater. 2010;26:360-7.

Ito S, Hashimoto M, Wadgaonkar B, et al. Effects of resin hydrophilicity on water sorption and changes in modulus of elasticity. Biomaterials. 2005;26:6449-59.

Paul SJ, Leach M, Rueggeberg FA, Pashley DH. Effect of water content on the physical properties of model dentine primer and bonding resins. J Dent. 1999;27:209-14.

Tay FR, Pashley DH, Yoshiyama M. Two modes of nanoleakage expression in single-step adhesives. J Dent Res. 2002;81:472-6.

Hashimoto M, Fujita S, Kaga M, Yawaka Y. In vitro durability of one-bottle resin adhesives bonded to dentin. Dent Mater J. 2007;26:677-86.

Torkabadi S, Nakajima M, Ikeda M, Foxton RM, Tagami J. Bonding durability of HEMA-free and HEMA-containing one-step adhesives to dentine surronded by bonded enamel. J Dent. 2008;36:80-6.

Fukegawa D, Hayakawa S, Yoshida Y, Suzuki K, Osaka A, Van Meerbeek B. Chemical interaction of phosphoric acid ester with hydroxyapatite. J Dent Res. 2000;79:709-14.

Yoshida Y, Van Meerbeek B, Nakayama Y, et al. Chemical bonding at biomaterial-hard tissue interfaces. J Dent Res. 2006;85:941-4.

Foxton RM, Melo L, Stone DG, Pilecki P, Sherriff M, Watson TF. Long-term durability of one-step adhesive-composite systems to enamel and dentin. Oper Dent. 2008;33:651-7.

De Munck J, Van Landuyt K, Peumans M, Poitevin A, Lambrechts P, Braem M, Van Meerbeek B. A critical review of the durability of adhesion to tooth tissue: methods and results. J Dent Res. 2005;84:118-32.

Pashley EL, Agee KA, Pashley DH, Tay FR. Effects of one versus two applications of an unfilled, all-in-one adhesive on dentine bonding. J Dent. 2002;30:83-90.

Tay FR, Pashley DH, Suh BI, Carvalho RM, Itthagarun A. Single-step adhesives are permeable membranes. J Dent. 2002;30:371-82.

Itoh S, Nakajima M, Hosaka K, et al. Dentin bond durability and water sorption/solubility of one-step self-etch adhesives. Dent Mater. 2010;29:623-30.

Pereira PN, Okuda M, Sano H, Yoshikawa T, Burrow MF, Tagami J. Effect of intrinsic wetness and regional difference on dentin bond strength. Dent Mater. 1999;15:46-53.

Van Landuyt KL, De Munck J, Snauwert J, et al. Monomer-solvent phase separation in one-step self-etch adhesives. J Dent Res. 2005;84:183-8.

Roulet JF, Van Meerbeek B. Editorial: Statistics: a nuisance, a tool, or a must? J Adhes Dent. 2007;9:287-8.

Miranda TA, Moura SK, Amorim VH, Terada RS, Pascotto RC. Influence of exposure time to saliva and antioxidant treatment on bond strength to enamel after tooth bleaching: an in situ study. J Appl Oral Sci. 2013;21:567-74.

Van Meerbeek B, Peumans M, Poitevin A, Mine A, Van Ende A, Neves A, De Munck J. Relationship between bond-strength tests and clinical outcomes. Dent Mater .2010;26:100-21.

Loguercio AD, Barroso LP, Grande RH, Reis A. Comparison of intra- and intertooth resin-dentin bond strength variability. J Adhes Dent. 2005;7:151-158

Nakaoki Y, Nikaido T, Pereira PN, Inokoshi S, Tagami J. Dimensional changes of demineralized dentin treated with HEMA primers. Dent Mater. 2000;16:441-6.

Van Landuyt KL, Snauwaert J, De Munck J, et al. Systematic review of the chemical composition of contemporary dental adhesives. Biomaterials. 2007;28:3757-85.

Ting S, Chowdhury AA, Pan F, et al. Effect of remaining dentin thickness on microtensile bond strength of current adhesive systems. Dent Mater J. 2015;34:181-8.

Goracci C, Sadek FT, Monticelli F, Cardoso PE, Ferrari M. Influence of substrate, shape, and thickness on microtensile specimens’ structural integrity and their measured bond strengths. Dent Mater. 2004;20:643-54.

Sano H, Shono T, Sonoda H, Pashley DH. Relationship between surface area for adhesion and tensile bond strength-evaluation of a microtensile test. Dent Mater. 1994;10:236-40.

Pashley DH, Ciucchi B, Sano H, Yoshiyama M, Carvalho RM. Adhesion testing of dentin bonding agents. A review. Dent Mater. 1995;11:117-25.

Phrukkanon S, Burrow MF, Tyas MJ. The influence of crosssectional shape and surface area on the microtensile bond test. Dent Mater. 1998;14:212-221.

Pashley DH, Carvalho RM, Sano H, Nakajima M, Yoshiyama M, Shono Y, Fernandes CA, Tay F. The microtensile bond test: a review. J Adhes Dent. 1999;1:299-309.

Chigira H, Itoh K, Tachikawa T, Wakumoto S, Hisamitsu H. Bonding efficacy and interfacial microstructure between resin and dentine primed with glyceryl methacrylate. J Dent. 1998;26:157-63.

Koliniotou-Koumpia E, Kouros P, Koumpia E, Helvatzoglou-Antoniades M. Shear bond strength of a “solvent-free” adhesive versus contemporary adhesive systems. Braz J Oral Sci. 2014;13:64-9.

Asmussen E, Munksgaard EC. Bonding of restorative resins to dentine: status of dentine adhesives and impact on cavity design and filling techniques. Int Dent J. 1988;38:97-104.

Sakano W, Nakajima M, Prasansuttiporn T, Foxton RM, Tagami J. Polymerization behavior within adhesive layer of one- and two-step self-etch adhesives: a micro-Raman spectroscopic study. Dent Mater J. 2013;32:992-8.

Tekce N, Demirci M, Tuncer S, Uysal Ö. Microtensile bond strength and sealing efficiency of all-in-one self-etching adhesives. Biotechnol Biotechnol Equip. 2015;29:570-8.

Yoshida Y, Nagakane K, Fukuda R, et al. Comparative study on adhesive performance of functional monomers. J Dent Res. 2004;83:454-8.

Yoshihara K, Yoshida Y, Nagaoka N, et al. Nano-controlled molecular interaction at adhesive interfaces for hard tissue reconstruction. Acta Biomater. 2010;6:3573-82.

Yoshihara K, Yoshida Y, Hayakawa S, et al. Nanolayering of phosphoric acid ester monomer on enamel and dentin. Acta Biomater. 2011;7:3187-95.

Yoshihara K, Yoshida Y, Hayakawa S, et al. Self-etch monomer-calcium salt deposition on dentin. J Dent Res. 2011;90:602-606.

Peumans M, De Munck J, Van Landuyt KL, Poitevin A, Lambrechts P, Van Meerbeek B. Eight-year clinical evaluation of a 2-step self-etch adhesive with and without selective enamel etching. Dent Mater. 2010;26:1176-84.

Van Meerbeek B, Yoshihara K, Yoshida Y, Mine A, De Munck J, Van Landuyt K. State of the art of self-etch adhesives. Dent Mater. 2011;27:17-28.

Feitosa VP1, Ogliari FA, Van Meerbeek B, Watson TF, Yoshihara K, Ogliari AO, Sinhoreti MA, Correr AB, Cama G, Sauro S. Can the hydrophilicity of functional monomers affect chemical interaction? J Dent Res. 2014;93:201-6.

Gauthier MA, Stangel I, Ellis TH, Zhu XX. Oxygen inhibition in dental resins. J Dent Res. 2005;84:725-9.



2020-09-30 — Updated on 2020-10-01




Clinical or Laboratorial Research Manuscript