Open Access, Peer-reviewed
eISSN 2234-7666
    J Korean Acad Conserv Dent. 2007 May;32(3):208-221. Korean.
    Published online May 31, 2007.
    https://doi.org/10.5395/JKACD.2007.32.3.208
    Copyright © 2007 Korean Academy of Conservative Dentistry
    Original Article

    A study on fractural behavior of dentin-resin interface

    Gil-Joo Ryu, Gi-Woon Choi, Sang-Jin Park and Kyung-Kyu Choi
      • Department of Conservative Dentistry, Division of Dentistry, Graduate of Kyung Hee University, Korea.
    • Corresponding Author: Kyoung-Kyu Choi. Professor of Division of Dentistry, Graduate school of KyungHee University, 1, Hoegi Dong, Dongdaemun Gu, Seoul, Korea, 130-701. Tel: 82-2-958-9337, Email: choikkyu@khu.ac.kr
    Received March 14, 2007; Revised April 20, 2007; Accepted April 24, 2007.

    This is an Open Access article distributed under the terms of the Creative Commons Attribution Non-Commercial License (http://creativecommons.org/licenses/by-nc/3.0/) which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.

    Abstract

    The fracture toughness test is believed as a clinically relevant method for assessing the fracture resistance of the dentinal restoratives. The objectives of this study were to measure the fracture toughness (K1C) and microtensile bond strength of dentin-resin composite interface and compare their relationship for their use in evaluation of the integrity of the dentin-resin bond.

    A minimum of six short-rod specimens for fracture toughness test and fifteen specimens for microtensile bond strength test was fabricated for each group of materials used. After all specimens storing for 24 hours in distilled water at 37℃, they were tensile-loaded with an EZ tester universal testing machin. Statistical analysis was performed using ANOVA and Tukey's test at the 95% confidence level, Pearson's coefficient was used to verify the correlation between the mean of fracture toughness and microtensile bond strength. FE-SEM was employed on fractured surface to describe the crack propagation.

    Fracture toughness value of Clearfil SE Bond (SE) was the highest, followed by Adper Single Bond 2 (SB), OptiBond Solo (OB), ONE-STEP PLUS (OS), ScotchBond Multi-purpose (SM) and there was significant difference between SE and other 4 groups (p < 0.05). There were, however, no significant difference among SB, OB, OS, SM (p > 0.05). Microtensile bond strength of SE was the highest, followed by SB, OB, SM, OS and OS only showed significant lower value (p < 0.05). There was no correlation between fracture toughness and microtensile bond strength values. FE-SEM examination revealed that dentin bonding agent showed different film thickness and different failure pattern according to the film thickness.

    From the limited results of this study, it was noted that there was statistically no correlation between K1C and µTBS. We can conclude that for obtaining the reliability of bond strength test of dentin bonding agent, we must pay more attention to the test procedure and its profound scrutiny.

    Keywords
    Fracture toughness; Microtensile bond strength; Short-rod specimen; Dentin-resin composite interface; FE-SEM; Dentin bonding agent

    Figures

    Figure 1
    Schematic geography of fracture toughness specimen.

    Figure 2
    Each component of the mold.

    Figure 3
    Assembled mold.

    Figure 4
    K1C value of experimental groups.

    Figure 5
    µTBS value of experimental groups.

    Figure 6
    The resin surface of fractured K1C specimen of SM group (× 50).

    It showed that bevel formed by spacer and crack occurred along the bevel.

    C: Composite resin, CAD: Composite adhered to dentin

    Figure 7
    The resin surface of fractured K1C specimen of OB group (× 500).

    The arrows showed that crack formed along the bevel move into the adhesive surface (see the black arrows).

    Figure 8
    The dentin surface of fractured K1C specimen of SB group (× 250).

    It revealed that the failure occurred between resin-infiltrated layer and adhesive layer.

    At the tip of the bonded surface(white arrow), failure occurred mainly within the adhesive resin layer.

    D: dentin, AR: Adhesive resin layer

    Figure 9
    The cross-sectional SEM photograph of bonded surface of SM group (× 1,000).

    The thickness of adhesive layer was 40 ~ 55 µm and dentinal tubules were running oblique direction.

    The adhesive layer was relatively thick and uniform.

    Figure 10
    The cross-sectional SEM photograph of bonded surface of SB group (× 3,000).

    The thickness of adhesive layer was 14 ~ 25 µm and the dentinal tubules were filled with resin tags.

    Some of the dentinal tubules were empty, some of the resin tags had many branches.

    RT: Resin tag, ID: Intertubular dentin, PD: Peritubular dentin

    Figure 11
    The cross-sectional SEM photograph of bonded surface of SE group (× 1,000).

    The thickness of adhesive layer was 50 ~ 60 µm and it was the thickest adhesive resin layer among the experimental groups.

    Most of dentinal tubules were filled with resin tags.

    Figure 12
    The resin surface (left) and dentin surface (right) of fractured SM group (× 2,000).

    Bond failure occurred predominantly between the resin-infiltrated layer and adhesive resin.

    The orifices of dentinal tubules were not seen clearly and irregular adhesive resin layer was showed at the dentin surface of fractured specimen.

    Figure 13
    The resin surface (left) and dentin surface (right) of fractured OS group (× 2,000).

    Many broken resin tags were seen on the both specimens,

    the fracture of the resin tags mainly occurred at the upper part of the resin-infiltrated layer.

    RT: resin tag, DT: dentinal tubule

    Figure 14
    The resin surface (left) and dentin surface (right) of fractured OB group (× 2,000).

    On the resin surface, many resin tags and adhesive resin layer was seen partially.

    The dentin surface of the fractured specimen showed relatively smooth appearance and many dentinal tubules filled with resin tags. The fracture of resin tags were occurred at the orifices of the dentinal tubules.

    AR: adhesive resin layer, RT: resin tag

    Figure 15
    The resin surface (left) and dentin surface (right) of fractured SB group (× 2,000).

    Relatively short broken resin tags were seen on the resin side.

    Irregular adhesive resin layer and dentinal tubules obstructed with resin tag or covered with adhesive resin were seen on the dentin side of the fractured specimen.

    Figure 16
    The resin surface (left) and dentin surface (right) of fractured SE group (× 2,000).

    Resin tags and dentinal tubules were seen rarely.

    Both sides showed very irregular appearance and bond failure occurred predominantly within the adhesive resin layer.

    Tables

    Table 1
    Dentin bonding agents (DBA) used in this study and their compositions

    Table 2
    Instructions for use of dentin bonding agents(DBA)

    Table 3
    Fracture toughness(Mean ± S.D., MPa·m1/2) of 5 experimental groups

    Table 4
    Microtensile bond strength(Mean ± S.D., MPa) of 5 experimental groups

    References

      1. Nakabayashi N. Resin reinforced dentin due to infiltration of monomers into the dentin at the adhesive interface. J Dent Mater 1982;1:78–81.
      1. Van Meerbeek B, Inokoshi S, Braem M, Lambrechts P, Vanherle G. Morphological aspects of the resin-dentin interdiffusion zone with different dentin adhesive systems. J Dent Res 1992;71:1530–1540.
      1. Eick JD, Robinson SJ, Chappell RP, Cobb CM, Spencer P. The dentinal surface ; its influence on dentinal adhesion. Part III. Quintessence Int 1993;24:571–582.
      1. Van Meerbeek B, Dhem A, Goret-Nicaise M, Braem M, Lambrechts P, Vanherle G. Comparative SEM and TEM examination of the ultrastructure of the resin-dentin interdiffusion zone. J Dent Res 1993;72:495–501.
      1. Tay FR, Gwinnett AJ, Pang KM, Wei SHY. Structural evidence of a sealed tissue interface with a total-etch wet-bonding technique in vivo. J Dent Res 1994;73:629–636.
      1. Van Meerbeek B, Mohrbacher H, Celis JP, Roos JR, Braem M, Lambrechts P, Vanherle G. Chemical characterization of the resin-dentin interface by micro-Raman spectroscopy. J Dent Res 1993;72:1423–1428.
      1. Eick JD, Miller RG, Robinson SJ, Bowles CQ, Gutshall PL, Chappelow CC. Quantitative analysis of the dentin adhesive interface by Auger spectroscopy. J Dent Res 1996;75:1027–1033.
      1. Kruger MB. Raman mapping of the dentin/adhesive interface. Appl Spectrosc 1996;50:1500–1504.
      1. Burke FJT, McCaughey AD. The four generations of dentin bonding. Am J Dent 1995;8:88–92.
      1. Pashley DH, Sano H, Ciucchi B, Yoshiyama M, Carvalho RM. Adhesion testing of dentin bonding agents : a reviews. Dent Mater 1995;11:117–125.
      1. Swift EJ Jr, Perdigão J, Heymann HO. Bonding to enamel and dentin : a brief history and state of the art. Quintessence Int 1995;26:95–110.
      1. Heymann HO, Sturdevant JR, Bayne S, Wilder AD, Sluder TB, Brunson WD. Examining tooth flexure effects on cervical restorations : A two-year clinical study. J Am Dent Assoc 1991;122:41–47.
      1. Duke ES, Robbins JW, Schwartz RS, Summitt JB, Conn LJ. Clinical and interfacial laboratory evaluation of a bonding agent in cervical abrasions. Am J Dent 1994;7:307–311.
      1. van Dijken JWV. Clinical evaluation of four dentin bonding agents in class V abrasion lesions : a four-year follow-up. Dent mater 1994;10:319–324.
      1. Van Meerbeek B, Peumans M, Verschueren M, Gladys S, Braem M, Lambrechts P, Vanherle G. Clinical status of ten dentin adhesive systems. J Dent Res 1994;73:1690–1702.
      1. Yamaguchi R, Powers JM, Dennison JB. Parameters affecting in vitro bond strength of composites to enamel and dentin. Dent Mater 1989;5:153–156.
      1. Chappell RP, Eick JD. Shear bond strength and scanning electron microscopic observation of current dentinal adhesives. Quintessence Int 1994;25:359–368.
      1. Sorensen JA, Dixit NV. In vitro shear bond strength of dentin adhesives. Int J Prosthodont 1991;4:117–125.
      1. Söderholm KJ. Correlation of in vivo and in vitro performance of adhesive restorative materials : a report of the ASC MD156 Task Group on Test Methods for the Adhesion of Restorative Materials. Dent Mater 1991;7:74–83.
      1. Retief DH. Standardizing laboratory adhesion tests. Am J Dent 1991;4:231–236.
      1. Tyas MJ. Guest editorial: reliability and validity in dental materials testing. J Dent Res 1991;70:1471.
      1. Jendresen MD, Allen EP, Bayne SC, Hansson TL, Klooster J, Preston JD. Report of the committee on scientific investigation of the American Academy of Restorative Dentistry. J Prosthet Dent 1992;68:137–190.
      1. van Noort R, Noroozi S, Howard IC, Cardew G. A critique of bond strength measurements. J Dent 1989;17:61–67.
      1. van Noort R, Cardew GE, Howard IC, Noroozi S. The effect of local interfacial geometry on the measurement of the tensile bond strength to dentin. J Dent Res 1991;70:889–893.
      1. Wang CT, Pilliar RM. Bond cement bonding-interfacial fracture toughness determination. Clin Mater 1989;4:135–153.
      1. Charalambides PG, Cao HC, Lund J, Evans AG. Development of a test method for measuring the mixed mode fracture resistance of bimaterial interfaces. Mech Mater 1990;8:269–283.
      1. Tam LE, Pilliar RM. Fracture toughness of dentin/resin-composite adhesive interfaces. J Dent Res 1993;72:953–959.
      1. Lin CP, Douglas WH. Failure mechanisms at the human dentin-resin interface: A fracture mechanics approach. J Biomech 1994;27:1037–1047.
      1. Hertzberg RW. In: Deformation and fracture mechanics of engineering materials. 2nd ed. New York: J. Wiley; 1983.
      1. Kelly JR. Perspectives on strength. Dent Mater 1995;11(2):103–110.
      1. Beaumont PWR, Young RJ. Slow crack growth in acrylic bone cement. J Biomed Mater Res 1975;9:423–439.
      1. Mecholsky JJ. Fracture mechanics principles. Dent Mater 1995;11(2):111–112.
      1. Griffith AA. The phenomena of rupture and flow in solids. Philos Trans R Soc Lond A 1920;221:163–198.
      1. Ferracane JL, Antonio RC, Matsumoto H. Variables affecting the fracture toughness of dental composites. J Dent Res 1987;66(6):1140–1145.
      1. Lloyd CH, Mitchell L. The fracture toughness of tooth coloured restorative materials. J Oral Rehabil 1984;11:257–272.
      1. Ferracane JL, Berge HX. Fracture toughness of experimental dental composites aged in ethanol. J Dent Res 1995;74(7):1418–1423.
      1. Young RJ, Beaumont PWR. Failure of brittle polymers by slow crack growth. Part 2. Failure processes in a silica particle-filled epoxy resin composite. J Mater Sci 1975;10:1343–1350.
      1. Kim KH, Park JH, Imai Y, Kishi T. Microfracture mechanisms of dental resin composites containing spherically-shaped filler particles. J Dent Res 1994;73(2):499–504.
      1. Lloyd CH, Adamson M. The development of fracture toughness and fracture strength in posterior restorative materials. Dent Mater 1987;3:225–231.
      1. Goldman M. Fracture properties of composite and glass ionomer dental restorative materials. J Biomed Mater Res 1985;19:771–783.
      1. de Groot R, Van Elst HC, Peters MC. Fracture-mechanics parameters of the composite-enamel bond. J Dent Res 1990;69:31–35.
      1. Barker LM. A simplified method for measuring plane strain fracture toughness. Eng Fract Mech 1977;9:361–369.
      1. Bubsey RT, Munz D, Pierce WS, Shannon JL. Compliance calibration of the short rod chevron-notch specimen for fracture toughness testing of brittle material. Int J Frac 1982:125–133.
      1. Van Meerbeek B, De Munck J, Yoshida Y, Inoue S, Vargas M, Vijay P, Van Landuyt K, Lambrechts P, Vanherle G. Adhesion to Enamel and Dentin : Current Status and Future Challenges. Oper Dent 2003;28(3):215–235.
      1. Chung SM, Yap AU, Tsai KT, Yap FL. Elastic modulus of resin-based dental restorative materials : a microindentation approach. J Biomed Mater Res B Appl Biomater 2005;72(2):246–253.
      1. Fujishima A, Ferracane JL. Comparison of four modes of fracture toughness testing for dental composites. Dent Mater 1996;12:38–43.
      1. Van Meerbeek B, De Munck J, Yoshida Y, Shirai K, Inoue S, Shiatani H, Lambrechts P. Chemical bonding potential of adhesive materials to hydroxyapatite. J Dent Res 2003;82(Special Issue)
      1. Tam LE, Khoshand S, Pilliar RM. Fracture resistance of dentin-composite interfaces using different adhesive resin layers. J Dent 2001;29:217–225.
      1. Ai H, Nagai M. Effect of the adhesive layer thickness on the fracture toughness of dental adhesive resin. Dent Mater J 2000;19(2):153–163.
      1. Rueggeberg FA, Margeson DH. The effect of oxygen inhibition on the unfilled/filled composite system. J Dent Res 1990;69:1652–1658.
      1. Finger WJ, Lee KS, Podszun W. Monomers with low oxygen inhibition as enamel/dentin adhesives. Dent Mater 1996;12:256–261.
      1. Miyazaki M, Ando S, Hinoura K, Onose H, Moore BK. Influence of filler addition to bonding agents on shear bond strength to bovine dentin. Dent Mater 1995;11:234–238.
      1. Nunes MF, Swift EJ, Perdigăo J. Effects of adhesive composition on microtensile bond strength to human dentin. Am J Dent 2001;14(6):340–343.
      1. Frankenberger R, Lopes M, Perdigão J, Ambrose WW, Rosa BT. The use of flowable composites as filled adhesives. Dent Mater 2002;18(3):227–238.
      1. Retief DH, Wendt SL, Bradley EL. Effect of adhesive thickness on the shear bond strength of Scotchbond 2/Silux to dentin. Am J Dent 1989;2(6):341–344.
      1. Leloup G, D'hoore W, Bouter D, Degrange M, Vreven J. Meta-analytical Review of Factors Involves in Dentin Adherence. J Dent Res 2001;80(7):1605–1614.
      1. Tantbirojn D, Cheng YS, Versluis A, Hodges JS, Douglas WH. Nominal Shear or Fracture Mechanics in the Assessment of Composite-Dentin Adhesion? J Dent Res 2000;79(1):41–48.
    Cited by
    Crossref 1
    Google Scholar 
    MeSH Terms
    Dentin
    Water
    Metrics
    Share
    Figures
    slide
    slide
    slide
    slide
    slide
    slide
    slide
    slide
    slide
    slide
    slide
    slide
    slide
    slide
    slide
    slide

    1 / 16

    Tables
    slide
    slide
    slide
    slide

    1 / 4

    PERMALINK