title: Mechanical disruption of dentin collagen fibrils during resin-dentin bond testing.
abstract: OBJECTIVE
  To determine if collagen fibrils on the dentin side of failed resin-dentin interfaces undergo mechanical disruption during microtensile bond testing.
  
  
  METHODS
  Extracted, caries-free human third molars were divided into four groups. The occlusal enamel was removed, leaving a flat dentin surface for bonding. Resin composite buildups were made after the acid-conditioned dentin was bonded with either Single Bond (S) or One-Step (O), and using either moist bonding (M) or air drying for 5 s (D). After storage in water for 24 h, the teeth were vertically sectioned into an array of 0.9 x 0.9 mm resin composite-dentin beams. They were stressed to failure using the nontrimming version of the microtensile bond test. Fractured dentin and resin composite sides of representative beams from each group that exhibited adhesive failures under light microscopy examination were prepared for scanning (SEM) and transmission electron microscopy (TEM).
  
  
  RESULTS
  A two-way ANOVA showed that moist bond strengths were significantly higher than those made to dry dentin (M > D; p < 0.001), but that there was no difference between the adhesives (S vs O; p = 0.547). SEM analysis showed the presence of loose collagen fibrils within fractured hybrid layers in the dry groups, but not in the moist groups. TEM examination of the dry-bonded groups revealed collagen fibrils that were thinner and exhibited abnormally wide interfibrillar spaces when hybrid layers were intact. Within dry-bonded fractured hybrid layers, broad mechanical disruption zones could be seen, consisting of fibrils that were devoid of cross banding, defibrillation of the subfibrillar architecture, and gross disaggregation into microfibrils. In the moist-bonded groups, only short mechanical disruption zones were found along the torn edges of the collagen fibrils. The rest of the fibrils beyond the fracture site were intact and retained their periodicity. Mechanical testing of demineralized matrices yielded a maximum modulus of elasticity of 43.9 +/- 6.1 MPa.
  
  
  CONCLUSIONS
  We speculate that adhesive resin has a protective function for demineralized collagen in well-infiltrated hybrid layers. We propose that both the collagen and resin contribute to load sharing during stress application until the final moment of rupture. On the other hand, collagen fibrils in poorly infiltrated hybrid layers, being unsupported by resin, undergo various degrees of irreversible mechanical disruption depending on how the stress is dissipated. The collagen fibril network has a much lower modulus of elasticity compared to those of resin-infiltrated fibrils or the demineralized dentin.
authors.affiliation: Department of Conservative Dentistry, Pediatric Dentistry and Orthodontics, School of Dentistry, University of Hong Kong, Hong Kong, SAR, China.
authors.forename: F R
authors.initials: FR
authors.lastname: Tay
authors.forename: R M
authors.initials: RM
authors.lastname: Carvalho
authors.forename: C K
authors.initials: CK
authors.lastname: Yiu
authors.forename: N M
authors.initials: NM
authors.lastname: King
authors.forename: Y
authors.initials: Y
authors.lastname: Zhang
authors.forename: K
authors.initials: K
authors.lastname: Agee
authors.forename: S
authors.initials: S
authors.lastname: Bouillaguet
authors.forename: D H
authors.initials: DH
authors.lastname: Pashley
mesh_terms: D000134:Acid Etching, Dental; D000388:Air; D000704:Analysis of Variance; D017438:Bisphenol A-Glycidyl Methacrylate / Q000737:chemistry; D003094:Collagen / Q000502:physiology / Q000648:ultrastructure*; D003188:Composite Resins / Q000737:chemistry*; D001840:Dental Bonding; D003804:Dentin / Q000502:physiology / Q000648:ultrastructure*; D017220:Dentin-Bonding Agents / Q000737:chemistry; D003890:Desiccation; D004548:Elasticity; D006801:Humans; D008422:Materials Testing; D008689:Methacrylates / Q000737:chemistry; D008854:Microscopy, Electron; D008855:Microscopy, Electron, Scanning; D008964:Molar, Third; D013223:Statistics as Topic; D013499:Surface Properties; D013718:Tensile Strength; D014867:Water
chemical_list: C103506:Bis-GMA, BPDM, HEMA dental-bonding resin; D003188:Composite Resins; D017220:Dentin-Bonding Agents; D008689:Methacrylates; C115612:single bond; D014867:Water; D017438:Bisphenol A-Glycidyl Methacrylate; D003094:Collagen