David H. Pashley

Relationship between surface area for adhesion and tensile bond strength--evaluation of a micro-tensile bond test.

OBJECTIVES The purpose of this study was to test the null hypothesis that there is no relationship between the bonded surface area of dentin and the tensile strength of adhesive materials. METHODS The enamel was removed from the occlusal surface of extracted human third molars, and the entire flat surface was covered with resin composite bonded to the dentin to form a flat resin composite crown. Twenty-four hours later, the bonded specimens were sectioned parallel to the long axis of the tooth into 10-20 thin sections whose upper part was composed of resin composite with the lower half being dentin. These small sections were trimmed using a high speed diamond bur into an hourglass shape with the narrowest portion at the bonded interface. Surface area was varied by altering the specimen thickness and width. Tensile bond strength was measured using custom-made grips in a universal testing machine. RESULTS Tensile bond strength was inversely related to bonded surface area. At surface areas below 0.4 mm2, the tensile bond strengths were about 55 MPa for Clearfil Liner Bond 2 (Kuraray Co., Ltd.), 38 MPa for Scotchbond MP (3M Dental Products), and 20 MPa for Vitremer (3M Dental Products). At these small surface areas all of the bond failures were adhesive in nature. SIGNIFICANCE This new method permits measurement of high bond strengths without cohesive failure of dentin. It also permits multiple measurements to be made within a single tooth.

Collagen Degradation by Host-derived Enzymes during Aging

Incompletely infiltrated collagen fibrils in acid-etched dentin are susceptible to degradation. We hypothesize that degradation can occur in the absence of bacteria. Partially demineralized collagen matrices (DCMs) prepared from human dentin were stored in artificial saliva. Control specimens were stored in artificial saliva containing proteolytic enzyme inhibitors, or pure mineral oil. We retrieved them at 24 hrs, 90 and 250 days to examine the extent of degradation of DCM. In the 24-hour experimental and 90- and 250-day control specimens, we observed 5- to 6-μm-thick layers of DCM containing banded collagen fibrils. DCMs were almost completely destroyed in the 250-day experimental specimens, but not when incubated with enzyme inhibitors or mineral oil. Functional enzyme analysis of dentin powder revealed low levels of collagenolytic activity that was inhibited by protease inhibitors or 0.2% chlorhexidine. We hypothesize that collagen degradation occurred over time, via host-derived matrix metalloproteinases that are released slowly over time.

Aggressiveness of contemporary self-etching systems. I: Depth of penetration beyond dentin smear layers.

OBJECTIVE This study examined, with the use of transmission electron microscopy (TEM), the aggressiveness of three self-etching adhesive systems in penetrating dentin smear layers of different thickness. METHODS Dentin disks were produced from extracted human third molars. For the control group, the middle dentin surface was cryofractured to create a bonding surface that was devoid of a smear layer. The experimental teeth were polished with wet 600 or 60-grit SiC paper to produce bonding surfaces with thin and thick smear layers. They were bonded using one of the three self-etching systems: Clearfil Mega Bond (Kuraray), Non-Rinse Conditioner and Prime&Bond NT (Dentsply DeTrey) and Prompt L-Pop (ESPE). Bonded specimens were then demineralized and embedded in epoxy resin for TEM examination. RESULTS For Mega Bond, thin authentic hybrid layers between 0.4-0.5 microm were found. Smear layer and smear plugs were retained as part of the hybridized complex. For Non-Rinse Conditioner/Prime&Bond NT, the authentic hybrid layers were between 1.2-2.2 microm thick. Smear layer and smear plugs were completely dissolved in dentin with thin smear layers, but were partially retained as part of the hybridized complex in those with thick smear layers. For Prompt L-Pop, authentic hybrid layers were 2.5-5 microm thick and smear layer and smear plugs were completely dissolved even in dentin with thick smear layers. SIGNIFICANCE Contemporary self-etching systems may be classified as mild, moderate and aggressive based on their ability to penetrate dentin smear layers and their depth of demineralization into the subsurface dentin. The more aggressive system completely solubilized the smear layer and smear plugs and formed hybrid layers with a thickness approaching those of phosphoric acid conditioned dentin.

Two Modes of Nanoleakage Expression in Single-step Adhesives

Self-etch adhesives that etch, prime, and bond simultaneously should not exhibit incomplete resin infiltration within hybrid layers. We hypothesized that nanoleakage patterns in these systems are artifacts caused by mineral dissolution in mildly acidic silver nitrate. Resin-dentin interfaces bonded with four single-step, self-etch adhesives were examined for nanoleakage by conventional (pH 4.2) and basic ammoniacal (pH 9.5) silver nitrate and prepared for transmission electron microscopy. All adhesives exhibited a reticular mode of nanoleakage within hybrid layers when conventional silver nitrate was used. With ammoniacal silver nitrate, an additional spotted pattern of nanoleakage was observed within adhesive and hybrid layers. The reticular mode of nanoleakage in self-etch adhesives probably represents sites of incomplete water removal that leads to regional suboptimal polymerization. The spotted pattern identified with the use of ammoniacal silver nitrate probably represents potentially permeable regions in the adhesive and hybrid layers that result from the interaction of the basic diamine silver ions with acidic/hydrophilic resin components.

Aggressiveness of contemporary self-etching adhesives: Part II: etching effects on unground enamel

OBJECTIVES The aggressiveness of three self-etching adhesives on unground enamel was investigated. Ultrastructural features and microtensile bond strength were examined, first using these adhesives as both the etching and resin-infiltration components, and then examining their etching efficacy alone through substitution of the proprietary resins with the same control resins. METHODS For SEM examination, buccal, mid-coronal, unground enamel from human extracted bicuspids were etched with either Clearfil Mega Bond (Kuraray), Non-Rinse Conditioner (NRC; Dentsply DeTrey) or Prompt L-Pop (ESPE). Those in the control group were etched with 32% phosphoric acid (Bisco) for 15s. They were all rinsed off prior to examination of the etching efficacy. For TEM examination, the self-etching adhesives were used as recommended. Unground enamel treated with NRC were further bonded using Prime&Bond NT (Dentsply), while those in the etched, control group were bonded using All-Bond 2 (Bisco). Completely demineralized, resin replicas were embedded in epoxy resin for examination of the extent of resin infiltration. For microtensile bond strength evaluation, specimens were first etched and bonded using the self-etching adhesives. A second group of specimens were etched with the self-etching adhesives, rinsed but bonded using a control adhesive. Following restoration with Z100 (3M Dental Products), they were sectioned into beams of uniform cross-sectional areas and stressed to failure. RESULTS Etching patterns of aprismatic enamel, as revealed by SEM, and the subsurface hybrid layer morphology, as revealed by TEM, varied according to the aggressiveness of the self-etching adhesives. Clearfil Mega Bond exhibited the mildest etching patterns, while Prompt L-Pop produced an etching effect that approached that of the total-etch control group. Microtensile bond strength of the three experimental groups were all significantly lower than the control group, but not different from one another. When the self-etching adhesives were replaced with the control adhesive after etching, bond strengths of NRC/Prime&Bond NT and Prompt L-Pop were not significantly different from that of the control group, but were significantly higher than that of Clearfil Mega Bond. SIGNIFICANCE Both etching efficacy and strength of the resins are important contributing factors in bonding of self-etching adhesives to unground enamel.

Dentine permeability and dentine adhesion

OBJECTIVES The objectives of this paper are to review the structure of dentine as it pertains to adhesive bonding and to describe the importance of resin permeation into dentinal tubules and into spaces created between collagen fibrils by acid-etching during resin bonding. The advantages and disadvantages of separate acid-etching, priming and adhesive applications are discussed. DATA SOURCES Although not an exhaustive review, the concepts included in the review were obtained from the dentine bonding literature. STUDY SELECTION Attempts were made to critically evaluate what is known about dentine permeability and adhesion and what remains to be discovered. Speculations were made on a number of controversial issues that are not yet resolved. CONCLUSIONS Acid-etching of dentine produces profound changes in the chemical composition and physical properties of the matrix which can influence the quality of resin-dentine bonds, their strength and perhaps their durability.

Adhesion testing of dentin bonding agents: A review

Adhesion testing of dentin bonding agents was reviewed starting with the adhesion substrate, dentin, the variables involved in etching, priming and bonding, storage variables and testing variables. Several recent reports attempting to standardize many of these variables were discussed. Recent advances in the development of new bonding systems have resulted in bond strengths on the order of 20-30 MPa. At these high bond strengths, most of the bond failure modes have been cohesive in dentin. As this precludes measurement of interfacial bond strength, new testing methods must be developed. One such new method, a microtensile method, was described along with preliminary results that have been obtained. The last decade has produced major advances in dentin bonding. The next decade should prove to be even more exciting.

Chlorhexidine Arrests Subclinical Degradation of Dentin Hybrid Layers in vivo

The recent paradigm that endogenous collagenolytic and gelatinolytic activities derived from acid-etched dentin result in degradation of hybrid layers requires in vivo validation. This study tested the null hypothesis that there is no difference between the degradation of dentin bonded with an etch-and-rinse adhesive and that in conjunction with chlorhexidine, an MMP inhibitor, applied after phosphoric-acid-etching. Contralateral pairs of bonded Class I restorations in primary molars of clinical subjects were retrieved after a six-month period of intra-oral functioning and processed for transmission electron microscopy. Hybrid layers from the chlorhexidine-treated teeth exhibited normal structural integrity of the collagen network. Conversely, abnormal hybrid layers were seen in the control teeth, with progressive disintegration of the fibrillar network, to the extent that it was beyond detection by collagen staining. Self-destruction of collagen matrices occurs rapidly in resin-infiltrated dentin in vivo and may be arrested with the use of chlorhexidine as an MMP inhibitor.

Microtensile bond strength between adhesive cements and root canal dentin.

OBJECTIVES The hypotheses tested were that the bond strength of adhesive cements to root canal dentin (1) would be reduced as a function of configuration factor, polymerization process and type of luting material and (2) would be lowered near the apex of the tooth. METHODS Human canines and premolars were prepared for post cementation using Single Bond/Rely X ARC, ED Primer/Panavia F, C and B Metabond, and Fuji Plus. The specimens were divided into two groups. For intact roots, the posts were luted using standard clinical procedures. For flat roots, the posts were applied directly into flat ground canals. All roots were sectioned into 0.6 mm thick slices, trimmed mesio-distally and stressed to failure at 1 mm/min. The muTBS of each slab was calculated as the force at failure divided by the bonded cross-sectional surface area. The results were compared using a one-way ANOVA and Tukey multiple comparison intervals (alpha=0.05). Least squares linear regression analysis was used to assess the effect of dentin location on bond strength. RESULTS All cements showed significantly (p</=0.05) lower bond strengths in intact vs. flat roots. The muTBS of posts to intact roots were not significantly different for Single Bond/Rely X ARC and Panavia F, but both were significantly lower (p</=0.05) than the bonds produced by C and B Metabond and Fuji Plus cements. For Single Bond/Rely X ARC and Fuji Plus a significant decrease in bond strength was observed in dentin closer to the apex of the root. SIGNIFICANCE Stresses from polymerization shrinkage and problems with adequate access to the root canal complicate the formation of high-strength bonds when cementing endodontic posts with resin cements.

Long-term Durability of Dentin Bonds Made with a Self-etching Primer, in vivo

The long-term durability of bonds between adhesive resins and dentin is of significant importance for the longevity of bonded restorations. We carried out an in vivo one-year study to evaluate the durability of resin-dentin bonds in the oral cavity, as well as to test the hypothesis that the adhesive interface would show morphological changes in vivo over time. Very shallow saucer-shaped dentin cavities were prepared in 12 intact teeth of one Japanese monkey (Macaca fuscata) under general anesthesia. The cavities were restored with Clearfil Liner Bond II and Clearfil Photo Posterior resin composite. The teeth were extracted at three different times: immediately, and 180 and 360 days after placement of the restorations. One day after the monkey was killed, specimens of the three time periods were subjected to the micro-tensile bond test at a crosshead speed of 1 mm/min. The surfaces of the failed bonds were observed under a field emission scanning electron microscope (FE-SEM). Bond strength measurements in this study were successfully performed and were stable at approximately 19 MPa during the one-year testing. Scanning electron microscopic observations of the failed surfaces revealed, at the top of the hybrid layer and within the adhesive resin, porosity which increased over time. Long-term bonds can be assessed in vivo by the combined evaluation of the microtensile bond strength and SEM morphological examination of the adhesive interface.