Michael F. Burrow

Tensile Bond Strength and SEM Evaluation of Caries-affected Dentin Using Dentin Adhesives

Tensile bond strength measurements are commonly used for the evaluation of dentin adhesive systems. Most tests are performed using extracted non-carious human or bovine dentin. However, the adhesion of resins to caries-affected dentin is still unclear. The objectives of this study were to test the hypothesis that bonding to caries-affected dentin is inferior to bonding to normal dentin, and that the quality of the hybrid layer plays a major role in creating good adhesion. We used a micro-tensile bond strength test to compare test bond strengths made to either caries-affected dentin or normal dentin, using three commercial adhesive systems (All Bond 2, Scotchbond Multi-Purpose, and Clearfil Liner Bond II). For scanning electron microscopy, the polished interfaces between the adhesive bond and dentin were subjected to brief exposure to 10% phosphoric acid solution and 5% sodium hypochlorite, so that the quality of the hybrid layers could be observed. Bonding to normal dentin with either All Bond 2 (26.9 ± 8.8 MPa) or Clearfil Liner Bond II (29.5 ± 10.9 MPa) showed tensile bond strengths higher than those to caries-affected dentin (13.0 ± 3.6 MPa and 14.0 ± 4.3 MPa, respectively). The tensile bond strengths obtained with Scotchbond Multi-Purpose were similar in normal and caries-affected dentin (20.3 ± 5.5 MPa and 18.5 ± 4.0 MPa, respectively). The hybrid layers created by All Bond 2 in normal dentin and by Clearfil Liner Bond II in normal or caries-affected dentin showed phosphoric acid and sodium hypochlorite resistance, whereas the hybrid layers created by All Bond 2 in caries-affected dentin and those created by Scotchbond Multi-Purpose to normal and caries-affected dentin showed partial susceptibility to the acid and sodium hypochlorite treatment. The results indicate that the strength of adhesion to dentin depends upon both the adhesive system used and the type of dentin. Moreover, the quality of the hybrid layer may not always contribute significantly to tensile bond strength.

New Approaches to Enhanced Remineralization of Tooth Enamel

Dental caries is a highly prevalent diet-related disease and is a major public health problem. A goal of modern dentistry is to manage non-cavitated caries lesions non-invasively through remineralization in an attempt to prevent disease progression and improve aesthetics, strength, and function. Remineralization is defined as the process whereby calcium and phosphate ions are supplied from a source external to the tooth to promote ion deposition into crystal voids in demineralized enamel, to produce net mineral gain. Recently, a range of novel calcium-phosphate-based remineralization delivery systems has been developed for clinical application. These delivery systems include crystalline, unstabilized amorphous, or stabilized amorphous formulations of calcium phosphate. These systems are reviewed, and the technology with the most scientific evidence to support its clinical use is the remineralizing system utilizing casein phosphopeptides to stabilize and deliver bioavailable calcium, phosphate, and fluoride ions. The recent clinical evidence for this technology is presented and the mechanism of action discussed. Biomimetic approaches to stabilization of bioavailable calcium, phosphate, and fluoride ions and the localization of these ions to non-cavitated caries lesions for controlled remineralization show promise for the non-invasive management of dental caries.

Dentin bond durability after three years using a dentin bonding agent with and without priming

OBJECTIVES This three-year study was conducted to evaluate the tensile bond strengths of a dual-cured bonding resin, with and without priming, to bovine dentin. METHODS Superficial bovine dentin was conditioned with 37% phosphoric acid and left unprimed (control) or was primed with 5-NMSA. Clearfil Photobond (Kuraray Co., Japan) was placed and light-cured, a layer of Protect Liner (Kuraray Co.) was applied, cured, then covered with Photo Clearfil Bright (Kurary Co.) resin composite and cured. Bonds were stressed in tension to failure at 1 d, 1 mon, 3 mon, 6 mon, 1 y and 3 y after preparation. Ten specimens were made for each group. Results were analyzed using one-way ANOVA and Duncans multiple range test. Visual and SEM observations determined mode of failure and were analyzed using the Mann-Whitney U-test. Separate 1 d and 3 y specimens were fractured across the bonded interface and observed using a Field Emission SEM. After observation, the photomicrographs were compared for visual qualitative changes between the two time periods. RESULTS The control (non-primed) group showed only a small decrease in bond strengths over 3 y, but in the primed group, a significant decrease was observed (p < 0.05). The bond strength of the non-primed group (5.2 MPa) was less than the primed group (10.6 MPa) at 1 d (p < 0.01), but by 3 y, the bonds of both groups were similar, 4.3 MPa and 5.5 MPa, respectively. Fractography indicated that only adhesive failure occurred in the control group. Failure in the primed group was cohesive in dentin initially, but shifted to the base or top of the hybrid layer after 1 y. Field Emission SEM observations showed hybrid layer formation in the primed group, but minimal resin infiltration in the control group. SIGNIFICANCE Initially greater bond strengths were obtained for the primed group compared to the unprimed group (p < 0.01). However, by 3 y, the bond strength had decreased markedly in the primed group (p < 0.01), being almost the same for both groups. It was concluded that priming may only be useful to achieve strong bonding in the short term. These results may have significant implications related to clinical longevity of restorations.

Effect of intrinsic wetness and regional difference on dentin bond strength

OBJECTIVES The aim of this investigation was to determine the influence of intrinsic wetness on regional bond strengths of adhesive resins to dentin. METHODS Human caries-free third molars were randomly divided into three groups for bonding: Group 1--no pulpal pressure; Group 2--pulpal pressure of 15 cm H2O; and Group 3--dentin dried overnight in a desiccator. Clearfil Liner Bond II (Kuraray) or One Step (Bisco) adhesive resins systems were applied to the flat dentin surfaces and the teeth were restored with APX resin composite (Kuraray). After 24 h in water at 37 degrees C, the specimens were sectioned into 0.7 mm thick slabs and divided into three regional subgroups according to the remaining dentin thickness and visual criteria: pulp horn, center, and periphery. The slabs were then trimmed for the micro-tensile bond test and subjected to a tensile force and crosshead of 1 mm/min. The data were analyzed with ANOVA and Fishers PLSD test at a confidence level of 95%. The fracture modes were determined under a scanning electron microscope (JXA-840, JEOL, Japan). RESULTS No significant regional difference was observed for the Group 1 and 2 specimens restored with Clearfil Liner Bond II (p > 0.05). However, bond strengths significantly decreased at the pulp horn region of the Group 1 and 2 specimens restored with One Step (p > 0.01). All bond strengths of Group 3 decreased significantly and regional differences were not evident (p > 0.05). SIGNIFICANCE The dentin adhesive system should be chosen according to the substrate and region to be bonded, since bond strengths can vary according to the intrinsic wetness, region, and the adhesive system.

The effect of dentine location and tubule orientation on the bond strengths between resin and dentine

This study determined the influence of dentine structure on the micro-tensile bond strengths between resin and dentine of two different dentine adhesive systems (Single Bond, 3M Dental Products, St Paul, MN; MF-102 (experimental self-etching primer), GC Corporation, Tokyo, Japan). The study was separated into two main parts: bond strength measurement and investigation of the bonding interface. Twenty-two human premolars were used for the bond strength measurement. Each tooth was cut vertically, separating the tooth into mesio-distal halves. One half of the tooth was used to bond to a surface perpendicular to the dentinal tubules and other half to bond to a surface parallel to the tubules. For each half, six locations of dentine were bonded. Each material was used in accordance to the manufacturers directions. Cylindrical hourglass-shaped specimens of 1.2 mm diameter at the bonded interface were manufactured. The bonds were stressed in tension at a crosshead speed of 1 mm/min. Mean bond strengths were compared using LSD, one-way ANOVA, and Students t-test. The fractured surfaces were examined under a scanning electron microscope, and the frequency of fracture modes was compared using the Kruskal-Wallis and Mann-Whitney U tests. For the investigation of the bonded interface, four teeth were prepared by the same procedure used for the bond test specimens. The bonded interfaces were observed after an acid-base treatment or fracturing across the bonded interface, prior to investigation with a field-emission scanning electron microscope. For Single Bond, the bond strengths for mid-root dentine were significantly lower than for other locations (p < 0.05). For MF-102, there was no significant difference for all locations (p > 0.05). MF-102 bonded well to all locations of dentine while Single Bond showed a porous zone at the base of the hybrid layer. The bonds were not influenced by tubule orientation. The results indicate that the bond for Single Bond may be affected by its ability to penetrate demineralised dentine in different locations of a tooth. The self-etching primer of MF-102 produces a good bond and is independent of the position on the tooth.

A light curing method for improving marginal sealing and cavity wall adaptation of resin composite restorations.

OBJECTIVE The aim of this study was to evaluate whether the method of light curing could influence: (a) marginal sealing and resin composite adaptation to the cavity wall; (b) polymerization contraction rate; and (c) the hardness at the top and bottom surfaces of a body of resin composite. METHODS Standard cylindrical cavities, 1mm deep and 3mm in diameter were prepared on flat superficial dentin surfaces in bovine teeth. The teeth were bonded with one of two adhesive systems (Clearfil Photo Bond, and Super-Bond D Liner) and filled with a hybrid resin composite. The resins were cured using three light intensities of 600, 270 and 20mW/cm(2), and various curing times. After thermal cycling, the specimens were subjected to a dye penetration test to evaluate marginal sealing and adaptation of the resin composite to the cavity walls. In addition, using the same curing conditions, the rate of polymerization contraction was measured. The difference of hardness over time of composite specimens was measured using Knoop hardness measurements taken at the top and bottom surfaces of resin specimens made in a Teflon mold the same dimensions as the cavity prepared in dentin. RESULTS When the composite was light cured with an initial light intensity of 270mW/cm(2) for 10s, a 5s interval then a light intensity of 600mW/cm(2) for 50s, the best marginal sealing and cavity wall adaptation was observed compared with the other curing modes. Earlier hardening occurred at the resin composite base compared with the top surface of the composite, and most of the polymerization contraction was completed during the initial flowable stage of the resin composite. All other methods demonstrated results with some degree of marginal opening and cavity wall gap formation, the worst being 600mW/s for 60s. SIGNIFICANCE The use of a low initial light intensity (270mW/cm(2)) for 10s followed by high intensity light (600mW/cm(2)) for 50s provides the best adaptation of resin composite to cavity walls and possibly the least polymerization contraction stress.

The influence of age and depth of dentin on bonding

OBJECTIVES The purpose of this study was to investigate what influence the two variables of dentin depth and age may have on the tensile bond strengths of three bonding systems. METHODS Dentin discs prepared from human molars were divided into young and old, superficial and deep surfaces. Three bonding systems, Scotchbond Multi-purpose (3M Dental Products), Superbond D-liner (Sun Medical Co.), and Liner Bond II (Kuraray Co.) were the materials tested for tensile bond strength. In addition, the structural variation of the resin-impregnated, or hybrid, layer was compared among the two variables and three bonding systems. RESULTS Tensile bond strengths exceeding 10 MPa were obtained for all materials. After ANOVA, an effect on tensile bond strength could be attributed to dentin age or depth for only Superbond D-liner used on deep-young dentin as compared with old-superficial dentin. All other group comparisons failed to show any variation between dentin depth or age. However, specimens bonded to deeper dentin showed slightly lower strengths. SEM observations showed thicker resin-impregnated layers for Scotchbond MP and Superbond D-liner compared with Liner Bond II. Liner Bond II exhibited a thinner and more diffuse resin-impregnated layer, believed to be due to the different dentin conditioning method. SIGNIFICANCE Dentin age or depth may not show as great an influence on bond strengths with the newer type of bonding systems. The resin-impregnated layer quality, rather than thickness, is believed to be the most important factor for obtaining high tensile bond strengths.

A comparison of microtensile bond strengths of several dentin bonding systems to primary and permanent dentin.

OBJECTIVES Limited information exists with regard to the adhesive ability of glass ionomer cements (GIC) and recently developed resin-based dentin bond systems to primary dentin. The aim of this study was to compare the microtensile bond strength of a conventional GIC (Fuji IX), a resin-modified GIC (Fuji II LC), and two resin-based dentin adhesives (Prime and Bond NT with NRC and Single Bond). The bonded interfaces were also observed using field emission electron microscopy(FE-SEM). METHODS Microtensile bond test specimens were prepared on superficial dentin of primary and permanent molars. The specimens were bonded according to each manufacturers instructions except for Prime and Bond NT/NRC which used Silux Plus resin composite instead of Dyract. Hour-glass shaped specimens were created (diameter of 1.2+/-0.02 mm) and stressed in tension at a crosshead speed of 1mm/min. Results were analyzed using two-way ANOVA and LSD test, fracture modes were analyzed using the Mann-Whitney U-test and Kruskall-Wallis test. Twelve specimens were prepared for each material on primary and permanent dentin. Samples were prepared in the same manner, then critical point dried, fractured and sputter-coated for the FE-SEM observations. RESULTS Two-way ANOVA showed the overall bond strengths were greater for the permanent dentin compared with primary dentin. However, for individual material comparisons no differences among the bond strengths to primary and permanent dentin for Fuji IX (9.7, 12.2 MPa), Fuji II LC (16, 20.1 MPa), Prime & Bond NT/NRC (18.1, 21.6 MPa) and Single Bond (18.2, 21.6 MPa), were detected. However, Fuji IX bond strengths were significantly lower than the other systems tested when bonded to either primary or permanent dentin (p<0.05). Failure mode showed cohesive failure of GIC and mostly adhesive failure for the resin-based adhesives. The FE-SEM observations showed hybrid-like layer formation for the GIC materials and hybrid layer formation for the resin-based adhesives. SIGNIFICANCE The materials tested would be suitable for bonding to either primary or permanent dentin, but the resin-modified GIC or resin-based systems are likely to provide a stronger bond than the conventional GIC, Fuji IX.

The influence of storage solution on dentin bond durability of resin cement

OBJECTIVES This study was conducted to determine the influence of storage solution on the bond durability of three resin cements to bovine dentin over the period of 1 year. METHODS Ten bovine dentin specimens were tested for shear bond strength with each material (Panavia 21, Kuraray Co.; BISTITE, Tokuyama Co; MASA Bond, Sun Medical Co.) and storage mode, listed below. Four storage environments were studied as follows: water changed every day for 1 year; water unchanged for 1 year; Phosphate Buffered Saline (PBS) changed every week over 1 year; PBS unchanged for 1 year. Ten teeth were also tested for each material at 1 day as a control. The mode of failure was classified after fracture of the bonds by SEM observation. The means of the bond strengths were compared statistically by two-way ANOVA and Fishers PLSD test (p < 0.05). Results for the mode of fracture were analyzed using the Mann-Whitney U test. RESULTS Although there was no statistical difference in the mean bond strengths between the water and PBS storage solutions (p > 0.05) in all cements, the results for the shear bond strengths in the changed storage solution groups were significantly lower than those where the storage solution remained unchanged (p < 0.05). There were statistical differences between the 1 day results and the changed water groups among all cements (p < 0.05). SIGNIFICANCE The storage condition influenced the long-term durability of dentin bonding with resin cements.

Nanoleakage patterns of four dentin bonding systems

OBJECTIVES The purpose of this study was to evaluate the nanoleakage patterns of four dentin bonding systems. METHODS The dentin bonding systems used in this study were: Single Bond, One Coat Bond, Prime & Bond NT/Non Rinse Conditioner (NRC), and PermaQuik. Flat occlusal dentin surfaces from extracted human molars were finished with wet 600-grit silicon carbide paper, and bonded with one of the dentin bonding systems. After 24 h storage at 37 degrees C in water, margins were finished with polishing discs and the surrounding tooth surfaces coated with nail varnish. The samples were immersed in a 50% (w/v) solution of silver nitrate for 24 h, and exposed to photodeveloping solution for 8 h. The samples were cut longitudinally, polished, and mounted on stubs, carbon coated and observed in a Field Emission-SEM using backscattered electron mode. RESULTS Different nanoleakage patterns were observed with the different adhesive systems. However, accumulations of silver particles were often noted at the base of the hybrid layer for all materials. Single Bond and One Coat Bond demonstrated uptake of silver particles both within the hybrid layer and the adhesive resin. Prime & Bond NT/NRC showed silver staining throughout almost the entire thickness of the hybrid layer. The leakage pattern of PermaQuik revealed loose silver deposition within the hybrid layer. The composition of each adhesive system may play a role in forming the different leakage patterns. SIGNIFICANCE The current dentin bonding systems used in this study do not achieve perfect sealing at the restoration/dentin interface, which may influence the durability of the bond to dentin.