Failure analysis of adhesive restorations with SEM and OCT: from marginal gaps to restoration loss.

OBJECTIVE: The objective of this study was to analyse the failure mode of adhesive interfaces by comparing OCT and scanning electron microscope (SEM) analysis of class V restoration margins located on enamel and dentin. MATERIALS AND METHODS: Three groups were tested that differed in the application of a 3-step etch-and-rinse adhesive system (OptiBond FL) prior to cavity filling with restorative composite resin (Clearfil AP-X). After tooth restoration and polishing, the samples were loaded in a fatigue machine, and adhesive interfaces were evaluated with OCT and SEM. RESULTS: Important and complementary information could be obtained with OCT analysis in respect to how marginal defects can propagate inside the cavity, compromising the restoration's long-term performance. A self-etching effect was observed with OptiBond FL due to the presence of an acidic primer (GPDM) within its composition. Our results could show that areas of bonding and gaps coexisted within the same restoration. CONCLUSIONS: When marginal imperfections, or non-continuous margins, were detected by SEM, also imperfections beneath the surface could be observed at the tooth-restoration interface with OCT. Restoration loss occurred above the borderline of 50% of marginal gaps on enamel and dentin. CLINICAL RELEVANCE: Marginal discrepancies of adhesive restorations can propagate inside the cavity and lead to restoration loss.

Corrosion-Effected Bond Behavior between PVA-Fiber-Reinforced Concrete and Steel Rebar under Chloride Environment.

Corrosion-effected bond behavior between polyvinyl-alcohol-fiber-reinforced concrete and steel rebar under a chloride environment is the experimental subject studied in the present work. Twenty-four pull-out specimens are designed and subjected firstly to an accelerated corrosion test. The effects of polyvinyl alcohol fibers on the cracking behavior, chloride penetration of concrete members and the corrosion loss of steel rebars during the corrosion test are discussed. After this, these corroded specimens are subjected to a pull-out test. The failure mode, the bond-slip curves and the typical bond-stress values are measured during the test. The effects of polyvinyl alcohol fibers and corrosion loss on bond behavior between polyvinyl-alcohol-fiber-reinforced concrete and steel rebar are clarified. Results show that the polyvinyl-alcohol-fiber-reinforced concrete exhibits worse resistance to corrosion damage than plain concrete. The cracking width, chloride penetration depth in concrete and the corrosion loss of steel rebar are more serious for the specimens with more polyvinyl alcohol fibers. The polyvinyl alcohol fibers also negatively affect bonding in ascending branches for both the specimens, but improve the bonding in descending branches after peak stress in the case of splitting. In the present test, the bond strength of corrosive specimens is increased slightly and then decreases gradually with the deepening of corrosion loss. The failures of specimens change from pull-out to splitting-pull-out as the corrosion time exceeds 30 days. Compared with uncorroded specimens, the maximum degradation of bond strength is about 50.1% when the corrosion is increased from 0% to 15%.

Effect of MMP Inhibitors on the Bond Strength of Fibre Posts After Ageing.

AIM: This in vitro study aimed to evaluate the effect of matrix metalloproteinase (MMP) inhibitors on the bond strength of resin-cemented fibre posts to radicular dentin under an aged-loaded condition. MATERIALS AND METHODS: Radicular dentin was prepared and irrigated by MMP inhibitor solution after root canal obturation in 60 extracted single-rooted teeth based on 6 groups: (1) 2% chlorhexidine (CHX) + loaded; (2) CHX + unloaded; (3) 0.5% benzalkonium chloride (BAC) + loaded; (4) BAC + unloaded; (5) 17% ethylenediaminetetraacetic acid (EDTA) + loaded; and (6) EDTA + unloaded. After final rinsing, all specimens were sliced cross-sectionally and kept in a water bath for 12 months of ageing. Groups 1, 3, and 5 were subjected to cyclic loading. Push-out tests were conducted using a universal testing machine, and failure mode was examined. The data were analysed using 3-way analysis of variance and post hoc tests at α = 0.05. RESULTS: BAC + unloaded demonstrated the highest mean bond strength (3.12 ± 0.18 MPa; P < .001), while the BAC + loaded and CHX + loaded groups showed a significantly lower push-out bond strength than their unloaded counterparts. Mixed adhesive-cohesive failure was the most common failure mode observed. CONCLUSIONS: Without cycling loading, BAC was superior to CHX and EDTA in preserving the bond strength of resin-cemented fibre posts after 12 months of ageing. Loading significantly weakened the effectiveness of BAC and CHX in preserving the bond strength.

Interplay between Diffusion and Bond Cleavage Reaction for Determining Release in Polymer-Drug Conjugates.

In conjugated polymeric drug delivery systems, both the covalent bond degradation rate and the diffusion of the freely moving drug particles affect the release profile of the formulation. Using Monte Carlo simulations in spherical matrices, the release kinetics resulting from the competition between the reaction and diffusion processes is discussed. For different values of the relative bond cleavage rate, varied over four orders of magnitude, the evolution of (i) the number of bonded drug molecules, (ii) the fraction of the freely moved detached drug within the polymer matrix, and (iii) the resulting fractional release of the drug is presented. The characteristic release time scale is found to increase by several orders of magnitude as the cleavage reaction rate constant decreases. The two extreme rate-limiting cases where either the diffusion or the reaction dominates the release are clearly distinguishable. The crossover between the diffusion-controlled and reaction-controlled regimes is also examined and a simple analytical formula is presented that can describe the full dependence of the release time on the bond cleavage rate constant. This simple relation is provided simply by the sum of the characteristic time for purely diffusional release and the bond cleavage decay time, which equals the inverse of the reaction rate constant.

Bond Degradation Mechanism and Constitutive Relationship of Ribbed Steel Bars Embedded in Engineered Cementitious Composites under Cyclic Loading.

In order to investigate the bond degradation mechanism and constitutive relationship of ribbed steel bars in engineered cementitious composites (ECCs) under cyclic loading, 12 groups of specimens were tested in this paper. The design parameters included ECC compressive strength, ECC flexural toughness, cover thickness, and anchorage length. The results indicated that the degradation of the bond behavior of the ribbed steel bars in the ECCs under cyclic loading was mainly caused by the degradation of the properties of the ECC material itself, concentrating on the development of cracks in the ECC, the extrusion and shear failure of the ECC between the steel bar ribs, and the continuous grinding of the ECC particles on the shear failure surface. The degradation of the bond stress-slip curves under cyclic loading was mainly reflected by the degradation in the ultimate bond strength and unloading stiffness. According to the monotonic loading test results, a monotonic bond stress-slip relationship model was proposed. On this basis, through building the hysteretic rules of the bond stress-slip curves under cyclic loading, a calculation model was proposed to predict the bond stress-slip constitutive relationship between the ribbed steel bars embedded in the ECCs under cyclic loading. Finally, the validity of the proposed model was verified by a comparison between the model curves and the tested curves.

Effect of chemical cross-linkers on surface topography and microtensile bond strength of sound dentin: An in vitro study.

AIM AND OBJECTIVES: The aim of the study was to investigate the effect of two different collagen cross-linking agents proanthocyanidin (Grape seed extract [GSE] and 1-Ethyl-3-(3-dimethylaminopropyl) carbodiimide) on the surface topography of etched dentin and microtensile bond strength (µTBS) of resin dentin bond. MATERIALS AND METHODS: Fifty-two sound human 3rd molars were collected, and their occlusal surfaces were ground flat to expose dentin. Dentin surfaces were etched using phosphoric acid and then teeth were randomly divided into four groups, according to the dentin treatment: Group 1: wet bonding technique, Group 2: dry bonding technique, Group 3: 6.5% proanthocyanidin, and Group 4: 0.1M carbodiimide. Scanning electron microscope analysis was done for twenty specimens (n = 5 per group) at ×10,000 and ×30,000 magnification. Remaining 32 specimens were restored with TETRIC N-Bond adhesive systems and resin composite. After 24 h, teeth were sectioned to produce a cross-sectional surface area of 1.0 mm2 and tested for µTBS. STATISTICAL ANALYSIS: Data were statistically analyzed using ANOVA and post hoc least significant difference test (P < 0.05). CONCLUSION: When acid-etched dentin is treated by 6.5% proanthocyanidin (GSE) and 0.1M carbodiimide, followed by application of adhesives, it results in increased µTBS due to cross-linking of collagen fibrils.

Microtensile bond strength, 4-point bending and nanoleakage of resin-dentin interfaces: Effects of two matrix metalloproteinase inhibitors.

Chronic degradation of hybrid layer collagen by matrix metalloproteinases (MMPs) jeopardizes resin-dentin interfacial integrity and limits the durability of dental restorations. The 4-point bending strength (BS) is a valid but uncommon method of testing the mechanical behavior of resin-dentin interfaces. The present study aims to analyze the influence of two matrix metalloproteinase inhibitors on microtensile bond strength (µTBS), BS and nanoleakage. A total of 48M were divided into three groups according to bonding procedure. Teeth were horizontally sectioned to produce a flat dentin surface. In the control group, etch-and-rinse Prime&Bond One (Dentsply) bonding was used; in the self-etch group, methacryloyloxydodecylpyridinium bromide (MDPB)-containing Clearfil SE Protect (Kuraray) was used; and in the benzalkonium chloride (BAC)-etch group, BAC-etchant (Bisco) was used. A Ceram.X-One (Dentsply) composite was built as three successive layers and was light-cured. Samples were sectioned to produce microrods that were randomly divided into two groups for analysis at baseline and after 6 months of water immersion (n = 32), plus one slab for nanoleakage analysis (n = 8) via scanning electron microscopy (SEM) and digital image analysis (Fiji). Data were analyzed using the Weibull distribution and a mixed-model ANOVA with a post hoc Tukey test. All groups showed deterioration of the initial bonds. The self-etch group had a worse baseline µTBS than the control but had the best BS after aging. BAC-etch did not improve bond stability of etch-and-rinse adhesive. The µTBS and BS test results after aging were moderately correlated. Mixed fractures prevailed with regard to µTBS, whereas adhesive fractures dominated with regard to BS. Nanoleakage was not eliminated in any group and increased after aging. MDPB self-etch resisted bond degradation better than etch-and-rinse adhesives, even after BAC-etching. Integrating BS in studies of µTBS and nanoleakage might provide more clinically relevant outcomes for predicting the performance of dental adhesives.

Biocompatibility and bond degradation of poly-acrylic acid coated copper iodide-adhesives.

OBJECTIVE: To investigate the effect of poly-acrylic acid (PAA) copper iodide (CuI) adhesives on bond degradation, tensile strength, and biocompatibility. METHODS: PAA-CuI particles were incorporated into Optibond XTR, Optibond Solo and XP Bond in 0.1 and 0.5mg/ml. Clearfil SE Protect, an MDPB-containing adhesive, was used as control. The adhesives were applied to human dentin, polymerized and restored with composite in 2mm-increments. Resin-dentin beams (0.9±0.1mm2) were evaluated for micro-tensile bond strength after 24h, 6 months and 1year. Hourglass specimens (10×2×1mm) were evaluated for ultimate tensile strength (UTS). Cell metabolic function of human gingival fibroblast cells exposed to adhesive discs (8×1mm) was assessed with MTT assay. Copper release from adhesive discs (5×1mm) was evaluated with UV-vis spectrophotometer after immersion in 0.9% NaCl for 1, 3, 5, 7, 10, 14, 21 and 30 days. SEM, EDX and XRF were conducted for microstructure characterization. RESULTS: XTR and Solo did not show degradation when modified with PAA-CuI regardless of the concentration. The UTS for adhesives containing PAA-CuI remained unaltered relative to the controls. The percent viable cells were reduced for Solo 0.5mg/ml and XP 0.1 or 0.5mg/ml PAA-CuI. XP demonstrated the highest ion release. For all groups, the highest release was observed at days 1 and 14. SIGNIFICANCE: PAA-CuI particles prevented the bond degradation of XTR and Solo after 1year without an effect on the UTS for any adhesive. Cell viability was affected for some adhesives. A similar pattern of copper release was demonstrated for all adhesives.

Physico-mechanical analysis data in support of compatibility of chitosan/κ-carrageenan polyelectrolyte films achieved by ascorbic acid, and the thermal degradation theory of κ-carrageenan influencing the properties of its blends.

This article presents the complementary data regarding compatibilization of chitosan/κ-carrageenan polyelectrolyte complex for synthesizing of a soft film using ascorbic acid. It includes the thermal-theory for estimating the degradation of κ-carrageenan, as reflected in alteration of the structural properties of the blend. The data has been provided to demonstrate that the blend solution based on chitosan, a polycation, and κ-carrageenan, a polyanion polymer, produces an incompatible polyelectrolyte composite, susceptible to coaservative phase separation. We present further data on water resistance, water barrier property, mechanical parameters, scanning electron micrograph, as well as contact angle image dataset of the chitosan/κ-carrageenan film. The physical data were collected by water solubility and water permeability assays, with a view to elucidate the role of ascorbic acid in the compatibility of polyelectrolyte blends. The mechanical data is obtained from a stress-strain curve for evaluation of tensile strength and elongation at break point of the chitosan/κ-carrageenan film. The microstructure observations were performed using scanning electron micrograph. These dataset confirm fabrication of a soft film in the presence of ascorbic acid, with reduced heterogeneities in the polyelectrolyte film structure. The κ-carrageenan was also treated by a thermal process, prior to inclusion into the chitosan solution, to investigate the impact of this on the mechanical and structural features of the resulting blend. We present the required data and the theoretical analysis supporting the thermal chain degradation of a polymer and its effects on behavior of the film. Additional information, characterizing the hydrophobicity of the surface of the blend layers is obtained by measuring water contact angles using a contact anglemeter.