Effect of tin-chloride pretreatment on bond strength of two adhesive systems to dentin

OBJECTIVES: To determine the effect on resin composite-to-dentin bond strength of incorporation of an acidic tin-chloride pretreatment in two adhesive systems. MATERIALS AND METHODS: Human molars were ground to expose mid-coronal dentin. For microtensile bond strength (μTBS) testing, dentin was treated with Optibond FL or Clearfil SE according to one of six protocols (n = 22/group). Group 1: Phosphoric acid etching, Optibond FL Prime, Optibond FL Adhesive (manufacturer's instructions; control); Group 2: Tin-chloride pretreatment, Optibond FL Prime, Optibond FL Adhesive; Group 3: Phosphoric acid etching, tin-chloride pretreatment, Optibond FL Prime, Optibond FL Adhesive; Group 4: Clearfil SE Primer, Clearfil SE Bond (manufacturer's instructions; control); Group 5: Phosphoric acid etching, Clearfil SE Primer, Clearfil SE Bond; and Group 6: Tin-chloride pretreatment, Clearfil SE Primer, Clearfil SE Bond. The molars were then built up with resin composite (Clearfil Majesty Esthetic). After storage (1 week, 100  % humidity, 37 °C) the μTBS was measured and failure mode was determined. Additionally, pretreated dentin surfaces were evaluated using SEM and EDX. The μTBS results were analyzed statistically by a Welch Two Sample t-test and a Kruskal-Wallis test followed by exact Wilcoxon rank sum tests with Bonferroni-Holm adjustment for multiple testing (α = 0.05). RESULTS: When Optibond FL was used, partial or total replacement of phosphoric acid with tin-chloride decreased μTBS significantly. In contrast, when Clearfil SE was used, inclusion of a tin-chloride pretreatment in the adhesive procedure increased μTBS significantly. CONCLUSIONS: Tin-chloride pretreatment had a beneficial influence on the bond promoting capacity of the MDP-containing adhesive system Clearfil SE.

Bisphenol-A and residual monomer leaching from orthodontic adhesive resins and polycarbonate brackets: a systematic review

INTRODUCTION The objective of this systematic review was to assess the short- and long-term release of components of orthodontic adhesives and polycarbonate brackets in the oral environment. METHODS Electronic database searches of published and unpublished literature were performed. The following electronic databases with no language and publication date restrictions were searched: MEDLINE (via Ovid and PubMed), EMBASE (via Ovid), Cochrane Oral Health Group's Trials Register, and CENTRAL. Unpublished literature was searched on ClinicalTrials.gov, the National Research Register, and Pro-Quest Dissertation Abstracts and Thesis database. The reference lists of all eligible studies were checked for additional studies. Two review authors performed data extraction independently and in duplicate using data collection forms. Disagreements were resolved by discussion or the involvement of an arbiter. RESULTS No randomized controlled trial was identified. In the absence of randomized controlled trials, observational studies were included. Eleven studies met the inclusion criteria. All were observational studies conducted in vivo or in vitro. The bisphenol-A release from orthodontic bonding resins was found to be between 0.85 and 20.88 ng per milliliter in vivo, and from traces to 65.67 ppm in vitro. Polycarbonate brackets released amounts of 22.24 μg per gram in ethanol solution and 697 μg per gram after 40 months in water. Bis-GMA and TEGDMA leaching in vitro reached levels of 64 and 174 mg per 10 μL, respectively. Because of the heterogeneity in methodologies and reporting, only qualitative synthesis was performed. CONCLUSIONS The available evidence on this topic derived from observational in-vivo and in-vitro studies that represent a moderate level of evidence. The variety of setups and the different units allied to the diversity of reporting among studies did not allow calculation of pooled estimates.

Does tin pre-treatment enhance the bond strength of adhesive systems to enamel?

OBJECTIVES The study investigated the modification of composite-to-enamel bond strength by pre-treatment of enamel with a concentrated, acidic SnCl2-solution. METHODS Six groups of flat human enamel specimens (n=44 per group) were treated as follows: OB-H: H3PO4 etching, Optibond FL application (primer+adhesive; manufacturer's instructions); OB-S: SnCl2 pre-treatment, Optibond FL application (primer+adhesive); OB-HS: H3PO4 etching+SnCl2 pre-treatment, Optibond FL application (primer+adhesive); CF-N: Clearfil SE application (primer+bond; manufacturer's instructions); CF-H: H3PO4 etching, Clearfil SE application (primer+bond); CF-S: SnCl2 pre-treatment, Clearfil SE application (primer+bond). Enamel specimens were then built up with resin composite (Clearfil Majesty Esthetic) and stored (100% humidity, 37 °C, 1 week). μTBS-measurement and failure mode analysis of one-half of the specimens were performed immediately after storage, while the other half was analysed after a thermocycling procedure (8500 cycles; 5 °C and 55 °C; dwell time 30s). Additional specimens were prepared for SEM- and EDX-analysis. RESULTS Highest values were measured for OB-H before and after thermocycling, lowest values for CF-N. Compared to OB-H treatment, OB-S treatment reduced μTBS before/after thermocycling by 23%/28% and OB-HS treatment by 8%/24% (except for OB-SH before (n.s.), all p≤0.001 compared to OB-H). In the Clearfil SE treated groups pre-treatment increased μTBS significantly compared to CF-N (before/after: CF-H: +46%/+70%; CF-S: +51%/42%; all p≤0.001). CONCLUSION Pre-treatment with H3PO4 or SnCl2 markedly increased the μTBS of Clearfil SE to enamel. However, thermocycling partly reduced the gain in μTBS obtained by SnCl2 pre-treatment. CLINICAL SIGNIFICANCE The application of an acidic and highly concentrated SnCl2 solution is a good option to increase the μTBS between enamel and a resin composite mediated by an adhesive system containing the multifunctional monomer MDP.

Bonding of simplified adhesive systems to caries-affected dentin of primary teeth.

PURPOSE To evaluate the bonding of simplified adhesive systems to sound and caries-affected dentin of primary teeth with microtensile (µTBS) and nanoleakage (NL) tests. MATERIALS AND METHODS Occlusal cavities were prepared in 36 sound second primary molars. Half of the specimens were submitted to pH cycling to simulate caries-affected dentin. Teeth were randomly restored with one of three materials: the etch-and-rinse adhesive system Adper Single Bond 2 (SB), the two-step self-etching adhesive system Adper SE Plus (SE), and the one-step self-etching adhesive system Adper Easy One (EASY). After storage for 24 h, specimens with cross-sectional areas of 0.8 mm2 were prepared for microtensile testing (1 mm/min). One stick from each tooth was immersed in silver nitrate solution (24 h) and allowed to develop for 8 h in order to score the nano leakage with SEM. The fracture pattern was evaluated using a stereomicroscope (400X). The µTBS means were analyzed by two-way ANOVA and Tukey's post-hoc test. For NL, the Kruskal- Wallis and Mann-Whitney tests were used (α < 0.05). RESULTS SB (35.5 ± 3.5) showed the highest µTBS value to sound dentin, followed by EASY (26.3 ± 1.9) and SE (18.2 ± 6.5) (p < 0.05). No difference among materials was observed for caries-affected dentin (SB: 17.8 ± 4.2; SE: 13.9 ± 3.2; EASY: 14.4 ± 4.2, p > 0.05). For all groups, adhesive/mixed fracture prevailed. Caries affected dentin promoted silver nitrate uptake into the adhesive interface; however, with SE, the nano leakage was more pronounced than in the other adhesive systems, even in sound dentin. CONCLUSION Caries-affected dentin negatively influences the bond strength and nano leakage of the two-step etch-and-rinse and one-step self-etching adhesive systems tested in primary teeth.

5-year results comparing mineral trioxide aggregate and adhesive resin composite for root-end sealing in apical surgery

INTRODUCTION Recent meta-analyses of the outcome of apical surgery using modern techniques including microsurgical principles and high-power magnification have yielded higher rates of healing. However, the information is mainly based on 1- to 2-year follow-up data. The present prospective study was designed to re-examine a large sample of teeth treated with apical surgery after 5 years. METHODS Patients were recalled 5 years after apical surgery, and treated teeth were classified as healed or not healed based on clinical and radiographic examination. (The latter was performed independently by 3 observers). Two different methods of root-end preparation and filling (primary study parameters) were to be compared (mineral trioxide aggregate [MTA] vs adhesive resin composite [COMP]) without randomization. RESULTS A total of 271 patients and teeth from a 1-year follow-up sample of 339 could be re-examined after 5 years (dropout rate = 20.1%). The overall rate of healed cases was 84.5% with a significant difference (P = .0003) when comparing MTA (92.5%) and COMP (76.6%). The evaluation of secondary study parameters yielded no significant difference for healing outcome when comparing subcategories (ie, sex, age, type of tooth treated, post/screw, type of surgery). CONCLUSIONS The results from this prospective nonrandomized clinical study with a 5-year follow-up of 271 teeth indicate that MTA exhibited a higher healing rate than COMP in the longitudinal prognosis of root-end sealing.

Bond Strength of Resin Composite to Dentin with Different Adhesive Systems: Influence of Relative Humidity and Application Time.

PURPOSE To investigate the influence of relative humidity and application time on bond strength to dentin of different classes of adhesive systems. MATERIALS AND METHODS A total of 360 extracted human molars were ground to mid-coronal dentin. The dentin specimens were treated with one of six adhesive systems (Syntac Classic, OptiBond FL, Clearfil SE Bond, AdheSE, Xeno Select, or Scotchbond Universal), and resin composite (Filtek Z250) was applied to the treated dentin surface under four experimental conditions (45% relative humidity/application time according to manufacturers' instructions; 45% relative humidity/reduced application time; 85% relative humidity/application time according to manufacturers' instructions; 85% relative humidity/reduced application time). After storage (37°C, 100% humidity, 24 h), shear bond strength (SBS) was measured and data analyzed with nonparametric ANOVA followed by Kruskal-Wallis tests and Mann-Whitney U-tests with Bonferroni-Holm correction for multiple testing (level of significance: α = 0.05). RESULTS Increased relative humidity and reduced application time had no effect on SBS for Clearfil SE Bond and Scotchbond Universal (p = 1.00). For Syntac Classic, OptiBond FL, AdheSE, and Xeno Select there was no effect on SBS of reduced application time of the adhesive system (p ≥ 0.403). However, increased relative humidity significantly reduced SBS for Syntac Classic, OptiBond FL, and Xeno Select irrespective of application time (p ≤ 0.003), whereas for AdheSE, increased relative humidity significantly reduced SBS at recommended application time only (p = 0.002). CONCLUSION Generally, increased relative humidity had a detrimental effect on SBS to dentin, but reduced application time had no effect.

Quantitative microstructure analysis of polymer-modified mortars

Digital light, fluorescence and electron microscopy in combination with wavelength-dispersive spectroscopy were used to visualize individual polymers, air voids, cement phases and filler minerals in a polymer-modified cementitious tile adhesive. In order to investigate the evolution and processes involved in formation of the mortar microstructure, quantifications of the phase distribution in the mortar were performed including phase-specific imaging and digital image analysis. The required sample preparation techniques and imaging related topics are discussed. As a form of case study, the different techniques were applied to obtain a quantitative characterization of a specific mortar mixture. The results indicate that the mortar fractionates during different stages ranging from the early fresh mortar until the final hardened mortar stage. This induces process-dependent enrichments of the phases at specific locations in the mortar. The approach presented provides important information for a comprehensive understanding of the functionality of polymer-modified mortars.

Development of corrosion of steel bars embedded in mortar made with slag from secondary metallurgy

The aim of this work is to study the evolution of the corrosion rate of reinforcements embedded in mortar specimens that have been partly or fully replaced by the sand ladle furnace white slag. Prisms are manufactured mortar 6cm x 8cm x 2cm in which are embedded reinforcing steel bars of 6mm diameter B500SD. At the time of mixing were added varying amounts of chloride ion content by weight of cement (0%, 0.4%, 0.8%, 1.2%, 2%). The specimens were made totally or partially replacing the white slag, getting four different mixes depending on the degree of substitution. After curing the specimens for 28 days in moist chambers proceeded to dry up naturally. Here are gradually dampened by its conservation in a moist chamber, periodically measuring the corrosion rate of the bars using the technique of polarization curve. The results, in terms of corrosion current and corrosion potential, were compared with those obtained on standard samples, without replacement by slag aggregate. The analysis of results allows us to know, depending on the type of mortar used, the chloride threshold with the depassivation produced steel and the corrosion rates achieved in steels in the active state in terms of mortar moisture, obtained from qualitatively using gravimetric techniques. The results achieved to date support the conclusion that no significant differences in the behavior against corrosion induced by chloride ions, between the steel bars embedded in standard samples and the steel bars embedded in samples including with aggregates from slag. Both the chloride threshold resulting in the depassivation steel as the corrosion rate reached through the bars in an active state are very similar in both types of mortars when they have the same moisture content.

Optimum adhesive thickness in structural adhesives joints using statistical techniques base on Weibull distribution

The geometrical factors defining an adhesive joint are of great importance as its design greatly conditions the performance of the bonding. One of the most relevant geometrical factors is the thickness of the adhesive as it decisively influences the mechanical properties of the bonding and has a clear economic impact on the manufacturing processes or long runs. The traditional mechanical joints (riveting, welding, etc.) are characterised by a predictable performance, and are very reliable in service conditions. Thus, structural adhesive joints will only be selected in industrial applications demanding mechanical requirements and adverse environmental conditions if the suitable reliability (the same or higher than the mechanical joints) is guaranteed. For this purpose, the objective of this paper is to analyse the influence of the adhesive thickness on the mechanical behaviour of the joint and, by means of a statistical analysis based on Weibull distribution, propose the optimum thickness for the adhesive combining the best mechanical performance and high reliability. This procedure, which is applicable without a great deal of difficulty to other joints and adhesives, provides a general use for a more reliable use of adhesive bondings and, therefore, for a better and wider use in the industrial manufacturing processes.

Mode II fracture energy in the adhesive bonding of dissimilar substrates: carbon fibre composite to aluminium joints

The end-notched flexure (ENF) test calculates the value of mode II fracture energy in adhesive bonding between the substrates of same nature. Traditional methods of calculating fracture energy in the ENF test are not suitable in cases where the thickness of the adhesive is non-negligible compared with adherent thicknesses. To address this issue, a specific methodology for calculating mode II fracture energy has been proposed in this paper. To illustrate the applicability of the proposed method, the fracture energy was calculated by the ENF test for adhesive bonds between aluminium and a composite material, which considered two different types of adhesive (epoxy and polyurethane) and various surface treatments. The proposed calculation model provides higher values of fracture energy than those obtained from the simplified models that consider the adhesive thickness to be zero, supporting the conclusion that the calculation of mode II fracture energy for adhesives with non-negligible thickness relative to their adherents should be based on mathematical models, such as the method proposed in this paper, that incorporate the influence of this thickness.

Effect of adhesive thickness and concrete strength on FRP-Concrete Bonds

The use of fiber-reinforced polymer (FRP) composites for strengthening, repairing, or rehabilitating concrete structures has become more and more popular in the last 10 years. Irrespective of the type of strengthening used, design is conditioned, among others, by concrete-composite bond failure, normally attributed to stress at the interface between these two materials. Single shear, double shear, and notched beam tests are the bond tests most commonly used by the scientific community to estimate bond strength, effective length, and the bond stress-slip relationship. The present paper discusses the effect of concrete strength and adhesive thickness on the results of beam tests, which reproduce debonding conditions around bending cracks much more accurately. The bond stress-slip relationship was analyzed in a cross section near the inner edge, where stress was observed to concentrate. The ultimate load and the bond stress-slip relationship were visibly affected by concrete strength. Adhesive thickness, in turn, was found to have no significant impact on low-strength concrete but a somewhat greater effect on higher strength materials.

Some theoretical aspects in computational analysis of adhesive lap joints

This paper is devoted to the numerical analysis of bidimensional bonded lap joints. For this purpose, the stress singularities occurring at the intersections of the adherend-adhesive interfaces with the free edges are first investigated and a method for computing both the order and the intensity factor of these singularities is described briefly. After that, a simplified model, in which the adhesive domain is reduced to a line, is derived by using an asymptotic expansion method. Then, assuming that the assembly debonding is produced by a macro-crack propagation in the adhesive, the associated energy release rate is computed. Finally, a homogenization technique is used in order to take into account a preliminary adhesive damage consisting of periodic micro-cracks. Some numerical results are presented.

Influence of different organoclays on the curing, morphology, and dynamic mechanical properties of an epoxy adhesive

The thermal, mechanical, and adhesive properties of nanoclay-modified adhesives were investigated. Two organically modified montmorillonites: Cloisite 93A (C93A) and Nanomer I.30E (I.30E) were used as reinforcement of an epoxy adhesive. C93A and I.30E are modified with tertiary and primary alkyl ammonium cations, respectively. The aim was to study the influence of the organoclays on the curing, and on the mechanical and adhesive properties of the nanocomposites. A specific goal was to compare their behavior with that of Cloisite30B/epoxy and Cloisite15A/ epoxy nanocomposites that we have previously studied. Both C30B and C15A are modified with quaternary alkyl ammonium cations. Differential scanning calorimetry results showed that the clays accelerate the curing reaction, an effect that is related to the chemical structure of the ammonium cations. The three Cloisite/nanocomposites showed intercalated clay structures,the interlayer distance was independent of the clay content. The I.30E/epoxy nanocomposites presented exfoliated structure due to the catalytic effect of the organic modifier. Clay-epoxy nanocompo-sites showed lower glass transition temperature (Tg) and higher values of storage modulus than neat epoxy thermoset, with no significant differences between exfoliated or intercalated nanocom-posites. The shear strength of aluminum joints using clay/epoxy adhesives was lower than with the neat epoxy adhesive. The wáter aging was less damaging for joints with I.30E/epoxy adhesive.

Influence of acrylic adhesive viscosity and surface roughness on the properties of adhesive joint

In adhesion, the wetting process depends on three fundamental factors: the surface topography of the adherend, the viscosity of the adhesive, and the surface energy of both. The aim of this paper is to study the influence of viscosity and surface roughness on the wetting and their effect on the bond strength. For this purpose, an acrylic adhesive with different viscosities was synthesized and some properties, such as viscosity and surface tension, were studied before adhesive curing took place. Furthermore, the contact angle and the lap-shear strength were analyzed using aluminum adherends with two different roughnesses. Scanning electron microscopy was used to determine the effect of the viscosity and the roughness on the joint interface. The results showed that the adhesive exhibits an optimal value of viscosity. Below this value, at low viscosities, the low neoprene content produces poor bond strength due to the reduced toughness of the adhesive. Additionally, it also produces a high shrinkage during curing, which leads to the apparition of residual stresses that weakens the interfacial strength. However, once the optimum value, an increase in the viscosity produces a negative effect on the joint strength as a result of an important decrease in the wettability.