Analysis of structural,morphological alterations,wettability characteristics and adhesion to enamel after various surface conditioning methods

Minimal invasive dental reconstructions and orthodontic appliances are bonded to enamel without removing the enamel with rotating instruments but the top layer of enamel may be partially aprismatic and impair adhesion. The objectives of this study were to investigate the effect of mechanical surface conditioning methods for removing enamel on its structural, morphological alterations, wettability characteristics, and adhesion of resin-based cement to the conditioned surfaces. Maxillary human incisors (N = 40, n_quadrant = 160) were obtained and coronal sections were embedded in acrylic with their labial surfaces exposed. The teeth were randomly divided into four groups and the enamel surface of each tooth was divided into four quadrants. The surfaces were conditioned in a clockwise manner by one of the following methods: (1) Non-conditioned enamel acted as the control group (C); (2) Silicone-coated disk (Sof-Lex disc, Black, 3 M ESPE) (SD); (3) Diamond bur at slow speed (DB) and (4) Airborne particle abrasion (50 μm Al₂O₃, 2 bar, 5 s) (AA). Surface roughness was measured at each quadrant using a non-contact digital profilometer and contact angle measurements were performed using a goniometer. Enamel surfaces were then etched with 37% H₃PO₄ for 60 s and roughness and wettability measurements were repeated. The enamel surfaces in each quadrant received resin composite luting cement (Variolink II, Ivoclar Vivadent) incrementally in a polyethylene mold (diameter: 1 mm²; height: 4 mm) and photopolymerized. The specimens were stored in distilled water for 24 h at 37 °C until the testing procedures and then shear force was applied to the adhesive interface until failure occurred in a Universal Testing Machine (0.5 mm/min). Microshear bond (μSBS) was calculated by dividing the maximum load (N) by the bonding surface area of the resin cement. Representative enamel surfaces were analyzed under the scanning electron microscope (SEM) (x5000) to assess the surface morphology. Failure types were analyzed using optical microscope and SEM. Data (MPa) were analyzed using one-way ANOVA and Tukey`s test for each parameter and Linear model for group comparisons (α = 0.05). Surface conditioning method significantly affected the adhesion results (p < 0.001), surface roughness (p = 0.017), and contact angle (p < 0.001). Interaction terms were significant (p > 0.05). AA (338 ± 182) created significantly higher surface roughness compared to SD (308 ± 180) and DB (242 ± 197) (p < 0.05). After etching with 37% H₃PO₄, DB (307 ± 223) resulted in significantly lower roughness than those of SD (385 ± 173) and AA (414 ± 193) (p < 0.05). AA (40 ± 11) delivered significantly lower contact angle compared to those of SD (61 ± 9) and DB (59 ± 10). After etching with 37% H₃PO₄, AA (42 ± 10) and DB (50 ± 10) presented the lowest contact angle (p < 0.05). Mean μSBS results (MPa) showed significant difference between the experimental groups (p = 0.011) and were in descending order as follows: DB (20 ± 8)^a?a b < C (12 ± 5)^b. Failure types were predominantly mixed failure type between the enamel and the resin cement with more than half of the resin remained on the enamel surface (32 to 33 out of 40) in all groups. Cohesive failure in the enamel was not observed in any of the groups. SEM analysis showed that AA group leaves abundant particles on the enamel surface and after DB and AA, etching could not remove the particles completely and expose the enamel prisms.     

Joining zirconia with nickel-based superalloys for extreme applications by using a pressure-free high-temperature resistant adhesive

In order to meet the high demand for joining ceramic/superalloy composite structure in extreme environments, a novel high-temperature resistant adhesion technique was developed for joining ZrO₂ and Inconel 625 by applying an aluminum phosphate emulsion/zirconium sol based adhesive. With increasing temperature, a series of reactions occurred in adhesive, and its high-temperature bonding was attributed to the formation of a composite structure containing various ceramics and intermetallics. The adhesive after RT curing could find direct applications in extreme environments, and provide bonding strength no less than 2.5 MPa in the temperature range of RT-1100 °C. The bonding strength was higher than 4 MPa in the temperature range of 800–1000 °C, which was further attributed to the formation of an effective CTE-gradient relationship among ZrO₂, adhesive and Inconel 625, as well as the interfacial reactions between the two substrates. The work broadened the application of adhesion technique and brought new ideas for joining dissimilar engineering materials.     

Molecular dynamics study of interfacial load transfer capability in amorphous SiOx films deposited on alumina surfaces

Effective adhesion between AlO_x and SiO_x is important for protective coatings and high-k films under extreme operating conditions. Here, we study the chemo-mechanical behavior of the AlO_x/SiO_x interface and its delamination mechanism using all-atom reactive molecular dynamics simulations. The structure of the interface is examined by the formation of bridge oxygen and the distribution of nanopores. The cleavage of ionic bonds during delamination and the resulting adhesion strength of the system are quantified using pull-out simulations. The results reveal the dependence of the nanopores and ionic bond formation on the oxide structure. The ionic bond density at the interface increases as the oxidation of the aluminum surface proceeds, which directly increases the adhesion strength with SiO_x. In particular, the global coordination distribution in the homogeneously grown oxide inhibits the formation of nanopores inside the aluminum substrate and contributes to extremely high adhesion strength. This reveals a fundamental relationship between physicochemical parameters and engineering mechanics for hetero-oxide structure design.     

The effect of post surface silanization and luting agents on the push-out bond strengths of adhesively inserted fiber reinforced posts

The effect of silane treatment on the push-out bond strengths of three different luting agents to fiber-reinforced composite (FRC) posts after thermocycling was evaluated.Sixty single-rooted human maxillary central incisors were sectioned below the cemento-enamel junction, and the roots were endodontically treated. RelyX Fiber Posts (size #2) were inserted using etch-and-rinse, self-etch, and self-adhesive luting agents (cementing agents). For half of the specimen in each group, the fiber posts were treated with a silane coupling agent. Bonded specimens were cut (2-mm-thick sections) and push-out tests were performed (crosshead speed, 0.5 mm/min). Failure modes were evaluated using a stereomicroscope at original magnification ×40.For each luting agent the use of silane did not result in any statistically significant difference at any level of the root compared to those of the control groups except for Variolink II and RelyX Unicem luting agents in apical root section (p<0.05; one-way ANOVA). The post hoc analysis showed that regardless of the pre-treatment procedures, Variolink II achieved significantly higher bond strengths than Panavia F 2.0 and RelyX Unicem in all root sections (p<0.05).The use of a silane coupling agent had no influence on bond strengths depending on the luting agent used, whereas the type of luting agent (etch-and-rinse, self-etch, and self-adhesive) appeared to be a significant influence on the push-out bond strength values independent of the pre-treatment used. Therefore, pre-treatment of fiber posts with a silane coupling agent does not seem to be mandatory, which saves time in the clinical situation.     

Comparative determination of TiO2 surface free energies for adhesive bonding application

The development of durable bonds using titanium adherens has been investigated from the point of view of surface energy theoretical models measurements. The traditional Chromium Acid Anodization, which provides excellent durability, has to be phased out due to the use of hazardous Cr (VI) in the bath and as a result, special attention is paid to the sodium hydroxide anodizing and other alkaline chemical etchers. There are hardly any references on the surface free energy of adhesive titanium oxide coatings and therefore the objective of this work was to evaluate the surface and interface energy parameters of the various types of alkaline chromate free surface treatments using Neumann, Fowkes and van Oss–Chaudhury–Good methods in order to determine which method provides greatest differentiation between the coatings. Results show that Fowkes method produced the greatest variance in surface energies of the compared surface treatments and hence can be considered as better suited for more accurate discrimination between the oxide surface treatments on Ti–6Al–4V alloy. Although, in the case of model liquids, i.e. water and diiodomethane, the trends obtained for contact angles, surface energies, works of adhesion and solid/liquid interface energies all correlated between each other, a disagreement between the trends of solid/liquid interface energies calculated using Fowkes and van Oss–Chaudhury–Good methods for surface treatment/adhesive resin was obtained. In case of real adhesive systems, the use of work of adhesion appears more adequate in order to discriminate the surface treatments. Based on these findings the anodization in the tested alkaline bath after a previous alkali etching in the same bath is recommended, although adhesion test has to be still performed.     

Adhesion between submicrometer polystyrene spheres

The sphere-substrate contact method was usually used to study adhesion theory because it is rather difficult to make two micrometer or submicrometer spheres contact precisely. Here, we used sphere-sphere contact method by a novel, simple process to investigate deformations of spheres. The polystyrene particles size ranges from 60 nm to 600 nm. We found that the polystyrene particles underwent plastic deformations due to van der Waals interaction. The contact radii were observed by the scanning electron microscope (SEM).     

Thermotropic liquid crystalline polymers as protective coatings for aerospace

Liquid crystalline polymers (LCPs) have potential as multifunctional, environmentally friendly coatings for aerospace, overcoming the disadvantages of current materials. Their use, however, has been hindered mainly by their poor adhesion strength. The present work studies novel liquid crystalline thermosetting polymers (LCTs), which can overcome the disadvantages of commercial LCPs for protective coatings in aerospace applications. Phenylethynyl terminated liquid crystalline oligomers based on 4-hydroxybenzoic acid (HBA) and 6-hydroxy-2-naphthoic acid (HNA) were synthesized and melt-pressed on grit-blasted aluminum to obtain 25 μm and 80 μm thick coatings. The presence of coating defects and curing kinetics were investigated, and the adhesion, mechanical properties and environmental resistance were compared with a commercial LCP reference material (Vectra^®). The LCTs showed highly improved adhesion; moreover, fully cured LCTs are harder and stiffer than commercial LCPs, which are expected to increase their wear and impact resistance. The coatings showed no swelling, peeling, or blistering after 500 h of full immersion in fluids such as jet fuel and turbine oil; furthermore, LCTs resisted 1000 h in corrosive fog (salt-spray) and hot moisture. Exposed samples retained their hardness, modulus, and pull-off strength, evidencing the outstanding chemical resistance of these LCTs. Our findings showed the potential of LCTs as protective and wear resistant coatings, particularly in the aggressive environments of aerospace applications. However, results suggest that exposed coating/substrate interfaces constitute paths for environmental attack. Further research aims at elucidating the possible mechanisms.     

INTERFACE/INTERPHASE ENGINEERING OF POLYMERS FOR ADHESION ENHANCEMENT: PART II. THEORETICAL AND TECHNOLOGICAL ASPECTS OF SURFACE-ENGINEERED INTERPHASE-INTERFACE SYSTEMS FOR ADHESION ENHANCEMENT

Part I of this paper reviewed the theoretical principles of the macromolecular design of polymer interface/interphase systems for obtaining maximum adhesion and fracture performance of adhesively bonded assemblies. In Part II a novel, relatively simple and industry-feasible technology for surface-grafting connector molecules is demonstrated and discussed in detail and supported by a range of experimental examples. It is shown, in agreement with contemporary theory, that the use of chemically attached graft chemicals of controlled spatial geometry and chemical functionality enables a significant increase in the strength and fracture energy of the interphase, to the point of cohesive fracture of the substrate, or that of an adjacent medium such as adhesive, elastomer, or other material. This occurs even after prolonged exposure of investigated systems to adverse environments such as hot water.     

EFFECT OF SURFACE ROUGHNESS ON THE ADHESION OF ELECTROLESSLY PLATED PLATINUM TO POLY(ETHYLENE TEREPHTHALATE) FILMS

Poly(ethylene terephthalate) films were treated with aqueous sodium hydroxide solutions of different concentrations for various times. The rate of weight loss increased with the addition of a swelling agent (methylene chloride) or a cationic surfactant. The surface roughness of the treated films was determined from atomic force microscopy (AFM) and pore diameter was obtained from scanning electron microscopy (SEM). In general, surface roughness was found to increase with increasing weight loss for the treated films. A maximum roughness was obtained for samples with a weight loss of approximately 15-20%, beyond which the roughness of the samples decreased. The addition of methylene chloride and surfactant resulted in an almost two-fold increase in the roughness for all treatment times investigated. The adhesion of electrolessly plated platinum film was dependent on the contact area produced by chemical treatment. Treatments producing smaller diameter pores of greater depth gave better adhesion.     

CONTACT BETWEEN A SMOOTH MICROSPHERE AND AN ANISOTROPIC ROUGH SURFACE

This article discusses the effects of asperities on elastic and adhesive contact between a smooth sphere and a rough surface. Two numerical methods are introduced: an asperity-superposition method and a direct-simulation method. In the first method, geometric parameters such as asperity heights, orientations, and radii of curvature are identified by a least-squares regression of neighboring surface heights measured using an atomic force microscope. The rough surface is reconstructed by the superposition of these asperities. The modeling of adhesive and elastic contacts begins with the modeling of a single parabolic-shaped asperity contact. A generalized JKR model for an arbitrary parabola is developed to suit this purpose. The contact between the rough surface (represented by the supposition of parabolic-shaped asperities) and the sphere consequently is modeled bythe mapping and integration of individual asperity contacts. In the second method, pure-elastic contact is modeled by half-space elastic theory. A contact-search algorithm is used to find solutions on the displacement and the contact-pressure distribution that satisfy both the load-displacement equation and the contactboundary conditions. Results from both methods are compared to reveal the effects of asperities on adhesion and elastic-contact pressure.