Two-step vs. one-step conditioning systems and adhesive interface of glass ceramic surface and resin systems

The effect of two-step and one-step ceramic surface conditioning/priming, and subjecting to exposure with boiling water on adhesion strength of resin cements was evaluated. Rectangular shaped specimens were cut from CAD blocks of E-max (Ivoclar Vivadent) and Mark II (VITA Zahnfabrik) and randomly assigned to two main study groups. Group one specimens’ surfaces were conditioned using the two-step conditioning/priming procedure and group two specimens were treated using the one-step conditioning/priming system. After treating, 3 mm thick resin cement layer was applied onto the surface using a split stainless steel mold. Each group was further divided into four subgroups (n = 10) depending on type of resin cement applied and subjecting to exposure in boiling water. Adhesion strength of all the specimens was measured using the universal material testing machine, results were tabulated and subjected to statistical analysis at a significance level of p < 0.05. Adhesive resin showed higher values of 22.05 and 18.65 MPa with E-max and Mark II respectively, and resin composites showed 18.13 and 15.13 MPa with E-max and Mark II respectively, when two-step conditioning system was employed. Majority of the adhesive resin specimens showed cohesive failure in cement. Subjecting the specimens to exposure in boiling water for 24 h not only showed adhesive failure but also significantly reduced adhesion strength of adhesive resin and resin composite. The significance of the study is that, the traditional two-step ceramic surface conditioning is more effective than the one-step conditioning and unfilled adhesive resin provides better adhesion strength.     

The influence of hydroxyl group concentration on epoxy–aluminium bond durability

The influence of hydroxyl group (OH) concentration on the durability of adhesive bonds formed between an epoxy resin and aluminium adherend has been examined. Initially, surface analysis in combination with chemical derivatisation was employed to characterise the OH and epoxy functional groups present in FM-73, a structural epoxy adhesive. Bulk FM-73 indicated a higher degree of cure than the surface of FM-73 present at the interface of an epoxy–aluminium adhesive joint. Plasma and water treatment of the aluminium adherend was employed to alter the metal oxide's surface OH concentration. Despite a several-fold difference of aluminium surface OH concentrations for the different metal pre-treatments, there was no significant variation in the adhesive joint fracture toughness in a humid environment, G _Iscc. In contrast, grit-blasting the aluminium prior to bonding increased G _Iscc almost 15-fold. Simple calculations indicate that the aluminium surfaces used in the bonding experiments would have a large excess of OH groups available to react with a standard epoxy resin and that the influence of surface roughness on adhesion durability is not insignificant.     

The Effect of Aging in Water on the Strength of Fiber-Polymer Systems

The effect of the exposure time in water on the adhesive strength of fiber/resin systems was studied. To this end, the adhesive strength of single-fiber/matrix systems was measured. Such a system simulates the unit cell of a fiber-reinforced composite. The resin was an epoxy (DGEBA-based) polymer. The substrate used consisted of boron fibers, a steel wire and glass fibers. The samples were kept in water for a period of 1-280 days at room temperature and the adhesive strength was measured also at room temperature. The water absorption of the resin and the impregnated strand produced on the basis of the glass fibers and the resin studied and also the physico-mechanical characteristics of the impregnated strand were studied at the same time. The samples used to determine the adhesive strength were kept in such a contact with water that the latter could penetrate into some of them only at the interface and into the others at the interface and through the resin layer.

It was found that the adhesive strength decreases with increasing amount of water absorbed. On the basis of the results obtained it was concluded that the principal factor that determines the loss in adhesive strength during the aging of the systems in water is the plasticization of the epoxy resin by water.     

Determination of Water Diffusion Coefficients and Dynamics in Adhesive/Carbon Fiber-Reinforced Phenolic Resin Composite Joints

Energy-dispersive X-ray spectroscopy analysis (EDX) is an easy and exact method for determination of water diffusion coefficients and dynamics. Here we have calculated the water diffusion coefficients and dynamics in adhesive/carbon fiber-reinforced phenolic resin composite joints subjected to different surface treatments with both EDX and elemental analysis. The water diffusion coefficients and dynamics in the adhesive joints determined with EDX analysis are almost the same as those determined with elemental analysis. The durability of the adhesive joints with carbon fiber-reinforced phenolic resin composites subjected to silane coupling agent treatment is better than those subjected to sandpaper burnishing and chemical oxidation treatment.     

Microscopic evaluation of the thickness and structure of the cement and cement–dentin interdiffusion zone after luting posts with three different luting cements

Clinical studies report that failures of fiber post cementation occur mainly at the cement–dentin interface. The aim of this in vitro study is to compare the scanning electron microscopic (SEM) evaluations of the cement thicknesses in the root canals and the thickness of cement–dentin interface zones obtained after luting standardized glass-fiber posts with three different types of luting cements. Thirty single-rooted mandibular premolars of similar sizes were prepared for post insertion after biomechanical preparation and obturation. They were divided into three groups containing 10 samples each. Standardized glass-fiber posts were cemented with zinc phosphate cement for ZNP group, with conventional adhesive resin cement for CAR group, and with self-adhesive resin cement for SAR group. The formation and thickness of cement and cement–dentin interface zone were evaluated by stereomicroscope and SEM using ×800 magnification, and the data were analyzed. There was no significant difference between groups in terms of cement thickness (p = 0.835); however, there were significant differences among the cement layer thicknesses measured at the three examined levels of the root canals (p = 0.000). The groups using conventional adhesive resin cement presented longer micromechanical interlocking while the groups using self-adhesive resin cement showed wide gaps and zinc phosphate cement showed no bonding between cement–dentin interdiffusion zones along the root canal. As a clinical consequence, the use of zinc phosphate cement may not provide strong bond between dentin–cement interface. Conventional adhesive resin cements showed reliable bond to dentin when compared to zinc phosphate and self-adhesive resin cement.     

The Effect of Lithium Disilicate Ceramic Surface Neutralization on Wettability of Silane Coupling Agents and Adhesive Resin Cements

This in vitro study was aimed to evaluate the possible changes in wettability of an etched glass ceramic surface to silane primers, adhesive resin and resin cement when the surface had been neutralized by a special neutralizing agent after etching. Rectangular shaped specimens were cut from the CAD blocks of an e-max lithium disilicate glass ceramic, cut specimens were sequentially polished and ultrasonically cleaned. All the specimens were etched for 20 s with 5% hydrofluoric acid and ultrasonically cleaned. Specimens were randomly assigned to one control group (without neutralization) and one treatment group (with neutralization) having 20 specimens each. The specimens of each group were further divided into two subgroups having 10 specimens each and tested to determine the effect of neutralizing agent on wettability of experimental and commercial silanes. Each subgroup specimen was tested for wettability to adhesive resin and commercial resin cement. Data were analyzed using two-way ANOVA. Neutralizing the ceramic surface did not show a significant effect on wettability to the silanes and the resin based materials, but the experimental silane showed better wettability than the commercial silane. The adhesive resin had statistically significant lower contact angle (high wettability) values than the commercial resin cement. The results of the current study suggested that the neutralizing agent did not have an impact on the wettability of the etched ceramic. However, there were differences in wetting properties of the silane primers, and adhesive resin versus resin composite luting cements.     

High performance wood composites from highly filled polybenzoxazine

Highly filled systems prepared by compression molding of Hevea brasiliensis woodflour filled polybenzoxazine composites with high mechanical properties and reduced water uptake has been developed. The effects of percent filler content and particle size of woodflour on the obtained composite's properties were examined. The low melt viscosity of BA‐a type polybenzoxazine allows substantial amount of woodflour to be easily incorporated into the composites. The results showed that mechanical properties from dynamic mechanical analysis and flexural test at filler content below the optimum filler packing show approximately linear relationship with filler loading. The outstanding compatibility between the woodflour and the polybenzoxazine matrix is evidently seen from the large improvement in the composite's T_g and char yield. Scanning electron micrographs of the composite also reveals substantially strong interface between the woodflour filler and the polybenzoxazine matrix. Water absorption of the composites is greatly reduced with increasing the amount of polybenzoxazine due to the inherent low water absorption of the matrix. The polybenzoxazine is; therefore, a highly attractive candidate as high performance lignocellulosic binder or adhesive and other related applications. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 99: 1240–1253, 2006     

Determination of Water Diffusion Coefficients and Dynamics in Adhesive/Carbon Fiber–Reinforced Phenolic Resin Composite Joints

Energy-dispersive X-ray spectroscopy analysis (EDX) is an easy and exact method for determination of water diffusion coefficients and dynamics. Here we have calculated the water diffusion coefficients and dynamics in adhesive/carbon fiber–reinforced phenolic resin composite joints subjected to different surface treatments with both EDX and elemental analysis. The water diffusion coefficients and dynamics in the adhesive joints determined with EDX analysis are almost the same as those determined with elemental analysis. The durability of the adhesive joints with carbon fiber–reinforced phenolic resin composites subjected to silane coupling agent treatment is better than those subjected to sandpaper burnishing and chemical oxidation treatment.     

Focused ion beam processing for transmission electron microscopy of composite/adhesive interfaces

Although most transmission electron microscope (TEM) investigations were carried out using conventional ultramicrotomy, they were limited to the tooth/adhesive resin interface and were difficult to accomplish for the resin-composite interface. Some of these limitations have been overcome with the introduction of focused ion beam (FIB) milling. Therefore, the objective of the study was to compare different composites/adhesive interfaces using FIB/TEM technique. Cylindrical cavities were prepared in extracted human molar teeth. The restored cavities were divided into four groups: (1) One-step self-etch Scotchbond Universal (SBU; 3M ESPE, USA), (2) all-in-one Xeno-V⁺ adhesive (X5P; DENTSPLY, Germany), (3) two-step etch-and-rinse Prime and Bond NT (PNT; DENTSPLY, Germany) that were restored with Filtek Supreme Ultra Universal composite (3M ESPE, USA), and (4) teeth restored with the two-step self-etch Filtek Silorane adhesive (SSA; 3M ESPE, USA) that were restored with its corresponding Filtek Silorane composite (3M ESPE, USA). All specimens were cross-sectioned and subjected to FIB preparation followed by composite/adhesive interfacial TEM examination. The TEM findings were variable and ranged from concentrated clusters of nanoparticles to phase separation of adhesive components and large osmotic blisters. The osmotic blisters in all-in-one adhesives appeared to be influenced by the presence of water and the solvent’s vapor pressure in the cavity. In conclusion, FIB/TEM is a powerful tool allowing the study of biomaterials interaction in situ. The absence of residual water in the adhesives may reduce osmotic blistering that, in turn, may improve the reactivity of the resin monomers, as well as interfacial bonding.     

Environmental Ageing of Adhesively-Bonded Joints. I. Dielectric Studies

High and low frequency dielectric measurements are reported on adhesively bonded aluminum structures aged by exposure to moisture over an extended period of time. The changes observed are interpreted in terms of initially water diffusing into the adhesive layer and there is little evidence of changes occurring to the surface oxide layer. Differences in the form and rate of change of the dielectric signature reflect the effects of the pretreatment and matrix resin on the water diffusion process. A good correlation is observed between the time domain data and the increased dielectric permittivity resulting from ingress of moisture into the adhesive bond. The paper illustrates the use of high frequency dielectric measurements in non-destructively probing adhesive bonds and indicates the potential for in-situ applications.     

The effects of fluids in the aircraft environment on a polyetherimide

Fluid absorption studies have been made for a polyetherimide thermoplastic film and a unidirectional composite of the thermoplastic with graphite fibers immersed in water, JP4 jet fuel, ethylene glycol, and hydraulic fluid. The changes in the weight, thickness, and tensile properties were measured for the film. The changes in the flexural properties of the composite were measured for specimens whose fiber orientation was transverse to their length. Only the hydraulic fluid, which caused an erosion or dissolving of the resin at the specimen surface, affected the film's properties. Both the water and the hydraulic fluid affected the flexural properties of the composite, due to capillary absorption along the fiber-resin interface.     

丙烯酸酯乳液压敏胶的改性研究

在丙烯酸酯乳液共聚中引入改性单体 ,通过交联等方法来调节水乳型压敏胶的内聚力和粘接力。并研究了增粘树脂、表面活性剂对压敏胶性能的影响。     

Flame retardant effect of polyhedral oligomeric silsesquioxane and triglycidyl isocyanurate on glass fibre‐reinforced epoxy composites

Polyhedral oligomeric silsesquioxane (POSS) and triglycidyl isocyanurate (TGIC) were added to an aerospace grade epoxy resin (EP) individually or in combinations at low concentrations. The EP samples containing additives were cast into resin laminates and also used to produce glass fibre‐reinforced composite laminates. The flammability of the two types of laminates was studied by limiting oxygen index, UL‐94 and cone calorimetry. The cone results indicated that the use of POSS (10 wt%) in EP can significantly decrease resin/composite's peak heat release rate, total heat release, and CO production. The mechanical performance in flexural modes of the fibre‐reinforced composite laminates was not adversely affected by the addition of POSS and TGIC in the resin. POSS containing samples had better retention of mechanical properties after exposure to radiant heat in a cone calorimeter compared with other samples. The results of thermogravimetry (TG), TG‐FTIR, and dynamic FTIR indicated that the thermal degradation behavior of the EP is significantly changed by the addition of POSS. POSS can get grafted on the EP's main chain during earlier stages of decomposition and form a stable char layer to protect the underlying material from further decomposition. POLYM. COMPOS., 2011. © 2010 Society of Plastics Engineers     

The effect of different cementing strategies and adhesive interface aging on microtensile bond strength (μTBS) of lithium disilicate ceramics to dentin

This study evaluated the effect of different cementing strategies and adhesive interface aging on microtensile bond strength (μTBS) of lithium disilicate ceramic (IPS e.max CAD) to dentin. Forty coronal dentin fragments were randomly assigned to four groups according to the cementing strategy used to bond lithium disilicate ceramic to coronal dentin surface (n = 10): U200 (self-adhesive resin cement (RC) RelyX U200®/3 M ESPE), SBU (single-step self-etching adhesive system (AS) Single Bond Universal®/3 M ESPE + RelyX ARC®/3 M ESPE RC), AdperSB (two-step etch-and-rinse AS Single Bond 2®/3 M + RelyX ARC®/3 M ESPE RC) and Scotchbond (three-step etch-and-rinse AS Scotchbond Multi-Purpose®/3 M + RelyX ARC®/3 M RC). After 48 h, the ceramic-tooth blocks were sectioned perpendicular to the adhesive interface in the form of sticks and randomly subdivided into two groups according to when they were to be submitted to μTBS testing: immediately or 6 months after storage in water. Some sticks were kept for analysis of the adhesive interface by scanning electron microscopy (SEM). The μTBS test was performed in a universal testing machine (0.5 mm/min). The data (MPa) were analyzed using split-plot ANOVA and Tukey’s test (α = 0.05). Water storage decreased μTBS in all cementing strategies. The μTBS was greatest in the Scotchbond group and lowest in the U200 group, at both storage times. No signs of interface degradation were detected under SEM after water storage. In conclusion, water storage decreased bond strength, regardless of the adhesive cementation strategy, and that the three-step adhesive system/dual-cure resin cement ultimately performed better in terms of bond strength.     

Characteristics of simultaneous epoxy-novolac full interpenetrating polymer network (IPN) adhesive

In this investigation, an attempt has been made on the synthesis of epoxy-novolac IPN adhesive simultaneously by using full interpenetrating polymer network (IPN) technique. Novolac resin is mixed in different weight ratios with respect to epoxy resin. Thereafter, both the resins are cross-linked with their respective cross linker agents simultaneously. This epoxy-novolac IPN adhesive is characterized by various studies such as swelling; cross-link density; dynamic mechanical and thermal analysis and fourier transform inferred spectroscopy (FTIR). The swelling study reveals that the epoxy-novolac IPN adhesive is synthesized through full IPN technique successfully. The cross-link density result shows that epoxy- novolac (4:1) IPN adhesive has greater interpenetration than other epoxy-novolac IPN adhesive systems. Dynamic mechanical and thermal analysis (DMTA) result exhibits that epoxy-novolac (4:1) IPN adhesive is stiffer than another epoxy-novolac IPN adhesive system. The result of FTIR proves that epoxy-novolac IPN adhesive undergoes simultaneously. The results of all these characterization techniques conclude that epoxy-novolac IPN adhesive system with 4:1 ratio is considered to be the best IPN adhesive compared to others epoxy-novolac IPN adhesive systems.     

Effect of clinical and laboratory contamination media on the adhesion of luting cement to direct and indirect resin composite materials

This study evaluated the effect of contamination media on the adhesion of resin cement to resin composites. Specimens of direct (DRC) (Quadrant Photo Posterior) and indirect resin composite (IRC) (Gradia) (N = 300, n = 15 per group) were prepared. Except the control group (C), the specimens of DRC and IRC were contaminated with one of the following media: (a) saliva (S), (b) silicon (SI), (c) dental stone (D), and (d) isolation medium (I). While one half was only rinsed with water, the other half was silica coated (30 μm SiO₂, Siljet). All specimens were silanized (Monobond Plus) and coated with adhesive resin (Heliobond). Resin cement (Variolink II) was bonded to the substrates and photo-polymerized for 40 s. After thermocycling (x5.000, 5–55 °C), composite–cement interface was loaded under shear in a Universal Testing Machine (1 mm/min). Data (MPa) were analyzed using Univariate analysis, Tukey’s and Dunnett-T3 tests. Both contamination media (p = 0.000) and surface conditioning (p = 0.005) significantly affected adhesion to DRC and IRC. No significant difference was found between the DRC and IRC (without: p = 0.098; with: p = 0.084). Significantly lower results were obtained after SI (DRC: 0.66 ± 0.6; IRC: 0.8 ± 1.3) followed by I contamination (DRC: 2.1 ± 2.6; IRC: 0.8 ± 1.3) (p < 0.05). Regardless of contamination medium, surface conditioning significantly increased the results for both DRC (15.1 ± 6.1–23.6 ± 3.7) and IRC (20.3 ± 5.4–25.1 ± 3.6) (p < 0.05). Weibull distribution increased after surface conditioning for both DRC (without: 1.33–3.27; with: 2.55–9.34) and IRC (without: 1.07–3.75; with: 3.7–7.73). Predominantly adhesive (132 out of 150) failures were observed when surfaces were not conditioned.     

Influence of surface treatment on properties of Cocos nucifera L. Var typica fiber reinforced polymer composites

Natural fibers are a powerful competitor in the polymer composite market due to their availability, sustainability, obtainability, cost, and biodegradability. The surface of natural fibers was changed to increase mechanical qualities, hydrophobicity, and bonding with polymer matrix. This study exposes the influence of several surface treatments of coconut tree peduncle fibers (CTPFs) on the thermomechanical and water absorption properties of CTPF-reinforced polymer composites. The CTPFs were treated with sodium hydroxide, benzoyl peroxide, potassium permanganate and stearic acid at a constant 40 wt% and individually reinforced in an unsaturated polyester resin matrix containing 60 wt% CTPFs. Chemically treated CTPFs improved reinforcement-matrix adhesion and enhanced composite mechanical characteristics. In addition, the scanning electron microscope fractographical study of stressed composite specimens shows improved reinforcement-matrix bonding. Moreover, the treated CTPFs have a higher cellulose wt%, which improves the composites crystalline nature, hydrophobicity and thermal stability. The potassium permanganate treated CTPF composite's maximum tensile strength of 128 MPa, flexural strength of 119 MPa, impact strength of 9.9 J/cm², hardness value of 99 HRRW and thermal stability up to 193°C make them appropriate for lightweight mobility and structural applications.     

Evaluation of different desensitizing agents effect on shear bond strength of adhesive resin cement to dentin

Desensitizing agents can inhibit the bonding strength between dentin and adhesive resin cement. This study evaluated the effects of different desensitizing agents on the shear bond strength of adhesive resin cement to dentin. Sixty freshly extracted and caries free teeth were classified into five experimental groups, randomly (n?=?12). Each group was treated with a different desensitizing agent (Teethmate, Shield Force Plus, Admira Protect and Ultra-Ez) respectively, except for an untreated control group. After desensitizing agents and adhesive resin cement were applied to each dentin surface, all specimens were stored in incubator at 37?°C for 24?h. The shear bond strength was tested with a Universal testing machine at a 0.5?mm/min crosshead speed. Data were analysed by using a statistical software (SPSS 22). The results of the measurements were analysed by Kruskal Wallis test with Bonferroni correction and multiple comparisons were made by Wilcoxon test (p???.01). Specimens were examined by a scanning electron microscope, additionally. The Shield Force Plus showed significantly the highest shear bond strength compared with other groups (p?<?.01). Ultra-Ez showed the lowest shear bond strength (p?>?.01). There was no significant difference among Teethmate and Admira Protect groups (p?>?.01). Desensitizing agents containing resin monomers increased the bonding strength, however desensitizers containing calcium phosphate, potassium nitrate and fluoride did not effect the bonding strength of resin cement to dentin.     

Performance of natural‐fiber–plastic composites under stress for outdoor applications: Effect of moisture,temperature, and ultraviolet light exposure

The effects of moisture, temperature, and ultraviolet (UV) light on performance of natural‐fiber–plastic composites (NFPC) were assessed. We conducted short‐term tests in the laboratory and long‐term tests under natural exposure and measured changes in mechanical properties and color in samples of the composite. Chemical changes of the composite's materials were measured by X‐ray photoelectron spectroscopy to elucidate the mechanisms of chemical transformations on the material surface. Relative humidity highly affected the modulus of rupture (MOR) and the modulus of elasticity (MOE), and had a greater effect than temperature and UV exposure on performance of the composite. The lightness of the composite was increased by the UV effect in the short‐ and the long‐term tests. The X‐ray photoelectron spectroscopy (XPS) analysis suggested that the composite was protected by the UV absorber. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 99: 2570–2577, 2006     

Effects of simulated pulpal pressure,mechanical and thermocycling challenge on the microtensile bond strength of resin luting cements

This study aimed at comparing the microtensile bond strength (µTBS) of three simplified luting strategies after different aging processes. Sixty human molars were prepared to expose flat middle dentin surfaces which received the following luting procedures: (i) SB+ARC – two-step etch-and-rinse adhesive+conventional resin cement (Adper Singlebond 2+RelyX ARC, 3M-ESPE); (ii) S3+PAN – one-step self-etch adhesive+conventional resin cement (Clearfil S3+Panavia F2.0, Kuraray Medical); (iii) U200 – self-adhesive resin cement (RelyX U200,3M-ESPE). The specimens were finally restored by indirect resin composite procedures (Filtek Z100,3M-ESPE). The aging regimens were water storage at 37 °C for one week (control), one week of 20 cm H₂O simulated pulpal pressure (SPP), 200,000 mechanical loading (ML) cycles, or 5000 thermal cycles (TC). The µTBS data was analyzed by two-way ANOVA and Tukey's test (α=0.05). SB+ARC showed significantly higher µTBS for control and all aging processes (p<0.001). Nevertheless, TC had no effect on the bond strength of SB+ARC. No difference in µTBS was observed between S3+PAN and U200 after SPP (p=0.251), but significant lower values were found for U200 after ML (p=0.010) besides being superior in the control groups (p<0.001). For U200, all ageing regimens induced significant reductions in the bond strength (p<0.001) with a more pronounced negative effect after ML. S3+PAN showed significant lower bond strength (p=0.010) only after ML aging. Two-step etch-and-rinse adhesive associated with dual-curing conventional resin cement may present the highest overall µTBS. However, the use of S3 one-step self-etch adhesive along with conventional resin cements may provide the most stable luting performance under the tested aging strategy.