Influence of Application Methods of Self-etching Adhesive Systems on Adhesive Bond Strength to Dentin

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Evaluation of Bond Strength of Self-adhesive Cements to Dentin With or Without Application of Adhesive Systems

Purpose: To evaluate the bond strength of indirect restorations to dentin using self-adhesive cements with and without the application of adhesive systems.Material and Methods: Seventy-two bovine incisors were used, in which the buccal surfaces were ground down to expose an area of dentin measuring a minimum of 4 x 4 mm. The indirect resin composite Resilab was used to make 72 blocks, which were cemented onto the dentin surface of the teeth and divided into 4 groups (n = 18): group 1: self-adhesive resin cement BiFix SE, applied according to manufacturer's recommendations; group 2: self-adhesive resin cement RelyX Unicem, used according to manufacturer's recommendations; group 3: etch-and-rinse Solobond M adhesive system + BiFix SE; group 4: etch-and-rinse Single Bond 2 adhesive system + RelyX Unicem. The specimens were sectioned into sticks and subjected to microtensile testing in a universal testing machine (EMIC DL-200MF). Data were subjected to one-way ANOVA and Tukey's test (alpha = 5%).Results: The mean values (+/- standard deviation) obtained for the groups were: group 1: 15.28 (+/- 8.17)(a), group 2: 14.60 (+/- 5.21)(a), group 3: 39.20 (+/- 9.98)(c), group 4: 27.59 (+/- 6.57)(b). Different letters indicate significant differences (ANOVA; p = 0.0000).Conclusion: The application of adhesive systems before self-adhesive cements significantly increased the bond strength to dentin. In group 2, RelyX Unicem associated with the adhesive system Single Bond 2 showed significantly lower mean tensile bond strengths than group 3 (BiFix SE associated with the etch-and-rinse Solobond M adhesive system).

Clinical performance of a self-etching adhesive at 18 months

Purpose: To test the null hypothesis that beveling and/or etching enamel would not affect the 18-month clinical performance of the self-etching adhesive Clearfil SE Bond (CSEB) in noncarious cervical lesions (NCCL). Methods: With Institutional Review Board approval, 34 patients were enrolled in this study. A total of 120 NCCL was selected and assigned to four groups: (1) CSEB was applied without any cavity preparation; (2) CSEB was applied after beveling enamel; (3) CSEB was applied after etching enamel for 15 seconds with 35% phosphoric acid; (4) CSEB was applied after beveling and etching enamel. A microfilled composite resin was used for all restorations. Resuts: At 6 months after initial placement, 120 restorations (a 100% recall rate) were evaluated. At 18 months, 87 restorations (a 72.5% recall rate) were available for evaluation. A survival rate of 100% was measured for all groups at both 6 and 18 months. Sensitivity to air decreased significantly only for Group 3 (no bevel+acid etch) from baseline to 18 months without statistical changes from 6 months to 18 months. None of the other parameters resulted in significant differences for any of the four groups. However, when data were pooled, both the overall marginal discoloration and the overall marginal adaptation were significantly worse at 18 months than at baseline, while sensitivity to air decreased significantly from baseline to 18 months. The 18-month survival rate of the self-etching adhesive Clearfil SE Bond was not improved by enamel bevel or by enamel etching. Both overall marginal adaptation and overall marginal discoloration were worse at 18 months than at baseline.

Localized mechanics of dentin self-etching adhesive system

The bond strength of composite resins (CRs) to dentin is influenced by the interfacial microstructure of the hybrid layer (HL) and the resin tags (TAG). The contemporary self-etching primer adhesive systems overcame the inconvenient of the etch-and-rinse protocol. Studies, however, have demonstrated that HL thickness and TAG length vary according to the wetting time and additional use of acid-etching prior to self-etching primers. This study investigated the localized stress distribution in the HL and the dentin/adhesive interface. Two HL thicknesses (3 or 6 mu m), two TAG lengths (13 or 17 mu m) and two loading conditions (perpendicular and oblique-25 degrees) were investigated by the finite element (FE) analysis. Five two-dimensional FE models (M) of a dentin specimen restored with CR (38 x 64 mu m) were constructed: M1 - no HL and no TAG; M2 - 3 mu m of HL and 13 mu m of TAG; M3 - 3 mu m of HL and 17 mu m of TAG; M4 - 6 mu m of HL and 13 mu m of TAG; and M5 - 6 mu m of HL and 17 mu m of TAG. Two distributed loadings (L) (20N) were applied on CR surface: L1 - perpendicular, and L2 - oblique (25 degrees). Fixed interfacial conditions were assigned on the border of the dentin specimen. Ansys 10.0 (Ansys (R), Houston, PA, USA) software was used to calculate the stress fields. The peak of von Mises (sigma(vM)) and maximum principal stress (sigma(max)) was higher in L2 than in L1. Microstructures (HL and TAG) had no effect on local stresses for L1. Decreasing HL decreased sigma(vM) and sigma(max) in all structures for L2, but the TAG length had influence only on the peributular dentin. The thickness of HL had more influence on the sigma(vM) and sigma(max) than TAG length. The peritubular dentin and its adjacent structures showed the highest sigma(vM) and sigma(max), mainly in the oblique loading.

Clinical evaluation of postoperative sensitivity using self-etching adhesives containing glutaraldehyde

The present clinical study aimed to assess the postoperative sensitivity (POS) after 48 hours and seven days in occlusal restorations bonded with three different adhesive systems, two of them containing glutaraldehyde. The restorative procedures were performed using the three-step etch-and-rinse Adper SBMP-Plus adhesive (SBMP), the two-step etch-and-rinse Gluma Comfort One Bond + Desensitizer adhesive (GC+D) and the all-in-one self-etching/priming I Bond (IB) adhesive, which also has glutaraldehyde in its formula. All cavities were restored with Filtek Supreme nanoparticle composite resin. After 48 hours and seven days the patients were recalled and the postoperative sensitivity evaluated. The data analyzed by non-parametric Friedman test showed no significant differences in POS among the three tested groups after 48 hours and seven days.

Two-year Clinical Performance of Self-etching Adhesive Systems in Composite Restorations of Anterior Teeth

Objective: The aim of this study was to evaluate the two-year clinical performance of Class III, IV, and V composite restorations using a two-step etch-and-rinse adhesive system (2-ERA) and three one-step self-etching adhesive systems (1-SEAs).Material and Methods: Two hundred Class III, IV, and V composite restorations were placed into 50 patients. Each patient received four composite restorations (Amaris, Voco), and these restorations were bonded with one of three 1-SEAs (Futurabond M, Voco; Clearfil S3 Bond, Kuraray; and Optibond All-in-One, Kerr) or one 2-ERA (Adper Single Bond 2/3M ESPE). The four adhesive systems were evaluated at baseline and after 24 months using the following criteria: restoration retention, marginal integrity, marginal discoloration, caries occurrence, postoperative sensitivity and preservation of tooth vitality. After two years, 162 restorations were evaluated in 41 patients. Data were analyzed using the chi(2) test (p<0.05).Results: There were no statistically significant differences between the 2-ERA and the 1-SEAs regarding the evaluated parameters (p>0.05).Conclusion: The 1-SEAs showed good clinical performance at the end of 24 months.

Push-out bond strength of CAD/CAM-ceramic luted to dentin with self-adhesive resin cements

OBJECTIVES: This study evaluated the initial and the artificially aged push-out bond strength between ceramic and dentin produced by one of five resin cements. METHODS: Two-hundred direct ceramic restorations (IPS Empress CAD) were luted to standardized Class I cavities in extracted human molars using one of four self-adhesive cements (SpeedCEM, RelyX Unicem Aplicap, SmartCem2 and iCEM) or a reference etch-and-rinse resin cement (Syntac/Variolink II) (n=40/cement). Push-out bond strength (PBS) was measured (1) after 24h water storage (non-aged group; n=20/cement) or (2) after artificial ageing with 5000 thermal cycles followed by 6 months humid storage (aged group; n=20/cement). Nonparametrical ANOVA and pairwise Wilcoxon rank-sum tests with Bonferroni-Holm adjustment were applied for statistical analysis. The significance level was set at alpha=0.05. In addition, failure mode and fracture pattern were analyzed by stereomicroscope and scanning electron microscopy. RESULTS: Whereas no statistically significant effect of storage condition was found (p=0.441), there was a significant effect of resin cement (p<0.0001): RelyX Unicem showed significantly higher PBS than the other cements. Syntac/Variolink II showed significantly higher PBS than SmartCEM2 (p<0.001). No significant differences were found between SpeedCEM, SmartCem2, and iCEM. The predominant failure mode was adhesive failure of cements at the dentin interface except for RelyX Unicem which in most cases showed cohesive failure in ceramic. SIGNIFICANCE: The resin cements showed marked differences in push-out bond strength when used for luting ceramic restorations to dentin. Variolink II with the etch-and-rinse adhesive Syntac did not perform better than three of the four self-adhesive resin cements tested.

Advancing atomic nanolithography: cold atomic Cs beam exposure of alkanethiol self-assembled monolayers

We report the results of a study into the quality of functionalized surfaces for nanolithographic imaging. Self-assembled monolayer (SAM) coverage, subsequent post-etch pattern definition and minimum feature size all depend on the quality of the Au substrate used in atomic nanolithographic experiments. We find sputtered Au substrates yield much smoother surfaces and a higher density of {111} oriented grains than evaporated Au surfaces. A detailed study of the self-assembly mechanism using molecular resolution AFM and STM has shown that the monolayer is composed of domains with sizes typically of 5-25 nm, and multiple molecular domains can exist within one Au grain. Exposure of the SAM to an optically-cooled atomic Cs beam traversing a two-dimensional array of submicron material masks ans also standing wave optical masks allowed determination of the minimum average Cs dose (2 Cs atoms per SAM molecule) and the realization of < 50 nm structures. The SAM monolayer contains many non-uniformities such as pin-holes, domain boundaries and monoatomic depressions which are present in the Au surface prior to SAM adsorption. These imperfections limit the use of alkanethiols as a resist in atomic nanolithography experiments. These studies have allowed us to realize an Atom Pencil suitable for deposition of precision quantities of material at the microand nanoscale to an active surface.

Atomic nanolithography patterning of submicron features: writing an organic self-assembled monolayer with cold bright Cs atom beams

Cs atom beams, transversely collimated and cooled, passing through material masks in the form of arrays of reactive-ion-etched hollow Si pyramidal tips and optical masks formed by intense standing light waves, write submicron features on self-assembled monolayers (SAMs). Features with widths as narrow as 43 ± 6 nm and spatial resolution limited only by the grain boundaries of the substrate have been realized in SAMs of alkanethiols. The material masks write two-dimensional arrays of submicron holes; the optical masks result in parallel lines spaced by half the optical wavelength. Both types of feature are written to the substrate by exposure of the masked SAM to the Cs flux and a subsequent wet chemical etch. For the arrays of pyramidal tips, acting as passive shadow masks, the resolution and size of the resultant feature depends on the distance of the mask array from the SAM, an effect caused by the residual divergence of the Cs atom beam. The standing wave optical mask acts as an array of microlenses focusing the atom flux onto the substrate. Atom 'pencils' writing on SAMs have the potential to create arbitrary submicron figures in massively parallel arrays. The smallest features and highest resolutions were realized with SAMs grown on smooth, sputtered gold substrates.

Writing self-assembled monolayers with Cs: Optimization of atomic nanolithography imaging using self-assembled monolayers on gold substrates

We report the results of a study into the factors controlling the quality of nanolithographic imaging. Self-assembled monolayer (SAM) coverage, subsequent postetch pattern definition, and minimum feature size all depend on the quality of the Au substrate used in material mask atomic nanolithographic experiments. We find that sputtered Au substrates yield much smoother surfaces and a higher density of {111}-oriented grains than evaporated Au surfaces. Phase imaging with an atomic force microscope shows that the quality and percentage coverage of SAM adsorption are much greater for sputtered Au surfaces. Exposure of the self-assembled monolayer to an optically cooled atomic Cs beam traversing a two-dimensional array of submicron material masks mounted a few microns above the self-assembled monolayer surface allowed determination of the minimum average Cs dose (2 Cs atoms per self-assembled monolayer molecule) to write the monolayer. Suitable wet etching, with etch rates of 2.2 nm min-1, results in optimized pattern definition. Utilizing these optimizations, material mask features as small as 230 nm in diameter with a fractional depth gradient of 0.820 nm were realized.

Study of the kinetics and mechanism of rapid self-assembly in block copolymer thin films during solvo-microwave annealing

Microwave annealing is an emerging technique for achieving ordered patterns of block copolymer films on substrates. Little is understood about the mechanisms of microphase separation during the microwave annealing process and how it promotes the microphase separation of the blocks. Here, we use controlled power microwave irradiation in the presence of tetrahydrofuran (THF) solvent, to achieve lateral microphase separation in high- lamellar-forming poly(styrene-b-lactic acid) PS-b-PLA. A highly ordered line pattern was formed within seconds on silicon, germanium and silicon on insulator (SOI) substrates. In-situ temperature measurement of the silicon substrate coupled to condition changes during "solvo-microwave" annealing allowed understanding of the processes to be attained. Our results suggest that the substrate has little effect on the ordering process and is essentially microwave transparent but rather, it is direct heating of the polar THF molecules that causes microphase separation. It is postulated that the rapid interaction of THF with microwaves and the resultant temperature increase to 55 degrees C within seconds causes an increase of the vapor pressure of the solvent from 19.8 to 70 kPa. This enriched vapor environment increases the plasticity of both PS and PLA chains and leads to the fast self-assembly kinetics. Comparing the patterns formed on silicon, germanium and silicon on insulator (SOI) and also an in situ temperature measurement of silicon in the oven confirms the significance of the solvent over the role of substrate heating during "solvo-microwave" annealing. Besides the short annealing time which has technological importance, the coherence length is on a micron scale and dewetting is not observed after annealing. The etched pattern (PLA was removed by an Ar/O-2 reactive ion etch) was transferred to the underlying silicon substrate fabricating sub-20 nm silicon nanowires over large areas demonstrating that the morphology is consistent both across and through the film.

High Precision Plasma Etch for Pattern Transfer: Towards Fluorocarbon Based Atomic Layer Etching

A basic requirement of a plasma etching process is fidelity of the patterned organic materials. In photolithography, a He plasma pretreatment (PPT) based on high ultraviolet and vacuum ultraviolet (UV/VUV) exposure was shown to be successful for roughness reduction of 193nm photoresist (PR). Typical multilayer masks consist of many other organic masking materials in addition to 193nm PR. These materials vary significantly in UV/VUV sensitivity and show, therefore, a different response to the He PPT. A delamination of the nanometer-thin, ion-induced dense amorphous carbon (DAC) layer was observed. Extensive He PPT exposure produces volatile species through UV/VUV induced scissioning. These species are trapped underneath the DAC layer in a subsequent plasma etch (PE), causing a loss of adhesion. Next to stabilizing organic materials, the major goals of this work included to establish and evaluate a cyclic fluorocarbon (FC) based approach for atomic layer etching (ALE) of SiO2 and Si; to characterize the mechanisms involved; and to evaluate the impact of processing parameters. Periodic, short precursor injections allow precise deposition of thin FC films. These films limit the amount of available chemical etchant during subsequent low energy, plasma-based Ar+ ion bombardment, resulting in strongly time-dependent etch rates. In situ ellipsometry showcased the self-limited etching. X-ray photoelectron spectroscopy (XPS) confirms FC film deposition and mixing with the substrate. The cyclic ALE approach is also able to precisely etch Si substrates. A reduced time-dependent etching is seen for Si, likely based on a lower physical sputtering energy threshold. A fluorinated, oxidized surface layer is present during ALE of Si and greatly influences the etch behavior. A reaction of the precursor with the fluorinated substrate upon precursor injection was observed and characterized. The cyclic ALE approach is transferred to a manufacturing scale reactor at IBM Research. Ensuring the transferability to industrial device patterning is crucial for the application of ALE. In addition to device patterning, the cyclic ALE process is employed for oxide removal from Si and SiGe surfaces with the goal of minimal substrate damage and surface residues. The ALE process developed for SiO2 and Si etching did not remove native oxide at the level required. Optimizing the process enabled strong O removal from the surface. Subsequent 90% H2/Ar plasma allow for removal of C and F residues.

Low-density Three-dimensional Foam Using Self-reinforced Hybrid Two-dimensional Atomic Layers.

Low-density nanostructured foams are often limited in applications due to their low mechanical and thermal stabilities. Here we report an approach of building the structural units of three-dimensional (3D) foams using hybrid two-dimensional (2D) atomic layers made of stacked graphene oxide layers reinforced with conformal hexagonal boron nitride (h-BN) platelets. The ultra-low density (1/400 times density of graphite) 3D porous structures are scalably synthesized using solution processing method. A layered 3D foam structure forms due to presence of h-BN and significant improvements in the mechanical properties are observed for the hybrid foam structures, over a range of temperatures, compared with pristine graphene oxide or reduced graphene oxide foams. It is found that domains of h-BN layers on the graphene oxide framework help to reinforce the 2D structural units, providing the observed improvement in mechanical integrity of the 3D foam structure.

[gait Speed, Grip Strength And Self-rated Health Among The Elderly: Data From The Fibra Campinas Network, São Paulo, Brazil].

The article seeks to investigate patterns of performance and relationships between grip strength, gait speed and self-rated health, and investigate the relationships between them, considering the variables of gender, age and family income. This was conducted in a probabilistic sample of community-dwelling elderly aged 65 and over, members of a population study on frailty. A total of 689 elderly people without cognitive deficit suggestive of dementia underwent tests of gait speed and grip strength. Comparisons between groups were based on low, medium and high speed and strength. Self-related health was assessed using a 5-point scale. The males and the younger elderly individuals scored significantly higher on grip strength and gait speed than the female and oldest did; the richest scored higher than the poorest on grip strength and gait speed; females and men aged over 80 had weaker grip strength and lower gait speed; slow gait speed and low income arose as risk factors for a worse health evaluation. Lower muscular strength affects the self-rated assessment of health because it results in a reduction in functional capacity, especially in the presence of poverty and a lack of compensatory factors.

Self-reported Diabetes In Older People: Comparison Of Prevalences And Control Measures.

The objective of this study was to analyze the prevalence of diabetes in older people and the adopted control measures. Data regarding older diabetic individuals who participated in the Health Surveys conducted in the Municipality of Sao Paulo, SP, ISA-Capital, in 2003 and 2008, which were cross-sectional studies, were analyzed. Prevalences and confidence intervals were compared between 2003 and 2008, according to sociodemographic variables. The combination of the databases was performed when the confidence intervals overlapped. The Chi-square (level of significance of 5%) and the Pearson's Chi-square (Rao-Scott) tests were performed. The variables without overlap between the confidence intervals were not tested. The age of the older adults was 60-69 years. The majority were women, Caucasian, with an income of between > 0.5 and 2.5 times the minimum salary and low levels of schooling. The prevalence of diabetes was 17.6% (95%CI 14.9;20.6) in 2003 and 20.1% (95%CI 17.3;23.1) in 2008, which indicates a growth over this period (p at the limit of significance). The most prevalent measure adopted by the older adults to control diabetes was hypoglycemic agents, followed by diet. Physical activity was not frequent, despite the significant differences observed between 2003 and 2008 results. The use of public health services to control diabetes was significantly higher in older individuals with lower income and lower levels of education. Diabetes is a complex and challenging disease for patients and the health systems. Measures that encourage health promotion practices are necessary because they presented a smaller proportion than the use of hypoglycemic agents. Public health policies should be implemented, and aimed mainly at older individuals with low income and schooling levels. These changes are essential to improve the health condition of older diabetic patients.