Anisotropic Etching and Nanoribbon Formation in Single-Layer Graphene

We demonstrate anisotropic etching of single-layer graphene by thermally activated nickel nanoparticles. Using this technique, we obtain sub-10-nm nanoribbons and other graphene nanostructures with edges aligned along a single crystallographic direction. We observe a new catalytic channeling behavior, whereby etched cuts do not intersect, resulting in continuously connected geometries. Raman spectroscopy and electronic measurements show that the quality of the graphene is resilient under the etching conditions, indicating that this method may serve as a powerful technique to produce graphene nanocircuits with well-defined crystallographic edges.

Erbium, chromium : yttrium scandium gallium garnet laser for caries removal: influence on bonding of a self-etching adhesive system

This study evaluated the influence of the dental substrates obtained after the use of different caries removal techniques on bonding of a self-etching system. Forty, extracted, carious, human molars were ground to expose flat surfaces containing caries-infected dentine surrounded by sound dentine. The caries lesions of the specimens were removed or not (control-G1) either by round steel burs and water-cooled, low speed, handpiece (G2), or by irradiation with an erbium, chromium:yttrium scandium gallium garnet (Er,Cr:YSGG) laser (2W, 20 Hz, 35.38 J/cm(2), fiber G4 handpiece with 0.2826 mm(2), non-contact mode at a 2 mm distance, 70% air/20% water-G3) or using a chemo-mechanical method (Carisolv-G4). Caries-infected, caries-affected and sound dentines were submitted to a bonding system followed by construction of a resin-based composite crown. Hour-glass shaped samples were obtained and submitted to a micro-tensile bond test. The bond strength data were compared by analysis of variance (ANOVA), complemented by Tukey`s test (P <= 0.05). The samples of sound dentine presented higher bond strengths than did samples of caries-affected dentine, except for the groups treated with the Er,Cr:YSGG laser. The highest bond strengths were observed with the sound dentine treated with burs and Carisolv. The bond strengths to caries-affected dentine were similar in all groups. Additionally, bonding to caries-affected dentine of the Er,Cr:YSGG laser and Carisolv groups was similar to bonding to caries-infected dentine. Thus, caries-affected dentine is not an adequate substrate for adhesion. Moreover, amongst the caries removal methods tested, the Er,Cr:YSGG laser irradiation was the poorest in providing a substrate for bonding with the tested self-etching system.

Lithography-free micro- and nanostructuring based on conventional plasma etching

In now-a-days semiconductor and MEMS technologies the photolithography is the working horse for fabrication of functional devices. The conventional way (so called Top-Down approach) of microstructuring starts with photolithography, followed by patterning the structures using etching, especially dry etching. The requirements for smaller and hence faster devices lead to decrease of the feature size to the range of several nanometers. However, the production of devices in this scale range needs photolithography equipment, which must overcome the diffraction limit. Therefore, new photolithography techniques have been recently developed, but they are rather expensive and restricted to plane surfaces. Recently a new route has been presented - so-called Bottom-Up approach - where from a single atom or a molecule it is possible to obtain functional devices. This creates new field - Nanotechnology - where one speaks about structures with dimensions 1 - 100 nm, and which has the possibility to replace the conventional photolithography concerning its integral part - the self-assembly. However, this technique requires additional and special equipment and therefore is not yet widely applicable. This work presents a general scheme for the fabrication of silicon and silicon dioxide structures with lateral dimensions of less than 100 nm that avoids high-resolution photolithography processes. For the self-aligned formation of extremely small openings in silicon dioxide layers at in depth sharpened surface structures, the angle dependent etching rate distribution of silicon dioxide against plasma etching with a fluorocarbon gas (CHF3) was exploited. Subsequent anisotropic plasma etching of the silicon substrate material through the perforated silicon dioxide masking layer results in high aspect ratio trenches of approximately the same lateral dimensions. The latter can be reduced and precisely adjusted between 0 and 200 nm by thermal oxidation of the silicon structures owing to the volume expansion of silicon during the oxidation. On the basis of this a technology for the fabrication of SNOM calibration standards is presented. Additionally so-formed trenches were used as a template for CVD deposition of diamond resulting in high aspect ratio diamond knife. A lithography-free method for production of periodic and nonperiodic surface structures using the angular dependence of the etching rate is also presented. It combines the self-assembly of masking particles with the conventional plasma etching techniques known from microelectromechanical system technology. The method is generally applicable to bulk as well as layered materials. In this work, layers of glass spheres of different diameters were assembled on the sample surface forming a mask against plasma etching. Silicon surface structures with periodicity of 500 nm and feature dimensions of 20 nm were produced in this way. Thermal oxidation of the so structured silicon substrate offers the capability to vary the fill factor of the periodic structure owing to the volume expansion during oxidation but also to define silicon dioxide surface structures by selective plasma etching. Similar structures can be simply obtained by structuring silicon dioxide layers on silicon. The method offers a simple route for bridging the Nano- and Microtechnology and moreover, an uncomplicated way for photonic crystal fabrication.

Micro-Raman spectroscopy and SEM/EDX applied to improve the zircon fission track method used for dating geological formations

The zircon mineral is widely studied in geochronology. In the case of the fission track method (FTM), the age is determined by the density of fission tracks at the zircon surface, which can be observed with an optical microscope after an appropriate chemical treatment (etching). The etching must be isotropic at the zircon grain surface to be used in the FTM, which leads those zircon grains whose etching is anisotropic to be discarded. The only reason for this discarding is the nonuniform morphology of the surface grain seen by optical microscopy, that is, no further physicochemical analysis is performed. In this work, combining micro-Raman and scanning electron microscopy (SEM) to study the etching anisotropy, it was shown that zircon grains that present at least one area at the surface where the density of fission track is uniform can be used in the FTM. The micro-Raman showed characteristic spectra of the standard zircon sample either from the areas where there are tracks or from where there are not. The only difference found was in the Raman bandwidths, which were broader for the areas with higher density of fission tracks. This suggests simply a decrease in the relative percentage of the crystalline/amorphous phases at these areas. The SEM/energy dispersive spectrometry (EDX) showed that there were no significant differences in the principal chemical composition at the areas with and without fission tracks. Copyright (c) 2008 John Wiley & Sons, Ltd.

Influence of human dentine on the antibacterial activity of self-etching adhesive systems against cariogenic bacteria

Objectives: The incorporation of antibacterial agents into adhesive systems has been proposed to eliminate residual bacteria from dentine. This study used the agar diffusion method to evaluate the antibacterial activity of Clearfil Protect Bond (CPB), Clearfil SE Bond (CSEB), Clearfil Tri-S Bond (C3SB) and Xeno-III (XIII) self-etching adhesive systems, with or without light-activation, against cariogenic bacteria, and to assess the influence of human dentine on the antibacterial activity of these materials.Methods: An aliquot of 10 mu l per material (and individual components) were pipetted onto paper and dentine discs distributed in Petri dishes containing bacterial culture in BHI agar. Positive control was 0.2% chlorhexidine digluconate (CHX).Results: After incubation, the adhesive components of CPB and CSEB, liquid A of XIII and C3SB did not present antibacterial activity when applied to paper discs. The non-light-activated CPB primer + adhesive promoted the greatest inhibition of Streptococcus mutans (p < 0.05), whereas with light-activation, there was no significant difference between primer + adhesive and primer alone. For Lactobacillus acidophilus, CPB primer presented the greatest antibacterial activity in both light-activation conditions (p < 0.05). Regarding the dentine discs, only CHX promoted an inhibitory effect, though less intense than on paper discs (p < 0.05). CHX presented greater antibacterial activity against S. mutans than against L. acidophilus (p < 0.05).Conclusions: Light-activation significantly reduced the antibacterial activity of the self-etching adhesive systems; MDPB incorporation contributed to the effect of adhesive systems against cariogenic bacteria; the components eluted from the adhesive systems were not capable to diffuse through 400 mu m-thick dentine disc to exert their antibacterial activity against cariogenic bacteria. (C) 2008 Elsevier Ltd. All rights reserved.

Microshear Bond Strength of Self-etching Bonding Systems to Ultrasound Diamond Bur-prepared Dentin

Purpose: The aim of this study was to evaluate the influence of dentin abrasion on the microshear bond strength of two self-etching adhesive systems, using either an ultrasound diamond bur or a high-speed diamond bur.Materials and Methods: Twenty noncarious human third molars were sectioned mesiodistally into halves. The enamel was ground to expose a flat dentin surface on both sections. The dentinal surfaces were randomly assigned to two groups, depending on the method of smear layer preparation: ultrasound diamond bur (UB) or conventional diamond bur (CB). The prepared dentin surfaces received one of two self-etching systems: Clearfil SE Bond (CF) and One-Up Bond F (OB). A composite cylinder with a 0.95-mm diameter was bonded to each specimen and the microshear bond test was performed. The results were expressed in MPa and were subjected to two-way analysis of variance (ANOVA) and Tukey's test (alpha = 0.05).Results: There was no significant difference in dentin bond strength when comparing the conventional and ultrasonic abrasion methods. When the adhesive systems were compared, Clearfil SE Bond achieved higher bond strength means than did One-Up Bond F.Conclusion: The dentin surface preparation method did not influence the microshear bond strength and the Clearfil SE Bond adhesive system, independent of bur type used, Clearfil SE Bond showed higher bond strengths than did the One-Up Bond F adhesive system.

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)

Microtensile bond strength of a resin cement to feldpathic ceramic after different etching and silanization regimens in dry and aged conditions

Objectives. This study evaluated the durability of bond strength between resin cement and a feldspathic ceramic submitted to different etching regimens with and without silane coupling agent application.Methods. Thirty-two blocks (6.4 mm x 6.4 mm x 4.8 mm) were fabricated using a microparticulate feldspathic ceramic (Vita VM7), ultrasonically cleaned with water for 5 min and randomly divided into four groups, according to the type of etching agent and silanization method: method 1, etching with 10% hydrofluoric (HF) acid gel for I min + silanization; method 2, HF only; method 3, etching with 1.23% acidulated phosphate fluoride (APF) for 5 min + silanization; method 4, APF only. Conditioned blocks were positioned in their individual silicone molds and resin cement (Panavia F) was applied on the treated surfaces. Specimens were stored in distilled water (37 degrees C) for 24 h prior to sectioning. After sectioning the ceramic-cement blocks in x- and Y-axis with a bonded area of approximately 0.6 mm(2), the microsticks of each block were randomly divided into two storage conditions: Dry, immediate testing; TC, thermal cycling (12,000 times) + water storage for 150 d, yielding to eight experimental groups. Microtensile bond strength tests were performed in universal testing machine (cross-head speed: 1 mm/min) and failure types were noted. Data obtained (MPa) were analyzed with three-way ANOVA and Tukey's test (alpha = 0.05).Results. Significant influence of the use of silane (p < 0.0001), storage conditions (p = 0.0013) and surface treatment were observed (p = 0.0014). The highest bond strengths were achieved in both dry and thermocycled conditions when the ceramics were etched with HF acid gel and silanized (17.4 +/- 5.8 and 17.4 +/- 4.8 MPa, respectively). Silanization after HF acid gel and APT treatment increased the results dramatically (14.5 +/- 4.2-17.4 +/- 4.8 MPa) compared to non-silanized groups (2.6 +/- 0.8-8.9 +/- 3.1 MPa) where the failure type was exclusively (100%) adhesive between the cement and the ceramic.Significance. Silanization of the feldspathic ceramic surface after APF or HF acid etching increased the microtensile bond strength results significantly, with the latter providing higher results. Long-term thermocycling and water storage did not decrease the results in silanized groups. (C) 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

A method for the digital image analysis of ceramic grains based on shape factor segmentation

A very simple and robust method for ceramics grains quantitative image analysis is presented. Based on the use of optimal imaging conditions for reflective light microscopy of bulk samples, a digital image processing routine was developed for shading correction, noise suppressing and contours enhancement. Image analysis was done for grains selected according to their concavities, evaluated by perimeter ratio shape factor, to avoid consider the effects of breakouts and ghost boundaries due to ceramographic preparation limitations. As an example, the method was applied for two ceramics, to compare grain size and morphology distributions. In this case, most of artefacts introduced by ceramographic preparation could be discarded due to the use of perimeter ratio exclusion range.

Influence of cavity preparation and curing method on the marginal seal of resin composite restorations: an in vitro evaluation.

OBJECTIVE: To evaluate the influence of cavity design and photocuring method on the marginal seal of resin composite restorations. METHOD AND MATERIALS: Seventy-two bovine teeth were divided into 2 groups: group 1 received box-type cavity preparations, and group 2 received plate-type preparations. Each group was divided into 3 subgroups. After etching and bonding, Z250 resin composite (3M Espe) was applied in 2 equal increments and cured with 1 of 3 techniques: (1) conventional curing for 30 seconds at 650 mW/cm2; (2) 2-step photocuring, in which the first step was performed 14 mm from the restoration for 10 seconds at 180 mW/cm2 and the second step was performed in direct contact for 20 seconds at 650 mW/cm2; or (3) progressive curing using Jetlite 4000 (J. Morita) for 8 seconds at 125 mW/cm2 and then 22 seconds at 125 mW/cm2 up to 500 mW/cm2. The specimens were thermocycled for 500 cycles and then submitted to dye penetration with a 50% silver nitrate solution. Microleakage was assessed using a stereomicroscope. Data were analyzed using analysis of variance and Tukey test (5% level of significance). RESULTS: A statistically significant difference was found between groups when a double interaction between photocuring and cavity preparation was considered (P = .029). CONCLUSIONS: No one type of cavity preparation or photocuring method prevented micro-leakage. The plate-type preparation showed the worst dye penetration when conventional and progressive photocuring methods were used. The best results were found using the 2-step photocuring with the plate-type preparation.

Resin microtensile bond strength to feldspathic ceramic: Hydrofluoric acid etching vs tribochemical silica coating

This study aimed to compare the microtensile bond strength of resin cement to alumina-reinforced feldspathic ceramic submitted to acid etching or chairside tribochemical silica coating. Ten blocks of Vitadur-α were randomly divided into 2 groups according to conditioning method: (1) etching with 9.6% hydrofluoric acid or (2) chairside tribochemical silica coating. Each ceramic block was luted to the corresponding resin composite block with the resin cement (Panavia F). Next, bar specimens were produced for microtensile testing. No significant difference was observed between the 2 experimental groups (Student t test, P> .05). Both surface treatments showed similar microtensile bond strength values.

Observation of tags and hybrid layer of a single bottle conventional adhesive system and a self-etching adhesive system, on sound dentin.

This experimental light microscopy study investigated the formation of a hybrid layer and resin tags on sound dentin, after utilization of conventional and self-etching adhesive systems. After restorative procedures, the specimens were decalcified in a formic acid and sodium citrate solution, embedded in paraffin, sectioned at 6-microm thickness and stained by the Brown & Brenn method for analysis and measurement by light microscopy (AXIOPHOT) (400x). The results were statistically analyzed by analysis of variance, at a significance level of 5%. Based on the results, it could be concluded that the conventional adhesive allowed the formation of a thicker hybrid layer than the self-etching adhesive, with similar penetration into the dentinal tubules (resin tags).

Analysis of the effects of thermal cycling on the microtensile shear bond strength of a self-etching and a conventional pit and fissure sealants to dental enamel

Objective: To analyze the effects of thermal cycling on the microtensile shear bond strength of a self-etching and a conventional pit and fissure sealants to dental enamel. Material and Method: Twenty-four healthy human molars extracted for orthodontic reasons, were sectioned in the mesio-distal direction and divided into two groups (n=24) according to the sealant to be applied: GI - conventional sealant Climpro (3M/ESPE) and GII - self-etching sealant Enamel Loc (Premier Dental). The sealants were applied on flattened enamel in matrixes 1 mm in diameter, in accordance with the manufacturers' recommendations. The specimens were stored in distilled water at 37°C for 24 hours. After this, half the samples of both groups were submitted to 500 thermal cycles in 30s baths at temperatures between 5 and 55°C. Forty-eight hours after the samples were made, the microtensile shear test was performed in an Instron 4411 test machine, with a stainless steel wire with a cylindrical cross section of 0.2mm in diameter at a constant speed of 0.5mm/s. The bond strength values were submitted to ANOVA for 2 factors and the fracture patterns were examined under an optical microscope at 65X magnification. Results: Thermal cycling did not influence the bond strength of the two sealants. The conventional sealant Climpro presented a statistically higher microtensile shear bond strength (11.72MPa, 11.34MPa with and without cycling, respectively) than the self-etching sealant Enamel Loc (5.92MPa, 5.02MPa with and without cycling, respectively). Fracture pattern analysis showed the occurrence of 100% of adhesive failures for Enamel Loc, while the conventional sealant Climpro presented 95% of adhesive failures and 5% of mixed failures. Conclusion: The conventional sealant presented higher microtensile shear bond strength to dental enamel in comparison with the self-etching sealant. Thermal cycling did not affect the bond strength of the sealants used in this study. © 2011 Nova Science Publishers, Inc.

Influence of concentration, time and method of application of citric acid and sodium citrate in root conditioning.

The aim of this study was to establish the parameters of concentration, time and mode of application of citric acid and sodium citrate in relation to root conditioning. A total of 495 samples were obtained and equally distributed among 11 groups (5 for testing different concentrations of citric acid, 5 for testing different concentrations of sodium citrate and 1 control group). After laboratorial processing, the samples were analyzed under scanning electron microscopy. A previously calibrated and blind examiner evaluated micrographs of the samples. Non-parametric statistical analysis was performed to analyze the data obtained. Brushing 25% citric acid for 3 min, promoted greater exposure of collagen fibers in comparison with the brushing of 1% citric acid for 1 minute and its topical application at 1% for 3 min. Sodium citrate exposed collagen fibers in a few number of samples. Despite the lack of statistical significance, better results for collagen exposure were obtained with brushing application of 25% citric acid for 3 min than with other application parameter. Sodium citrate produced a few number of samples with collagen exposure, so it is not indicated for root conditioning.

Effects of surface treatment, hydration and application method on the bond strength of a silorane adhesive and resin system to dentine

Objectives: To evaluate the effects of surface treatment, surface hydration (SH) and application method (AM) on the tensile bond strength of the Silorane Adhesive System (SAS) to dentine. Methods: Ninety bovine teeth were used. For the control group (n = 10), each dentine surface was treated according to the manufacturer's instructions of the SAS. The remaining teeth were randomly distributed into two groups (n = 40), according to the type of dentine surface treatment (ST) - 37% phosphoric acid or Er:YAG Laser prior to the application of the SAS. Each group was further divided into 2 subgroups (n = 20), according to the SH status: dry (D) or wet (W). Each subgroup was further divided into 2 subgroups (n = 10), according to the application method [AM: Active (AC) mode or Passive (PA) mode]. A coat of resin composite (Filtek P90) was applied on the surface. Artificial ageing was performed with a thermo-mechanical cycling machine. The specimens were sectioned into 1 mm × 1 mm × 10 mm sticks and stressed to failure using a universal testing machine. The remaining teeth in each group were used for Scanning Electron Microscopy to examine the fractured area. Data were subjected to a three-way ANOVA, Tukey's test and Dunnet's test (α = 0.05). Results: The ANOVA showed significant differences for SH and AM, but not for ST. For SH, the results of Tukey's test were (in MPa): D-14.9(±3.8)a, W-17.1(±4.3)b; and for AM: PA-14. 9(±4.2)a, AC-17.1(±3.9) b. Conclusions: Acid etching, when combined with a moist dentine surface and the use of primer agitation, improves the bond strength of the SAS to dentine. Clinical Significance: According to the results of the present in vitro study, modification of the application protocols for the silorane-based adhesive system may improve its clinical performance. © 2012 Published by Elsevier Ltd.