Load dependence and lifetime studies of self‐assembled monolayers

A comparative study of the microtribological properties of native oxide on Si (100), Si (100) coated with octadecyltrichlorosilane (OTS) and perfluorode‐cyltrichlorosilane (FDTS) self‐assembling monolayers (SAMs) is presented. The frictional properties between these samples and a bare silicon sphere were examined using a microtribometer. Microfriction was investigated as a function of the normal load and relative humidity. Also, the microfriction of OTS‐ and FDTS‐coated surfaces was studied as a function of sliding time and normal load to examine the lifetime of these monolayers. Confirming the results of earlier studies, in the microtribological regime OTS and FDTS significantly reduce the friction force in comparison to the bare, native oxide covered (hydrophilic) silicon surface. The friction vs. normal load curve of oxide‐covered surfaces as well as the SAMs can be described by contact mechanics. Lifetime measurements of the SAMs, examined as a function of the normal load and relative humidity, indicate that the OTS monolayers wear quickly in both dry and moist environments, while the lifetime of FDTS monolayers appears to increase in moist environments. Copyright © 2006 John Wiley & Sons, Ltd.     

Multi‐walled carbon nanotubes decorated by platinum catalyst nanoparticles—Examination and microanalysis using scanning and transmission electron microscopies

Carbon nanotubes (CNTs) decorated with platinum (Pt) nanoparticles (NPs) have been characterized using a cold field‐emission scanning electron microscope (SEM) and a high resolution field‐emission transmission electron microscope (TEM). With this particular composite material, the complementary nature of the two instruments was demonstrated. Although the long CNTs were found to be mostly bent and defective in some parts, the nucleation of Pt occurred randomly and uniformly covered the CNTs. The NPs displayed a large variation in size, were sometimes defective with twins and stacking faults, and were found to be faceted with the presence of surface steps. The shape and size of the NPs and the presence of defects may have significant consequences on the activity of the Pt catalyst material. Also, thin layers of platinum oxide were identified on the surface of some NPs.     

Comparison of microtensile bond strength and resin–dentin interfaces of two self‐adhesive flowable composite resins by using different universal adhesives: Scanning electron microscope study

The aim of this in‐vitro study was to evaluate microtensile bond strength (μTBS) of two different self‐adhesive composites (SACs) on the permanent dentin by applying five different universal adhesive systems. In this study, two different SACs [Vertise Flow (VF), Fusio Liquid Dentin (FLD)] and five different bonding systems [Clearfil Universal Bond Quick (CUB), Single Bond Universal (SBU), All Bond Universal (ABU), Prime Bond Universal (PBU), Futurabond U (FBU)] were used. A total of 22 groups were created in which SACs were applied without adhesive and with five different universal bonding agents in total‐etch (TE) and self‐etch (SE) modes. Two hundred and forty test sticks were obtained using 48 healthy human molar teeth in total with groups having 10 samples each. The μTBS test was applied to each sample in the Universal test device and the data obtained were analyzed statistically by variance analysis and Tukey HSD test. In addition, the resin–dentin interface and fractures modes in the groups were examined by SEM. Upon examining the μTBS results, the highest values were seen in the use of SBU adhesive in TE mode in VF group, while the lowest values were seen in the FLD control group. The difference between the control and experimental groups was found statistically significant (p < .05). Upon comparing the control groups with each other, it was seen that VF group had higher μTBS values than FLD group and the difference between the groups was found statistically significant (p < .05). The μTBS results and SEM images of the study showed that the use of SACs with universal adhesive systems provides a more effective bond strength.     

Effect of laser preparation on adhesion of a self‐adhesive flowable composite resin to primary teeth

The aim of the study was to evaluate the adhesion of a self‐adhering flowable composite resin to primary tooth enamel and dentin after silicon carbide paper (SiC) and laser pretreatment. Adhesive properties were evaluated as shear bond strength (SBS) and scanning electron microscopic (SEM) characteristics. A total 120 primary canine teeth were randomly divided into two groups to study enamel and dentin. Each group was divided into 6 subgroups (n = 10) according to type of surface preparation (SiC or Er:YAG laser) of enamel or dentin. Three methods were used to build cylinders of restoration on tooth surface: OptiBond All‐In‐One + Premise Flowable composite, OptiBond All‐In‐One + Vertise Flow and Vertise flow. After restoration, samples were tested for SBS and failure mode. Twenty eight samples were examined by SEM. The results of the study showed SBS of Vertise Flow was lower than others in enamel and dentin samples pretreated with SiC and in dentin samples pretreated with laser (P < 0.001). Compared to SiC pretreatment, laser pretreatment led to a significantly higher SBS with Vertise Flow on enamel (P < 0.001). Vertise Flow associated with the adhesive led to a higher SBS in enamel and dentin compared to Vertise Flow alone. Adhesive and mixed failure modes were observed more frequently in Vertise Flow groups. SEM images showed that Vertise Flow led to more irregularities on enamel and more open dentinal tubules after laser ablation compared SiC pretreatment. Microsc. Res. Tech. 79:334–341, 2016. © 2016 Wiley Periodicals, Inc.     

Efficacy of ethylene‐diamine‐tetra‐acetic acid associated with chlorhexidine on intracanal medication removal: A scanning electron microscopy study

The aim of this study was to evaluate the effectiveness of 17% ethylene‐diamine‐tetra‐acetic acid (EDTA) used alone or associated with 2% chlorhexidine gel (CHX) on intracanal medications (ICM) removal. Sixty single‐rooted human teeth with fully formed apex were selected. The cervical and middle thirds of each canal were prepared with Gates Glidden drills and rotary files. The apical third was shaped with hand files. The specimens were randomly divided into two groups depending on the ICM used after instrumentation: calcium hydroxide Ca(OH)₂+CHX or Ca(OH)₂+sterile saline (SS). After seven days, each group was divided into subgroups according to the protocol used for ICM removal: instrumentation and irrigation either with EDTA, CHX+EDTA, or SS (control groups). All specimens were sectioned and processed for observation of the apical thirds by using scanning electron microscopy. Two calibrated evaluators attributed scores to each specimen. The differences between the protocols for ICM removal were analyzed with Kruskal‐Wallis and Mann‐Whitney U tests. Friedman and Wilcoxon signed rank tests were used for comparison between the score of debris obtained in each root canal third. Remains of Ca(OH)₂ were found in all specimens independently of the protocol and ICM used (P > 0.05). Seventeen percent EDTA showed the best results in removing ICM when used alone (P < 0.05), particularly in those associated with CHX. It was concluded that the chelating agent 17% EDTA significantly improved the removal of ICM when used alone. Furthermore, the type of the vehicle associated with Ca(OH)₂ also plays a role in the ICM removal. Microsc. Res. Tech. 77:735–739, 2014. © 2014 Wiley Periodicals, Inc.     

A comparative study on the self‐assembly of an amyloid‐like peptide at water–solid interfaces and in bulk solutions

In the past years the self‐assembly of amyloid‐like peptides has attracted increasing attentions, because it is highly related to neurodegenerative diseases and has a potential for serving as nanomaterial to fabricate novel and useful nanostructures. In this paper, we focused on the role of interfacial conditions in the self‐assembly of an amyloid‐like peptide, termed Pep11. It was found that, when dissolved in bulk solutions, Pep11 formed into β‐sheet structures and assembled into long filaments in several hours, as revealed by Thioflavin T fluorescence and transmission electron microscopy (TEM) morphology characterization, respectively. When the peptide solution was added onto a mica/HOPG substrate, peptide filaments with three preferred orientations with an angle of 60° to each other were formed immediately, as imaged in situ by atomic force microscopy (AFM). However, the kinetics in filament formation and the morphologies of the formed beta sheet either on HOPG and mica or in bulk solutions were quite different. These results indicate that the interfacial properties dramatically affect the peptide self‐assembly process. Microsc. Res. Tech. 78:375–381, 2015. © 2015 Wiley Periodicals, Inc.     

Modelling and experimental investigations of thin filmsof Mg phosphorus‐doped tungsten bronzes obtainedby ultrasonic spray pyrolysis

In this study, the synthesis of thin films of Mg phosphorus doped tungsten bronzes (MgPTB; MgHPW₁₂O₄₀·29H₂O) by the self‐assembly of nano‐structured particles of MgPTB obtained using the ultrasonic spray pyrolysis method was investigated. As the precursor, MgPTB, prepared by the ionic exchange method, was used. Nano‐structured particles of MgPTB were obtained using the ultrasonic spray pyrolysis method. The nano‐structure of the particles used as the building blocks in the MgPTB thin film were investigated experimentally and theoretically, applying the model given in this article. The obtained data for the mean particle size and their size distribution show a high degree of agreement. These previously tailored particles used for the preparation of thin films during the next synthesis step, by their self‐assembly over slow deposition on a silica glass substrate, show how it is possible to create thin MgPTB films under advance projected conditions of the applied physical fields with a fully determined nanostructure of their building block particles, with a relatively small roughness and unique physical properties.     

Platelet‐rich fibrin and collagen membrane in the preservation of the alveolar bone: Feasibility of the elemental inorganic composition and scanning electron microscopy analysis

The success of dental implants is related to the amount, quality, and composition of the alveolar bone. The placement of platelet‐rich fibrin (PRF) clot associated with a resorbable collagen membrane (RCM) in a postextraction alveolus is a technique used for ridge preservation. This case report study analyzed the ultrastructural characteristics of cross‐sectioned alveolar bone that received PRF and RCM using scanning electron microscopy and the inorganic composition using “energy dispersive X‐ray spectrometry,” in order to explore the feasibility of this method to clinical studies. Three alveolar bone samples from two male patients (37 and 58 years old), obtained in the procedure of placing the dental implant, were analyzed. Two bone samples previously received PRF and RCM (M37 and M58), the third sample represented a physiological bone formation without treatment (M37‐control). The bone sample M37 showed irregularly shaped islets of calcified material intermingled with connective tissue. The other samples, from the 58‐year‐old patient with PRF and RCM (M58); and the other untreated bone sample from the same 37‐year‐old patient (M37‐control) showed similar ultrastructural morphology with trabecular conformation without islets agglomerations. The inorganic composition analysis showed higher concentrations of calcium and phosphorus in both samples treated with PRF and RCM in comparison to the untreated bone sample. The Ca/P ratio was higher in the M37 sample compared to the others samples. The results showed morphology and inorganic composition differences among the treatments used, suggesting that this method is feasible to analyze parameters of the alveolar bone tissue.     

The effects of osmium tetroxide post‐fixation and drying steps on leafy liverwort ultrastructure study by scanning electron microscopy

Leafy liverwort is one of the most abundant and diverse plants in Indonesia. Their high variation and beneficial secondary metabolites contained in the oil bodies have attracted researchers' attention. The ultrastructural analysis of leafy liverworts is important as a means of species identification and also for further exploration of their oil bodies. However, the optimization of the preparation steps for observing leafy liverworts by SEM is necessary to avoid sample destruction. Fixation and drying play important roles in maintaining a sample's structure as close to its natural state as possible. Thus, in this study, we evaluated the effect of 4% Osmium tetroxide (OsO₄) and drying on leafy liverworts ultrastructure. Microlejeunea, Acrolejeunea, and Frullania were fixed with 2.5% glutaraldehyde. Some samples were then post‐fixed with 4% OsO₄, while the rest were directly dehydrated with an ethanol series and then subjected to different drying methods, i.e. air drying, freeze drying, and drying with hexamethyldisilazane (HMDS). According to the data obtained, post‐fixation with 4% OsO₄ could better maintain the integrity of the samples and enhance the contrast of leafy liverwort SEM images. In addition, samples dried with HMDS showed more detailed structures compared to those that were air dried. Different ultrastructure were found among the different leafy liverworts observed by SEM. Our data suggested the advantages of SEM in providing ultrastructure information on leafy liverworts as well as the optimum conditions to observe them with less deformation. OsO₄ post‐fixation could enhance the contrast of leafy liverwort SEM images and maintain the structure of the samples. Drying with HMDS provided a convenient way for rapid SEM preparation with less structural distortion.     

Localized grounding, excavation, and dissection using in-situ probe techniques for focused ion beam and scanning electron microscopy: experiments with rock varnish

While investigating rock varnish, we explored novel uses for an in‐situ micromanipulator, including charge collection, sample manipulation, as well as digging and dissection at the micron level. Dual‐beam focused ion beam microscopes (DB‐FIB or FIBSEM) equipped with micromanipulators have proven to be valuable tools for material science, semiconductor research, and product failure analysis. Researchers in many other disciplines utilize the DB‐FIB and micromanipulator for site‐specific transmission electron microscope (TEM) foil preparation. We have demonstrated additional applications for in‐situ micromanipulators. SCANNING 34: 279–283, 2012. © 2012 Wiley Periodicals, Inc.     

High‐temperature oxidation of nickel and chromium studied with an in‐situ environmental scanning electron microscope

Investigations of the morphology of metal oxide scales formed at high temperatures in oxidative environments are usually undertaken after exposure of the samples is completed. In this study, an environmental scanning electron microscope (ESEM) was used as a tool for the in‐situ observation of oxide scale formation. Pure nickel and chromium samples were oxidized at a temperature of 973 K in either pure oxygen or water vapour at a pressure of 667 Pa. The evolution of an oxide scale was followed in‐situ for up to 3 h. The morphology of the developing oxide scales was found to be a function of the metal substrate and the gaseous species. The growth mechanisms of the different metal oxide scales are reviewed and related to the analysed in‐situ images. Emphasis is placed on the relationship between oxidation mechanism and scale morphology. Nickel is seen to oxidise by outward diffusion of nickel probably on oxide grain boundaries when exposed to oxygen. Water vapour changes the scale morphology and a duplex‐type scale arises due to preferential overgrowth. The scale which develops due to chromium oxidation in oxygen is a fine‐grained, thin, and dense layer. In contrast, water vapour leads to whisker growth on chromium and an open, felt‐like structure forms. The applicability of the ESEM to the study of such systems is demonstrated, and its limitations are outlined. The results are encouraging examples of the possibilities which the in‐situ ESEM technique possesses.     

The role of spatial frequency analysis in correlating atomic force microscopy and optical profilometry with self‐etch adhesive enamel bond fatigue durability

The purpose of this study was to: (a) evaluate the role of enamel surface roughness on bond fatigue durability and (b) evaluate statistical differences in roughness values based on measurement technique, including the use of spatial filtering for optical profilometry (OP). OptiBond XTR (Kerr Corp), Prime & Bond elect (DENTSPLY Caulk), Scotchbond Universal (3 M Oral Care), and XTR pre‐etched with Ultra‐Etch phosphoric acid (35%) (Ultradent) self‐etch adhesives were used to treat enamel. A flat ground enamel surface was included as a control. Atomic force microscopy (AFM) and OP were used to measure the surface topography of each enamel surface following the application of adhesives. AFM, OP, and filtered OP (FOP) roughness values, where FOP was designed to only include the lateral spatial resolution consistent with AFM roughness values, were collected. Spatial resolution filtering with OriginPro was used to compare line scans from the two imaging techniques and generate the FOP group. These micro‐ versus nanoscale lateral roughness values were correlated with shear bond and shear fatigue strengths of the adhesives bonded to enamel. Roughness values showed differences based on measurement technique and strong correlations with bond and fatigue strength. The filtered OP group demonstrated the importance of careful usage and reporting of atomic force microscopy and OP metrics in adhesive dentistry. Best practices for surface roughness analysis were also discussed.     

Ultra‐thin resin embedding method for scanning electron microscopy of individual cells on high and low aspect ratio 3D nanostructures

The preparation of biological cells for either scanning or transmission electron microscopy requires a complex process of fixation, dehydration and drying. Critical point drying is commonly used for samples investigated with a scanning electron beam, whereas resin‐infiltration is typically used for transmission electron microscopy. Critical point drying may cause cracks at the cellular surface and a sponge‐like morphology of nondistinguishable intracellular compartments. Resin‐infiltrated biological samples result in a solid block of resin, which can be further processed by mechanical sectioning, however that does not allow a top view examination of small cell–cell and cell–surface contacts. Here, we propose a method for removing resin excess on biological samples before effective polymerization. In this way the cells result to be embedded in an ultra‐thin layer of epoxy resin. This novel method highlights in contrast to standard methods the imaging of individual cells not only on nanostructured planar surfaces but also on topologically challenging substrates with high aspect ratio three‐dimensional features by scanning electron microscopy.     

Comparison of total‐etch,self‐etch,and selective etching techniques on class V composite restorations prepared by Er:YAG laser and bur: a scanning electron microscopy study

The purpose of this study was to compare total‐etch, self‐etch, and selective etching techniques on the marginal microleakage of Class V composite restorations prepared by Er:YAG laser and bur. Class V cavities prepared on both buccal and lingual surfaces of 30 premolars by Er:YAG laser or bur and divided into six groups. The occlusal margins were in enamel, and the cervical margins were in cementum. Group‐1: bur preparation(bp)+Adper Single Bond 2 (ASB)+Filtek Z550 (FZ); Group‐2: laser preparation(lp)+(ASB)+(FZ); Group‐3: bp + Clearfil S3 Bond Plus (CSBP)+(FZ); Group‐4: lp+(CSBP) (FZ); Group‐5: bp + acid etching+(CSBP)+(FZ); Group‐6: lp + acid etching+(CSBP)+(FZ). All teeth were stored in distilled water at 37°C for 24 hr, and then thermocycled 1000 times (5–55°C). Five teeth from each group were chosen for the microleakage investigation, and two teeth for the scanning electron microscope evaluation. Teeth which were prepared for the microleakage test were immersed in .5% methylene blue dye for 24 hr. After immersion, the teeth were sectioned and observed under a stereomicroscope for dye penetration. Data were analyzed using Kruskal–Wallis and Mann–Whitney U tests (p < .05). More microleakage was observed in the cervical regions compared to the occlusal regions in Groups 3, 5, and 6, respectively (p < .05). There is no statistically significant difference in Groups 1, 2, and 4, in terms of cervical regions versus occlusal regions (p > .05). No significant differences were observed among any groups in terms of occlusal and cervical surfaces, separately (p > .05). Different etching techniques did not influence microleakage of Class V restorations prepared by Er:YAG laser and bur.     

Adverse effects of respiratory disease medicaments and tooth brushing on teeth: A scanning electron microscopy,X‐ray fluorescence and infrared spectroscopy study

The present study aims to evaluate the effect of brushing with fluoride dentifrice on teeth severely affected by erosion due to respiratory medicaments. Enamel (n = 50) and dentin (n = 50) bovine specimens were prepared and treated with artificial saliva (S‐control), acebrofilin hydrochloride (AC), ambroxol hydrochloride (AM), bromhexine hydrochloride (BR), and salbutamol sulfate (SS) and subjected to cycles of demineralization (immersing in 3 mL, 1 min, three times a day at intervals of 1 hr, for 5 days) followed by remineralization (saliva, 37°C, 1 hr). Simulated brushing with fluoridated toothpaste was performed using 810 strokes in a reciprocal‐action brushing simulator. Scanning electron microscopy, micro energy dispersive X‐ray fluorescence (μ‐EDXRF) spectroscopy and attenuated total reflection Fourier transform infrared (ATR FTIR) spectroscopy were then performed. μ‐EDXRF images showed extensive erosion after treatment with all medicaments. SEM images showed enamel erosion in order SS > BR > AC = AM > S after brushing and fluoridation. FTIR results were in agreement. In case of dentin, μ‐EDXRF measurements showed significant difference in mineral content (percent weight of calcium and phosphate) in SS + brushing + fluoridation treated enamel compared to control, while μ‐EDXRF images showed erosive effects in the order SS > AM>BR > AC = S post brushing + fluoridation. SEM images showed erosion in the order SS > AM = BR > AC > S post brushing + fluoridation. Again, FTIR multivariate results were in agreement. Overall, our study shows that proper oral care is critical when taking certain medication. The study also demonstrates the possible use of FTIR for rapid clinical monitoring of tooth erosion in clinics.