Evaluation of microleakage in class v cavities prepared by different caries removal methods

The purpose of this study was to comparatively evaluate the effects of different caries removal methods on microleakage success of class V adhesive restorations by means of light microscopy (stereomicroscope) and scanning electron microscopy (SEM) observations. Sixty‐four human teeth with class V caries that measured with DIAGNOdent were used. The samples were divided into four groups (n = 16) randomly according to caries removing methods of conventional method, Carisolv, Papacarie, and Er,Cr:YSGG laser system. The self‐etch Clearf?l SE Bond and Clearf?l Majesty Es‐II were used as restoration materials. After thermal cycles of 2,000 (5 and 55°C) samples were immersed in a 50% wt/wt AgNO_3. Samples were finally imaged and scored under light microscopy and SEM, respectively. The data were statistically analyzed using Kruskal–Wallis H, pairwise comparison and Wilcoxon's T tests at 5% significance level (p < .05). Statistical analysis demonstrated that there was no significant difference between microleakage scores in dentin regions but there were significant difference between the Papacarie and Er,Cr:YSGGlaser in terms of leakage scores in enamel sites. No statistically significant difference in leakage scores emerged between light microscopy and SEM.     

Oral tissue response to ovine grafting biomaterial: Morphological and morphometric study using scanning electron and light microscopy tissue response to ovine grafting biomaterial

OBJECTIVE: To evaluate the oral tissue response to an experimental particle ovine biomaterial by scanning electron microscopy (SEM) and light microscopy (LM). MATERIAL AND METHODS: Forty‐eight rats had surgical periodontal defects treated with either blood clotting (control), bovine biomaterial? (B), or an experimental ovine biomaterial (O). Data from SEM analysis (defect exposure, root surface exposure, diameter of matrix fibers and bundles, and globuli areas; n = 5) were applied to Shapiro–Wilk, Kruskal–Wallis, and Dunn's test, whereas LM analysis (tissue cicatrization characteristics and diameter defect; n = 3) had data applied to two‐way analysis of variance. Animals were monitored for 1 and 3 weeks. RESULTS: By SEM, the O samples showed significant differences from B and C in the area of defect exposure (H_2,15 = 8.66; P < 0.05). In both periods, O and B samples showed similar results for matrix fiber diameters, differently than C samples (H_2,15 = 14.0; P < 0.05). All other SEM variables were considered equivalent among the groups (P > 0.05). Under LM, an acute and chronic granulomatous inflammation was seen in the presence of both biomaterials (B and O, 1 week); both the control and the ovine grafting samples showed mature bone in the repair site (3 weeks); the defect diameter showed similar values among groups, at both monitoring periods (F_2,12 = 1.0401; P > 0.05). CONCLUSION: The ovine particles of this study showed a favorable response to oral tissue repair, demonstrating to be a potential source for the development of bone grafting biomaterials. Microsc. Res. Tech. 2012. © 2012 Wiley Periodicals, Inc.     

Contrast in the transmission mode of a low-voltage scanning electron microscope

The contrast thicknesses (x_k) of thin carbon and platinum films have been measured in the transmission mode of a low-voltage scanning electron microscope for apertures of 40 and 100 mrad and electron energies (E) between 1 and 30 keV. The measured values overlap with those previously measured for E (≥ 17keV) in a transmission electron microscope. Differences in the decrease of x_k with decreasing E between carbon and platinum agree with Wentzel-Kramer-Brillouin calculations of the elastic cross-sections. Knowing the value of x_k allows the exponential decrease ∝ exp(—x/x_k) in transmission with increasing mass-thickness (x = ρt) of the specimen and the increasing gain of contrast for stained biological sections with decreasing electron energy to be calculated for brightfield and darkfield modes.     

Control of charging in low-voltage SEM

Charging of the specimen under electron beam irradiation is a common problem in scanning electron microscopy (SEM). It results in unstable imaging conditions and a loss in resolution due to defocus of the beam. In addition, it can cause permanent changes in some specimens from translocation of mobile ions under the influence of the induced electrostatic field. To minimize charging and its associated problems, the incident beam energy must be carefully chosen to be the value E₂ at which a dynamic charge balance is obtained. This article presents data on E₂ values for a variety of materials and demonstrates how E₂ is affected by the choice of angle of beam incidence.     

Stress and strain distribution in demineralized enamel: A micro‐CT based finite element study

Physiological oral mechanical forces may play a role on the progression of enamel carious lesions to cavitation. Thus, the aim of this study was to describe, by 3D finite element analysis, stress, and strain patterns in sound and carious enamel after a simulated occlusal load. Micro‐CT based models were created and meshed with tetrahedral elements (based on an extracted third molar), namely: a sound (ST) and a carious tooth (CT). For the CT, enamel material properties were assigned according to the micro‐CT gray values. Below the threshold corresponding to the enamel lesion (2.5 g/cm³) lower and isotropic elastic modulus was assigned (E = 18 GPa against E₁ = 80 GPa, E₂ = E₃ = 20 GPa for sound enamel). Both models were imported into a FE solver where boundary conditions were assigned and a pressure load (500 MPa) was applied at the occlusal surface. A linear static analysis was performed, considering anisotropy in sound enamel. ST showed a more efficient transfer of maximum principal stress from enamel to the dentin layer, while for the CT, enamel layer was subjected to higher and concentrated loads. Maximum principal strain distributions were seen at the carious enamel surface, especially at the central fossa, correlating to the enamel cavity seen at the original micro‐CT model. It is possible to conclude that demineralized enamel compromises appropriate stress transfer from enamel to dentin, contributing to the odds of fracture and cavitation. Enamel fracture over a dentin lesion may happen as one of the normal pathways to caries progression and may act as a confounding factor during clinical diagnostic decisions. Microsc. Res. Tech. 78:865–872, 2015. © 2015 Wiley Periodicals, Inc.     

Effect of super short pulse Er:YAG laser on human dentin—Scanning electron microscopy analysis

This study evaluated the effect of different pulse widths in the morphological characteristics of human dentin irradiated with Er:YAG in cavity preparation protocols and dentin pretreatment. Dentin discs with 2 mm thickness were obtained from 18 human molars. The experimental groups were composed from two variables: (1) clinical protocol—cavity preparation (E = 200 mJ/20 Hz)—and pretreatment (E = 80 mJ/2 Hz); and (2) pulse duration—50, 300, and 600 μs. This formed six experimental groups (n = 3): G1 (E = 200 mJ/20 Hz/50 μs); G2 (E = 200 mJ/20 Hz/300 μs); G3 (E = 200 mJ/20 Hz/600 μs); G4 (E = 80 mJ/2 Hz/50 μs); G5 (E = 80 mJ/2 Hz/300 μs); G6 (E = 80 mJ/2 Hz/600 μs). The samples were irradiated with the Er:YAG laser by noncontact mode at a focal distance of 7 mm from the target point under continuous water spray (60% water and 40% air). After the irradiation, they were processed for scanning electron microscopy (SEM). Morphological analysis showed an irregular dentin surface, absence of smear layer with opening of the exposure of dentinal tubules and protruding peritubular dentin—without indications of changes for all protocols used. Regardless of the analyzed experimental group, the dentin surface showed a microretentive morphology characteristic of ablation. The G1 and G4 showed a rougher surface when compared to other groups. Finally, we concluded that the pulse width can influence the morphological characteristics of the irradiated dentin tested in different clinical indications. The larger surface irregularity caused by regulation with less pulse width (50 µs) seems more appropriate to get a microretentive pattern necessary for successful adhesives restoration procedures. Microsc. Res. Tech. 78:472–478, 2015. © 2015 Wiley Periodicals, Inc.     

Evaluation of the effective cross‐sections for recombination and trapping in the case of pure spinel

In this paper, we have investigated the evolution of the secondary electron emission in the case of pure spinel during electron irradiation, achieved in a scanning electron microscope at room temperature, which is derived from the measurement of the induced and the secondary electron currents. It was observed from the experimental results, that there are two regimes during the charging process: a plateau followed by a linear variation, which are better identified by plotting the logarithm of the secondary electron emission yield lnσ as function of the total surface density of trapped charges in the material Q_T. For positive charging, E₀ = 1.1 and 5 keV, the slope of the linear part, whose value is of about 10^?10 cm² charge^?1, is independent of the primary electron energy. It is interpreted as a microscopic cross section for electron–hole recombination. For negative charging of pure spinel, E₀ = 15 and 30 keV, the slope is associated with an electron trapping cross section close to 10^?14 cm² charge^?1, which can be assigned to the microscopic cross section for electron trapping. This trapping cross section is four orders of magnitude lower than the recombination one.     

Papain‐gel degrades intact nonmineralized type I collagen fibrils

Papain‐gel has been utilized as a chemo‐mechanical material for caries removal due to its ability to preserve underlying sound dentin. However, little is known about the effect of the papain enzyme on intact type I collagen fibrils that compose the dentin matrix. Here we sought to define structural changes that occur in intact type I collagen fibrils after an enzymatic treatment with a papain‐gel. Intact and nonmineralized type I collagen fibrils from rat tail were obtained and treated with a papain‐gel (Papacarie) for 30 s, rinsed with water and imaged using an atomic force microscope (AFM). Additionally, polished healthy dentin specimens were also treated using the same protocol described above and had their elastic modulus (E) and hardness (H) measured by means of AFM‐based nanoindentation. AFM images showed that the papain‐gel induced partial degradation of the fibrils surface, yet no rupture of fibrils was noticed. The distinction between gap and overlap zones of fibrils vanished in most regions after treatment, and overlap zones appeared to be generally more affected. Mechanical data suggested a gradual decrease in E and H after treatments. A significant two‐fold drop from the values of normal dentin (E=20±1.9, H=0.8±0.08 GPa) was found after four applications (E=9.7±3.2, H=0.24±0.1 GPa) (P<0.001), which may be attributed to the degradation of proteoglycans of the matrix. In summary, this study provided novel evidence that intact nonmineralized type I collagen fibrils are partially degraded by a papain‐gel. SCANNING 31: 253–258, 2009. © 2010 Wiley Periodicals, Inc.     

Recent developments and new strategies in scanning electron microscopy*

In addition to improvements in lateral resolution in scanning electron microscopy, recent developments of interest here concern extension of the incident beam energy, E₀, over two decades, from ≈ 20 keV to ≈ 0.1–0.5 keV and the possibility of changing the take-off emission, α, of detected secondary electrons. These two degrees of freedom for image acquisition permit a series of images of the same field of view of a specimen to be obtained, each image of the series differing from the others in some aspect. The origins of these differences are explored in detail and they are tentatively interpreted in terms of the change in the secondary electron emission yield δ vs. E₀, δ = f(E₀), and also of the change in δ vs. α, ∂δ/∂α. Various origins for the chemical contrast and topographic contrast have been identified. Illustrated by correlating a secondary electron image and a backscattered electron image, use of the scatter diagram technique facilitates image comparison. The difference between the lateral resolution and the size of the minimum detectable detail is outlined to avoid possible errors in nanometrology. Some aspects related to charging are also considered and possible causes of contrast reversal are suggested. Finally, the suggested strategy consists of the acquisition of various images of a given specimen by changing one parameter: primary beam energy and take-off angle for conductive specimens; working distance or beam intensity for high-resolution experiments; scanning frequency for insulating specimens.     

Low‐temperature‐SEM study of dihedral angles in the ice‐I/sulfuric acid partially molten system

The transport and mechanical properties of partially molten materials are influenced by the wetting behaviour of the melt with respect to the crystalline solid. The equilibrium microstructure of an ice + melt system was examined using low‐temperature scanning electron microscopy. The samples were prepared by spraying a liquid solution of H₂O‐H₂SO₄ into liquid nitrogen and packing the frozen particulates into aluminium capsules. Samples were then sintered at –35 °C or –55 °C (above the eutectic temperature, T_E=–62 °C) for various durations and were quenched in liquid nitrogen to capture the equilibrium microstructure. This paper reports the first quantitative measurements of dihedral angle in this system. The measured median dihedral angle between the solid and vitrified melt is approximately 26 ± 2° at –35 °C and increases slightly as temperature decreases and approaches the solidus (32 ± 3° at –55 °C).     

Measurement of specimen charging in scanning electron microscopy with a kelvin probe

A vibrating Kelvin probe in form of a platinum wire loop is used to measure the surface potential U_s on electron-irradiated free-floating metal and insulator specimens as a function of electron energy E. This allows an accurate measurement of the critical electron energy E₂ for no charging. At energies below E₂, the positive charging increases with decreasing energy to U_s=2–5 eV at E=0.5 keV and switching off the collector bias of the Everhart-Thornley detector. A two-to threefold increase of U_s is observed when the bias is switched on. For E > E₂, the strong increase of a negative surface potential can be measured. Insulating films free-supported on a conductive substrate show a steep decrease to small positive and negative U_s when the film thickness becomes lower than the electron range at a critical energy E₃ > E₂. At insulating specimen the temporal decrease of charging can be measured when the electron beam is switched off.     

Substrate influence on cell shape and cell mechanics: HepG2 cells spread on positively charged surfaces

A human hepatoma cell line (HepG2) was cultured on positively and negatively charged polyelectrolytes. Cell/surface adhesion and cell shape evolution were followed with quartz microbalance with dissipation (QCM‐D) and optical microscopy as a function of time, respectively. In particular, substrates coated with poly(ethyleneimine) (PEI) led to fast cell attachment and further spreading, with average maximum frequency Δf = 79 Hz and dissipation ΔD = 40 × 10^?6. On the contrary, no cell spreading was observed on poly(sodium‐4‐styrenesulfonate) (PSS), with Δf = 33 Hz and ΔD = 4.5 × 10^?6. Atomic force microscopy (AFM) was used to investigate the influence of cell shape on its mechanical properties. Considering the cells as an homogenous solid material, the corresponding elastic modulus was estimated using the Hertz model. The elastic modulus was calculated at the central part of the cell, and the average values obtained were 191 ± 14 Pa and 941 ± 58 Pa for cells adsorbed on PSS and PEI, respectively. Thus, different cell–substrate interaction implied different cell mechanical properties reflected in a higher elastic modulus for stronger cell/substrate interaction. The combination of QCM‐D, AFM, and optical microscopy allowed the online study of the cell adhesion process, and the mechanical properties of the adhered cells. Microsc. Res. Tech. 2009. © 2009 Wiley‐Liss, Inc.     

An electron microscopy study of the phase Al3Fe

The phase Al₃Fe (monoclinic C2/m, a = 1·549 nm, b = 0·808 nm, c = 1·248 nm, β = 107·8°) has been studied by transmission electron microscopy (TEM) and high resolution electron microscopy (HREM). Crystals were obtained from a direct chill-cast ingot of an Al-0·25 wt% Fe-0·13 wt% Si alloy. Extracted crystals were prepared by dissolving the aluminium phase in butanol and filtering off the particles. The extracted Al₃Fe crystals were mainly (100) platelets. The monclinic lattice was confirmed by tilt experiments and the mirror plane was confirmed by convergent beam electron diffraction. Experimental HREM images from the [100] and [110] projection agreed with images calculated by the multislice method. The interpretation of images in terms of a projected crystal structure is discussed. Common defects in Al₃Fe crystals were: twins on (100) and faults on (001). The (001) faults could be described by a displacement 1/2·[100] on a fault plane at z = 0·5 in the unit cell. A model for (001) faults, based on multiple twinning, is proposed.     

Structure and biomechanics of culms of Phragmites australis used for reeds of Japanese wind instrument “hichiriki”

Hichiriki is a traditional Japanese double‐reed wind instrument used in Japanese ancient imperial court music, gagaku, which has been performed since the 7th century. The best reeds for hichiriki have been made of culms or stems of Phragmites australis (P. australis) that are harvested from only a limited reed bed at Udono near Kyoto. The aim of this study is to elucidate why the stems from Udono are the best materials for hichiriki reeds. Plant anatomy was examined for choice stems of P. australis grown in different reed beds in Japan as well as morphology, and the local indentation hardness and Young's modulus of tissues on the cross‐sections of some representatives of hichiriki reeds were measured. It is concluded that the good stems for hichiriki reeds have an outer diameter of about 11 mm, a wall thickness of about 1 mm and comparatively homogeneous structure where harder materials, such as epidermis, hypodermis, sclerenchymatous cells, and vascular bundle sheaths with hard walls, are orderly deployed with softer materials such as parenchyma cells and vascular bundles. This structure has smaller differences of hardness and Young's modulus between the hard and soft materials in the reed, providing the best music performance. Microsc. Res. Tech. 78:260–267, 2015. © 2015 Wiley Periodicals, Inc.     

Effects of prolonged use of over-the-counter bleaching agents on enamel: An in vitro study

This study evaluated the effects of four over-the-counter (OTC) bleaching products on the properties of enamel. Extracted human molars were randomly assigned into four groups (n = 5): PD: Poladay (SDI), WG: White Teeth Global (White Teeth Global), CW: Crest3DWhite (Procter & Gamble), and HS: HiSmile (HiSmile). The hydrogen peroxide (H₂O₂) content in each product was analyzed via titration. Twenty teeth were sectioned into quarters, embedded in epoxy resin, and polished. Each quarter-tooth surface was treated with one of the four beaching times: T0: control/no-bleaching, T14: 14 days, T28: 28 days, and T56: 56 days. Materials were applied to enamel surfaces as recommended. Enamel surfaces were examined for ultramicrohardness (UMH), elastic modulus (EM), superficial roughness (Sa), and scanning electron microscopy (SEM). Ten additional teeth were used to evaluate color and degree of demineralization (DD) (n = 5). Data were statistically tested by two-way ANOVA and Tukey's tests (α = 5%). Enamel surfaces treated with PD and WG presented UMH values significantly lower than the controls (p < .05). Elastic modulus (E) was significantly reduced at T14 and T28 for PD, and at T14 for HS (p < .05). A significant increase in Sa was observed for CW at T14 (p < .05). Color changes were observed in the PD and WG groups. Additionally, DD analysis showed significant demineralization at T56 for CW. Overall, more evident morphological alterations were observed for bleaching products with higher concentrations of H₂O₂ (p < .05), PD, and WG. Over-the-counter bleaching products containing H₂O₂ can significantly alter enamel properties, especially when application time is extended.     

Analysis of spatial vapor-phase distribution using the LIF method on multi-component fuel

We analyzed the vapor-phase distribution and behavior of each component in multi-component fuel (MCF). Evaporation characteristic of MCF was researched by laser-induced fluorescent (LIF) method. A pulsed Nd-YAG laser was used as incident light, and an experiment was performed in a constant-volume vessel so that optical measurement could be possible. MCF was injected through electronically controlled common rail injector into the vessel. I-octane (C₈H₁₈), n-dodecane (C₁₂H₂₆) and n-hexadecane (C₁₆H₃₄) were selected to be low boiling point (LO-B.P.), mid boiling point (MI-B.P.) and high boiling point (HI-B.P.) components, respectively, and Fuel A, Fuel B and Fuel C, made by compounding those components at different mass fractions, were used as MCF. Experimentation was performed under the conditions that injection pressures were 42MPa, 72MPa and 112MPa, respectively, ambient gas density was 15kg/m3 and ambient gas temperature was 700K. The spatial vapor-phase distribution, dispersion process of mixture, and vaporphase homogeneity were researched. It was ascertained that the vapor-phase of MCF showed stratified distribution and the dispersion of mixture was improved in proportion to the mass fraction of the LO-B.P. component.     

Nonradiative recombination at dislocations in III–V compound semiconductors

Carrier recombination at individual dislocations is investigated for the case of misfit dislocations at a heterojunction between Ga_1–xAl_xAs_1–yP_y epitaxial layers. Through the combined use of scanning transmission electron microscopy, electron beam induced current and cathodoluminescence analysis, it is shown that the non-radiative and radiative recombination properties of dislocations are associated with their fine crystallographic configuration. The edge Lomer-Cottrell dislocation is found to be electrically neutral. The absence of carrier recombination strongly suggests that core reconstruction may be important in eliminating dangling bonds and kink sites along the core of these dislocations. An undissociated dislocation with a Burgers vector b =1/2a〈110〉 is proposed as the more likely configuration for the edge Lomer-Cottrell dislocation. An asymmetry in the nonradiative recombination properties and crystallographic structure of the 60° dislocation is also reported and discussed.     

Study of two tungstates Ca0.5Cd0.5WO4 and Ca0.2Cd0.8WO4 by transmission electron microscopy

To better understand the role of crystal structures and local disorder in the photonic properties of the system (1 ? x)CaWO₄ ? xCdWO₄ with 0 < x < 1, two specific phases with compositions x = 0.5 (scheelite phase) and 0.8 (wolframite phase) have been studied by scanning and transmission electron microscopies. High‐resolution electron microscopy images and image simulations, associated with X‐ray diffraction data, allowed confirming the lattices and space groups I4₁/a and P2/c of the two scheelite and wolframite phases, at the local scale. The electron microscopy data show the existence of a high degree of crystallization associated with statistical distribution of Ca or Cd atoms on a Ca_1?xCd_x site in each lattice.     

An Electromagnetic Calorimeter with a Transversal Orientation of the Scintillating Fibers

The space and energy resolutions of the SPACAL electromagnetic calorimeter with a transverse orientation of the scintillating fibers have been measured. The main parameters of the calorimeter are presented. The results of experiments with an electron test beam of the DESY synchrotron at energies E = 1–6 GeV are discussed. The measured energy resolution of the calorimeter is found to be (/E) = 12.7%/E 2.0% (E is expressed in terms of GeV), and the space resolution is _{x, y} (E) = 1 mm at E = 4 GeV.     

Experimental characterization of biphasic materials using rate-controlled Hertzian indentation

This paper describes a new method, based on Hertzian biphasic theory (HBT), to characterize properties of biphasic materials with reduced time demands, increased surface sensitivity, and reduced computational demands compared to the current gold standards. Indentation experiments were conducted at a single location on a representative osteochondral plug to demonstrate and validate the HBT method against two gold standards, linear biphasic theory (LBT) and tension–compression nonlinear biphasic theory (TCN). The (1) aggregate moduli, (2) permeability and (3) tensile moduli from HBT, LBT, and TCN were (1) H_A=0.47, 0.47, and 0.40 MPa, (2) k=0.0026, 0.0014 and 0.0016 mm⁴/Ns, and (3) E_t=8.7, 0.46, and 10.3 MPa, respectively. The results support the HBT method and encourage its use, especially in light of its practical advantages.