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A new method for efficiently converting electron backscatter diffraction data obtained using serial sectioning by focused ion beam of a polycrystalline thin film into a computational, three-dimensional (3D) structure is presented. The reported data processing method results in a more accurate representation of the grain surfaces, reduced computer memory usage, and improved processing speed compared to traditional voxel methods. The grain structure of a polycrystalline absorption layer from a high-efficiency Cu(In,Ga)Se2 solar cell (19.5%) is reconstructed in 3D and the grain size and surface distribution is investigated. The grain size distribution is found to be best fitted by a log-normal distribution. We further find that the grain size is determined by the [Ga]/([Ga] + [In]) ratio in vertical direction, which was measured by glow discharge optical emission spectroscopy. Finally, the 3D model derived from the structural information is applied in optoelectronic simulations, revealing insights into the effects of grain boundary recombination on the open-circuit voltage of the solar cell. An accurate 3D structure like the one obtained with our method is a prerequisite for a detailed understanding of mechanical properties and for advanced optical and electronic simulations of polycrystalline thin films.
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To robustly assess the antibacterial mechanisms of nanotopographies, it is critical to analyze the bacteria-nanotopography adhesion interface. Here, we utilize focused ion beam milling combined with scanning electron microscopy to generate three-dimensional reconstructions of Staphylococcus aureus or Escherichia coli interacting with nanotopographies. For the first time, 3D morphometric analysis has been exploited to quantify the intrinsic contact area between each nanostructure and the bacterial envelope, providing an objective framework from which to derive the possible antibacterial mechanisms of synthetic nanotopographies. Surfaces with nanostructure densities between 36 and 58 per µm2 and tip diameters between 27 and 50 nm mediated envelope deformation and penetration, while surfaces with higher nanostructure densities (137 per µm2) induced envelope penetration and mechanical rupture, leading to marked reductions in cell volume due to cytosolic leakage. On nanotopographies with densities of 8 per µm2 and tip diameters greater than 100 nm, bacteria predominantly adhered between nanostructures, resulting in cell impedance.
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Here we describe the first automated fully integrated in-microscope broad ion beam (BIB) system. Ar+-BIB has several advantages over Ga+ focused ion beam (FIB) and Xe+ plasma-FIB (PFIB) methods inducing less beam damage, especially for ion beam sensitive materials. It can mill areas several orders of magnitude larger (up to millimetre scale), and is not confined to the edge of the sample with associated curtaining issues. BIB is shown to have sputter rates up to five times higher than comparable FIB techniques. This new coupled BIB-SEM system (commercial name 'iPrep™II') enables in-microscope surface polishing to remove contaminants or damage for two dimensional (2D) imaging, as well as automated serial section tomography (SST) by milling and imaging hundreds of slices, cost and time efficiently. The milled slice thickness can be controlled from a few nanometers up to a micrometre. A novel sample transfer, handling and interlock system allows automated and sequential BIB polishing, scanning electron microscopy (SEM) and analysis by secondary electron (SE) imaging, electron back scatter diffraction (EBSD) and energy dispersive spectroscopy (EDS) for 3D microstructure analysis. Furthermore, insulating surfaces can be sputter coated after milling each slice to reduce charging during SEM analysis. The performance of the instrument is demonstrated through a series of case studies across the materials, earth and life sciences exploiting the imaging, crystallographic and chemical mapping capabilities. These include the study of butterfly defects in bearing steels, meta-stable intermetallic phases in bronze bearings, shale gas rock, aluminium plasma electrolytic oxide (PEO) coatings as well as liver and mouse brain tissues.
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Automatización/métodos , Angiografía por Tomografía Computarizada/métodos , Imagenología Tridimensional/métodos , Iones/química , Animales , Encéfalo/citología , Encéfalo/ultraestructura , Técnicas Histológicas/métodos , Procesamiento de Imagen Asistido por Computador/métodos , Hígado/citología , Hígado/ultraestructura , Ciencia de los Materiales/métodos , Ratones , Microscopía Electrónica de Rastreo/métodos , Microtomía/métodosRESUMEN
Nanostructuring is recognized as an efficient route for enhancing thermoelectric response. Here, we report a new synthesis strategy for nanostructuring oxide ceramics and demonstrate its effectiveness on an important n-type thermoelectric SrTiO3. Ceramics of Sr0.9La0.1TiO3 with additions of B2O3 were synthesized by the mixed oxide route. Samples were sintered in air followed by annealing in a reducing atmosphere. Crystallographic data from X-ray and electron diffraction showed Pm3Ì m cubic symmetry for all the samples. High-resolution transmission electron microscopy (HRTEM) showed the formation of a core-shell type structure within the grains for the annealed ceramics. The cores contain nanosize features comprising pairs of nanosize voids and particles; the feature sizes depend on annealing time. Atomic-resolution, high-angle annular-dark-field imaging and electron energy loss spectroscopy in the scanning transmission electron microscopy (STEM-HAADF-EELS) showed the particles to be rich in Ti and the areas around the voids to contain high concentrations of Ti3+. Additionally, dislocations were observed, with significantly higher densities in the shell areas. The observed dislocations are combined (100) and (110) edge dislocations. The major impact of the core-shell type microstructures, with nanosize inclusions, is the reduction of the thermal conductivity. Sr0.9La0.1TiO3 ceramics containing grain boundary shells of size ≈ 1 µm and inclusions in the core of 60-80 nm exhibit a peak power factor of 1600 µW/m·K2 at 540 K; at 1000 K, they exhibit a low thermal conductivity (2.75 W/m·K) and a power factor of 1050 µW/m·K2 leading to a high of ZT of 0.39 ± 0.03. This is the highest ZT reported so far for Sr0.9La0.1TiO3 based-compositions. This nanostructuring strategy should be readily applicable to other functional oxides.
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This study examined the tribological performance of three gear oils (Oils A, B and C), in relation to surface and microstructural changes. Oil A contains molybdenum dithiophosphate friction modifier, Oil B contains amine molybdate combined with zinc dialkyl dithiophosphate antiwear additive, while Oil C contains phosphonate and a commercial gear oil package. Following sliding tests of a hardened AISI 52100 steel ball on a spheroidized AISI 52100 steel disc, the worn surfaces were chemically studied using Raman and energy-dispersive X-ray spectroscopy. The tribological performance for each oil was different, likewise the nature of the tribofilm formed. After a 5 min sliding test, the hardness-depth profile of the worn surfaces was measured; also the cross-sectional microstructure was examined using scanning electron microscopy combined with focused ion beam preparation and transmission electron backscattered diffraction (t-EBSD) techniques. With Oil A, there was a relatively small increase in surface hardness (33% greater than that of the unworn surface), whereas with Oils B and C, the average hardness near the surface was 100% greater than that of the unworn surface. The cross-sectional microstructure using Oil A also differed from Oils B and C, which were quite similar. The result shows that with Oil A refinement of the ferrite grains spreads deeper into the material (> 10 µm), whilst with Oils B and C it was largely limited to 2-3 µm below the surface. It is concluded that the lubricant formulations and their associated tribofilms influenced the extent of deformation in the subsurface layers and consequently influenced the wear performance.
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The authors of the present work propose a color coding technique using quaternions for the display of crystallographic orientation data such as EBSD maps. The main difference to existing color coding techniques in this field is that it creates a color space, within which the perceived color differences are approximately proportional to Euclidean distances in the corresponding 3D quaternion vector space, and thus approximately proportional to mutual disorientation angles. Since all disorientation parameters (axis and angle pairs, but represented as quaternions) are taken into account, color ambiguities appearing in maps created by other techniques are successfully avoided, and the sub-grain orientation differences within grains can be unambiguously visualized.
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Plasmon-induced phenomena have recently attracted considerable attention. At the same time, relatively little research has been conducted on electrochemistry mediated by plasmon excitations. Here we report plasmon-induced formation of nanoscale quantized conductance filaments within metal-insulator-metal heterostructures. Plasmon-enhanced electromagnetic fields in an array of gold nanodots provide a straightforward means of forming conductive CrOx bridges across a thin native chromium oxide barrier between the nanodots and an underlying metallic Cr layer. The existence of these nanoscale conducting filaments is verified by transmission electron microscopy and contact resistance measurements. Their conductance was interrogated optically, revealing quantised relative transmission of light through the heterostructures across a wavelength range of 1-12 µm. Such plasmon-induced electrochemical processes open up new possibilities for the development of scalable devices governed by light.
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INTRODUCTION: The present study was conducted to assess the morphology of mandibular canines using cone-beam computed tomography (CBCT) in a north Iranian population. METHODS AND MATERIALS: For the morphological assessment of mandibular canines, 150 CBCT images taken from patients for different reasons were used. The mandibular canines were examined in sagittal, coronal and axial dimensions. The canal pattern, number of roots/canals, the tooth length, the orientation of the roots and the position of the apical foramina were evaluated and the effect of gender on each variable was assessed. The obtained data were analyzed using the Chi-square and student's t-tests. RESULTS: According to the Vertucci's criteria, the most common pattern was type I morphology (89.7%), followed by types III (5.7%), II (3.7%) and V (1%). No significant differences were observed between the male and female patients in terms of canal type (P>0.05). Gender difference is a factor which affected the root length and the number of mandibular canine root and root canal. There were 296 single-root and four double-root canines. The double-root canines and mandibular canine with two canals were significantly more common among men than women (P=0.00). The apical foramen was laterally positioned in 68.3% and centrally in 31.7% of the cases, and the root curvatures were mostly oriented toward the buccal region. No significant statistical difference was observed for mentioned parameters in right and left half of the jaw. CONCLUSION: Due the diverse morphology and the potential presence of a second mandibular canine among Iranians, dentists should perform endodontic treatments with greater care. CBCT is an accurate tool for the morphological assessment of root canals.
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Perovskite solar cells continue to attract strong attention because of their unprecedented rate of power conversion efficiency increase. CH3NH3PbI3 (MAPbI3) is the most widely studied perovskite. Typically one-step (1-s) or two-step (2-s) deposition methods are used to prepare MAPbI3 films. Here, we investigate a new MAPbI3 film formation method that combines 1-s and 2-s deposition (termed 1 & 2-s) and uses systematic variation of the stoichiometric mole ratio (x) for the PbI2 + xMAI solutions employed. The PbI2 + xMAI solutions were used to deposit precursor films that were subsequently dipped in MAI solution as a second step to produce the final MAPbI3 films. The morphologies of the 1 & 2-s MAPbI3 films consisted of three crystal types: tree-like microcrystals (â«1 µm), cuboid meso-crystals (â¼0.1-1 µm) and nanocrystals (â¼50-80 nm). Each crystal type and their proportions were controlled by the value for x. The new 1 & 2-s deposition method produced MAPbI3 films with tuneable optoelectronic properties that were related to those for the conventional 1-s and 2-s films. However, the 1 & 2-s film properties were not simply a combination of those for the 1-s and 2-s films. The 1 & 2-s films showed enhanced light scattering and the photoluminescence spectra displayed a morphologically-dependent red-shift. The unique morphologies for the 1 & 2-s films also strongly influenced PbI2 conversion, power conversion efficiency, hysteresis and recombination. The trends for the performance parameters and hysteresis were compared for devices constructed using spiro-MeOTAD and P3HT and were similar. The 1 & 2-s method should apply to other perovskite formulations and the new insights concerning MAPbI3 crystal growth conditions, morphology and material properties established in this study should also be transferable.
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Transmission Kikuchi diffraction (TKD), also known as transmission-electron backscatter diffraction (t-EBSD) is a novel method for orientation mapping of electron transparent transmission electron microscopy specimen in the scanning electron microscope and has been utilized for stress corrosion cracking characterization of type 316 stainless steels. The main advantage of TKD is a significantly higher spatial resolution compared to the conventional EBSD due to the smaller interaction volume of the incident beam with the specimen. Two 316 stainless steel specimen, tested for stress corrosion cracking in hydrogenated and oxygenated pressurized water reactor chemistry, were characterized via TKD. The results include inverse pole figure (IPFZ) maps, image quality maps and misorientation maps, all acquired in very short time (<60 min) and with remarkable spatial resolution (up to 5 nm step size possible). They have been used in order to determine the location of the open crack with respect to the grain boundary, deformation bands, twinning and slip. Furthermore, TKD has been used to measure the grain boundary misorientation and establish a gauge for quantifying plastic deformation at the crack tip and other regions in the surrounding matrix. Both grain boundary migration and slip transfer have been detected as well.
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Here we report a methodology combining TEM, STEM, Transmission-EBSD and EELS to analyse the structural and chemical properties of the metal-oxide interface of corroded Zr alloys in unprecedented detail. TEM, STEM and diffraction results revealed the complexity of the distribution of suboxide grains at the metal-oxide interface. EELS provided accurate quantitative analysis of the oxygen concentration across the interface, identifying the existence of local regions of stoichiometric ZrO and Zr3O2 with varying thickness. Transmission-EBSD confirmed that the suboxide grains can be indexed with the hexagonal ZrO structure predicted with ab initio by Nicholls et al. (2014). The t-EBSD analysis has also allowed for the mapping of a relatively large region of the metal-oxide interface, revealing the location and size distribution of the suboxide grains.
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The celebrated electronic properties of graphene have opened the way for materials just one atom thick to be used in the post-silicon electronic era. An important milestone was the creation of heterostructures based on graphene and other two-dimensional crystals, which can be assembled into three-dimensional stacks with atomic layer precision. Such layered structures have already demonstrated a range of fascinating physical phenomena, and have also been used in demonstrating a prototype field-effect tunnelling transistor, which is regarded to be a candidate for post-CMOS (complementary metal-oxide semiconductor) technology. The range of possible materials that could be incorporated into such stacks is very large. Indeed, there are many other materials with layers linked by weak van der Waals forces that can be exfoliated and combined together to create novel highly tailored heterostructures. Here, we describe a new generation of field-effect vertical tunnelling transistors where two-dimensional tungsten disulphide serves as an atomically thin barrier between two layers of either mechanically exfoliated or chemical vapour deposition-grown graphene. The combination of tunnelling (under the barrier) and thermionic (over the barrier) transport allows for unprecedented current modulation exceeding 1 × 10(6) at room temperature and very high ON current. These devices can also operate on transparent and flexible substrates.