Structural observations and biomechanical measurements of clarinet reeds made from Arundo donax

Plant anatomy was examined for two clarinet reeds made out of Arundo donax by different means of microscopy: light microscopy, low‐energy secondary electron scanning electron microscopy (SEM), backscattered electron SEM, and helium ion microscopy (HiM). The local indentation hardness H_IT and Young's modulus E_IT of different tissues on their cross sections were measured. A vascular bundle (Vb) (H_IT = 60–100 MPa, E_IT = 1,500–2,000 MPa) that includes soft tissues of phloem and xylem and a vascular bundle sheath (Bs) (H_IT = 300–500 MPa, E_IT = ～7,000 MPa) form a pipe of the strong string along the longitudinal direction of the cane. This Vb/Bs string is connected transversally with a net of thin cell‐walls of parenchyma cells (Pa) (H_IT = 70–200 MPa, E_IT = 2,000–3,000 MPa) that also range along the longitudinal direction of the cane. It was turned out that the acoustic quality of a reed is mainly ascribed to the shape and configuration of Vb and the size of Pa. A reed where Vb bundles with continuous Bs rings are homogeneously distributed with higher proportion among a softer network of small Pa cells enables musical performance.     

High‐contrast optical microscopy of graphene sheets

In the way of making graphene an industry‐friendly material, it must be mass‐produced with high‐quality and reduced cost over large areas. Assisted by machine‐learning techniques, rapid, nondestructive and accurate determination of large graphene sheets on SiO₂/Si substrates has been made possible in recent years by the optical microscopy method. Optimization of the substrate to achieve the maximum contrast can further extend the application of the optical microscopy method for quality control of the mass‐produced graphene. Graphene/n₂/n₃three‐layer structures, where n₂ and n₃ are refractive indices, are routinely used for identifying the number of graphene layers by optical reflection microscopy. In this paper, two analytical equations are derived that can be easily used for high‐contrast optical imaging of graphene sheets without any need to resort to the cumbersome numerical methods. One of the equations is derived for choosing the best material with refractive index n₂ that when coated on a substrate with refractive index n₃, maximizes the optical contrast. The other equation is derived for finding the best thickness of the SiO₂ layer in graphene/SiO₂/Si structures, which are in common use for fabrication of graphene‐based devices. The results are implemented in a MATLAB GUI, see Supporting Information, to assist the users in using the equations.     

Microstructure, chemical and tribological investigations of Mo x W1−x S y co-sputtered composite films

Mo _x W_1−x S _y composite films were co-sputtered by the combination of MoS₂ and WS₂ targets, which were shown to have much superior tribological performance with lower and more stable friction coefficient, longer durability and higher bearing resistance than pure MoS₂ films in room temperature air with a relative humidity of 45–50%. Especially for the Mo_0.6W_0.4S_1.6 (40 at.% WS₂) composite film, an increase in durability of more than a one order of magnitude was reached. X-ray diffraction (XRD), scanning electron microscopy, transmission electron microscopy, and X-ray photoelectron spectroscopy were used to investigate the relationship between the microstructure and the tribological performance of the films. The composite films are shown to have a densified structure and accordingly improved oxidation resistance and lubrication properties. Moreover, the composite films have a lattice expansion in the c direction, along with a reduced the friction within the films.     

STM and AFM investigations of high-Tc superconductors

We have studied the (001) surface of single crystal YBa₂Cu₃O_7-x high-T_c superconductors using scanning tunnelling microscopy (STM) and atomic force microscopy (AFM) at room temperature at ambient pressure. Both methods show flat terraces with steps which are multiples of the c-axis lattice constant (of 1·17 nm) high. Our results show that the bulk crystal structure extends to the surface and that the crystals were formed by island growth. Only occasionally tunnelling was possible with sample bias voltages below +1·0 V. We interpret the observed voltage dependence and the difficulty to get good STM images to be due to the presence of a less-conducting surface layer. Auger spectroscopy indicates that carbon is present at the surface, which is probably related to a contamination layer.     

Vacuum Methods in Electron Microscopy. By Wilbur C. Bigelow

Microstructural evolution in two in situ reinforced composite systems, one produced by partial reduction and the other by grain growth, has been examined over a range of size scales using light microscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Metal-ceramic matrix composites were formed by the partial reduction of Al₂O₃–Cr₂O₃ solid solutions to form Cr metal particles in an Al₂O₃–Cr₂O₃ matrix which had a lower Cr₂O₃ concentration. In a second system, grain growth of Si₃N₄ during liquid phase sintering produced large, whisker-like grains in a fine-grained Si₃N₄ matrix, bonded by an oxynitride phase. The mechanisms controlling microstructural evolution in these two systems were examined.     

Comparative studies of perfluorinated lubricants adsorbed on hydrogenated amorphous carbon and amorphous carbon nitride

Temperature-programmed desorption and scanning force microscopy have been used to probe the interaction of a perfluorinated lubricant (Fomblin ZDOL) with hydrogenated amorphous carbon (a:C-H _x ) and amorphous carbon nitride (a:C-N _x ) substrates, two materials used as hard coatings in disk drive products. Temperature-programmed desorption measurements indicate that the nitride surfaces are more reactive toward this perfluorinated lubricant and, as a result, the thin lubricant film is more tightly bound to this substrate. Frictional force microscopy has been used to measure the coefficient of friction of the lubricated surfaces, 0.18 ± 0.02 for both substrate materials, and finds that frictional properties of these interfaces in the low load regime are influenced more by the presence of the lubricant rather than the adsorbed state of the film. Likewise, similar disjoining pressures were measured for the lubricant adsorbed on the different coating materials and suggest that the ultrathin nature of the adsorbed lubricant film dominates this property rather than adsorption states.     

Experimental simulation of phosphites additives tribochemical reactions by gas phase lubrication

Abstract

Tribochemical reactions of phosphites additives on steel surface have been simulated by gas phase lubrication. Trimethylphosphite (TMPi), P(OCH₃)₃, has been used as model molecule for phosphites additives. It has been introduced under gas phase up to 5 hPa in a new tribometer dedicated to gas phase lubrication. Friction tests have been carried out at ambient temperature and 100°C. Chemical analyses by X-ray photoelectron spectroscopy and by Auger electron spectroscopy have been conducted inside and outside of the track. Two kinds of analysis have been carried out: ex situ and in situ surface analyses after tribological test. Indeed, a new environmentally controlled tribometer allows friction test then accurate analyses without air exposure of the formed tribofilm. Tribotests conducted under TMPi gas phase show a reduction of friction coefficient until 0˙2 instead of 1˙4 under high vacuum. Jointly, formation of tribofilm has been confirmed by optical microscopy and ex situ chemical analysis. Comparison between analyses performed inside and outside of the wear scar indicates that the friction induces the formation of phosphide compound that could reduce friction. Moreover analyses show the formation of methoxy group (CH₃O) and carbonate originally from the decomposition of TMPi under friction into H₂ and CO. In situ analyses clearly show the importance to investigate an uncontaminated tribofilm in order to obtain a better characterisation of it and then a better comprehension of the tribochemical mechanisms.     

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.     

Two‐photon microscopy of deep intravital tissues and its merits in clinical research

Multiphoton excitation laser scanning microscopy, relying on the simultaneous absorption of two or more photons by a molecule, is one of the most exciting recent developments in biomedical imaging. Thanks to its superior imaging capability of deeper tissue penetration and efficient light detection, this system becomes more and more an inspiring tool for intravital bulk tissue imaging. Two‐photon excitation microscopy including 2‐photon fluorescence and second harmonic generated signal microscopy is the most common multiphoton microscopic application. In the present review we take diverse ocular tissues as intravital samples to demonstrate the advantages of this approach. Experiments with registration of intracellular 2‐photon fluorescence and extracellular collagen second harmonic generated signal microscopy in native ocular tissues are focused. Data show that the in‐tandem combination of 2‐photon fluorescence and second harmonic generated signal microscopy as two‐modality microscopy allows for in situ co‐localization imaging of various microstructural components in the whole‐mount deep intravital tissues. New applications and recent developments of this high technology in clinical studies such as 2‐photon‐controlled drug release, in vivo drug screening and administration in skin and kidney, as well as its uses in tumourous tissues such as melanoma and glioma, in diseased lung, brain and heart are additionally reviewed. Intrinsic emission two‐modal 2‐photon microscopy/tomography, acting as an efficient and sensitive non‐injurious imaging approach featured by high contrast and subcellular spatial resolution, has been proved to be a promising tool for intravital deep tissue imaging and clinical studies. Given the level of its performance, we believe that the non‐linear optical imaging technique has tremendous potentials to find more applications in biomedical fundamental and clinical research in the near future.     

Two‐photon laser scanning microscopy as a useful tool for imaging and evaluating macrophage‐, IL‐4 activated macrophage‐ and osteoclast‐based In Vitro degradation of beta‐tricalcium phosphate bone substitute material

Two‐photon microscopy is an innovative technology that has high potential to combine the examination of soft and hard tissues in vitro and in vivo. Calcium phosphates are widely used substitutes for bone tissue engineering, since they are degradable and consequently replaced by newly formed tissue. It is well known that osteoclasts are responsible for the resorption processes during bone remodelling. We hypothesize that also macrophages are actively involved in the resorption process of calcium phosphate scaffolds and addressed this question in in vitro culture systems by two‐photon laser scanning microscopy. Beta‐tricalcium phosphate specimens were incubated with (1) macrophages, (2) interleukin‐4 activated macrophages, and (3) osteoclasts for up to 21 days. Interestingly, macrophages degraded beta‐tricalcium phosphate specimens in an equivalent fashion compared to osteoclasts and significantly more than IL‐4 activated macrophages. An average of ～32% of the macrophages was partially filled with ceramic material while this was 18% for osteoclasts and 9% for IL‐4 activated macrophages. For the first time by applying two‐photon microscopy, our studies show the previously unrecognized potential of macrophages to phagocytose ceramic material, which is expected to have implication on osteoconductive scaffold design. Microsc. Res. Tech. 77:143–152, 2014. © 2013 Wiley Periodicals, Inc.     

New mechanism for field-induced anisotropy of cobalt-rich amorphous alloys

It is generally assumed that amorphous magnetic alloys respond to field annealing by a process of local directional ordering which leaves the amorphous structure intact. We have made a comparative microstructural study of field-annealed Co_95-xFe₅(BSi)x amorphous alloys using transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) with thin sections parallel to the ribbon surface. Field annealing response was measured from anisotropy in low-field hysteresis loops. These alloys show appreciable surface crystallization for annealing as much as 80 K below the bulk crystallization temperature. The surface crystallization proceeds by a known mechanism (selective oxidation) to which we have added a more detailed understanding. Three steps are involved: (1) formation of an amorphous borosilicate surface oxide layer during annealing; (2) depletion of glass stabilizing elements (boron and silicon) from the underlying amorphous metal substrate; (3) primary crystallization of the destabilized, metal-enriched subsurface layer to an fee or hep cobalt-rich phase. Striking differences in the microstructural morphology were revealed for different glass former ratios B/Si. For high B/Si ratios, the surface crystallites are predominantly fee Co and show a high density of oxygen faults. For low B/Si ratios, the surface crystallites are predominantly hep Co and almost free of faults. Response to field annealing is proportional to the B/Si ratio and correlates with the presence of oxygen faults in surface crystallites. Electron diffraction and microprobe analysis indicate that the surface oxide in silicon-rich alloys is a dense silica glass which appears to be an effective diffusion barrier to oxygen. The surface oxide in boron-rich alloys is a more porous oxide richer in B₂O₃. These observations appear to be related to those from perminvar alloys where oxygen was found to be necessary for field annealing to be effective.     

Quantitative analysis of backscattered-electron contrast in scanning electron microscopy

Backscattered-electron scanning electron microscopy (BSE-SEM) imaging is a valuable technique for materials characterisation because it provides information about the homogeneity of the material in the analysed specimen and is therefore an important technique in modern electron microscopy. However, the information contained in BSE-SEM images is up to now rarely quantitatively evaluated. The main challenge of quantitative BSE-SEM imaging is to relate the measured BSE intensity to the backscattering coefficient η and the (average) atomic number Z to derive chemical information from the BSE-SEM image. We propose a quantitative BSE-SEM method, which is based on the comparison of Monte–Carlo (MC) simulated and measured BSE intensities acquired from wedge-shaped electron-transparent specimens with known thickness profile. The new method also includes measures to improve and validate the agreement of the MC simulations with experimental data. Two different challenging samples (ZnS/Zn(O_xS_1–x)/ZnO/Si-multilayer and PTB7/PC₇₁BM-multilayer systems) are quantitatively analysed, which demonstrates the validity of the proposed method and emphasises the importance of realistic MC simulations for quantitative BSE-SEM analysis. Moreover, MC simulations can be used to optimise the imaging parameters (electron energy, detection-angle range) in advance to avoid tedious experimental trial and error optimisation. Under optimised imaging conditions pre-determined by MC simulations, the BSE-SEM technique is capable of distinguishing materials with small composition differences.     

Excitation under the scanning electron microscope of DNA-associated fluorescence from chicken erythrocyte nuclei,polytene chromosomes and adenovirus 2 virions

Biological structures not seen by conventional light microscopy, such as longitudinal striations in polytene chromosomes, and, at the limit of sensitivity, virions of adenovirus 2, have been detected via DNA-associated fluorescence excited under the scanning electron microscope. The maximum sensitivity realized, about 1 detected photon per 700 base pairs, falls short by about an order of magnitude of that required to achieve, in unreplicated specimens, the 2 nm intrinsic resolution of the method. A combination of D₂O-H₂O substitution with freeze-drying provides the best unquenching procedure found for in situ DNA. DNA-associated fluorescence for light microscopy can be created by moderate exposure of the specimen in the electron microscope.     

Structural analyses of Nd-doped CeO2 thin films deposited by pulsed laser deposition

CeO₂ thin films doped with neodymium oxides for application to gas sensors have been elaborated by the pulsed laser deposition technique. The films were deposited on orientated Si (100) substrates with variable deposition times (t = 90, 180 and 360 s) and molar fractions of Nd₂O₃ (0, 6.5, 15, 21.5 and 27 at.%). The resulting Nd–CeO₂ thin films were characterized by means of X‐ray diffraction analysis, scanning electron microscopy and transmission electron microscopy equipped with EDS (Energy Dispersive Spectrometer) microanalysis. From X‐ray diffraction analyses, it is clearly established that the texture is modified by Nd additions. The preferred (111) orientations of the CeO₂ crystals change into the (200) orientation. The morphology of the CeO₂ grains changes from triangles, for pure CeO₂ thin films, to spherical grains for Nd‐doped films. In addition, cell parameter analyses from X‐ray diffraction data show that a partial chemical substitution of Ce by Nd should occur in the face‐centred cubic lattice of ceria: this should give rise to Ce_1‐xNd_xO_2?z phases with oxygen non‐stoichiometry.     

Energy Spectra Of Dislocations In Silicon And Germanium

The properties of edge-type dislocations are strongly dependent on the temperature at which they have been introduced into the crystal. Dislocations produced at T < 0·6 T_m (T_m melting point) exhibit a richer variety of properties than those introduced at T > 0·6 T_m: in germanium a strong increase of the hole density, in silicon an electron para-magnetic resource (EPR)-signal, showing many fine details, and several peaks in the deep level transient spectroscopy (DLTS)-signal, are only found after low-temperature deformation. The increase in the hole density has been ascribed to point defect clouds, which surround the dislocation, and seem to control their mobility. The clouds are not stable at the deformation temperature. The electrical and optical properties of edge-type dislocations, introduced at T > 0·6 T_m into germanium, can be interpreted in terms of a half-filled one-dimensional band (for T ≥ 50 K), which might be due to dangling bonds in the dislocation core. In silicon the experimental data indicate a similar form of the local energy spectrum at dislocations.     

Toughening of hot pressed beta-alumina using zirconia additions prepared from zirconate,tartrate and carbonate precursor materials

The development of second phase zirconia precipitates in a beta-alumina matrix has been achieved using chemical reactions which occur during the firing process. The degree of success of each of several fabrication routes has been evaluated by use of toughness measurements and electron microscopy techniques. Approximately half of the routes yielded ～90% retention of tetragonal zirconia, resulting in an approximate doubling of the Mode 1 critical stress intensity factor (K_1c).     

Morphological and microscopic identification of three major medicinal Dendrobium species in Ta‐pieh Mountains area

Dendrobium is an important medicinal material in China. It has the effect of nourishing the stomach, nourishing yin and clearing heat. In China, there are many types of Dendrobium, and different Dendrobium species have different efficacy. The present study is aimed at distinguishing three major Dendrobium species from morphological and microscopic identification in Ta‐pieh mountains area. In this article, the roots, stems and leaves of Dendrobium huoshanense, Dendrobium officinale, and Dendrobium moniliforme are used as materials to compare the differences of tissues of these three Dendrobium species by morphological indexes and microscopic identification of different Dendrobium. The stem morphology of these three Dendrobium species was significantly different except for stem internodes number and the middle part of the stem diameter by measuring the stems of Dendrobium. To ensure the safe use of Dendrobium, we built a fast and convenient method combining normal and fluorescence microscopy was applied in the present study to distinguish D. huoshanense, D. officinale, and D. moniliforme. The microscopic results show that different types of Dendrobium exhibit different states that can be distinguished under normal light normal and fluorescence microscopy. This comparative study of morphology and microscopy contributes to the development of identification and quality evaluation of Dendrobium.     

Estimation of length and surface of anisotropic capillaries

Surface density (S_V) and length density (L_V) of myocardial capillaries have hitherto been estimated from their profile boundary length (B_A) and their numerical density (Q_A) on transverse sections by the simplifying assumptions of the Krogh model (perfectly anisotropic, straight, unbranched capillaries with constant cross-sectional area). As the capillaries actually are partially anisotropic, curved, branching cylinders with variable cross-sectional area, a geometrical bias arises from the model-reality discrepancies. We have applied and compared two methods to overcome these inconsistencies: (1) estimation of L_V and S_V by a more realistic model (the Dimroth-Watson distribution); (2) estimation of L_V and S_V from isotropic uniform random (IUR) sections. Twelve male Wistar rats were fixed by retrograde vascular perfusion. One pair of longitudinal and transverse sections, and six IUR sections per animal were selected at random from the left ventricular papillary muscles. Ultrathin sections were silver-impregnated and studied by light microscopic morphometry. Nearly identical estimates of L_V and S_V were found by both methods. The model-based estimation provides biologically meaningful anisotropy constants, but it presupposes knowledge of the anisotropy axis. The IUR method provides no measure of anisotropy, but it can be applied in tissues where the anisotropy axis is not known. Both methods are equally efficient and practically unbiased in S_V estimation, but the model-based estimation is far more efficient in L_V estimation.