A metallographic and electron microscopic study of the structure of copper after dynamic pressing

Structural changes in copper samples subjected to severe plastic deformation with the use of the dynamic loading technique were studied. The deformation was caused by pressing blanks through two or three channels situated at an angle with respect to one another. The velocity of a blank before it got into the first channel was 280–450 m/s. Pressure in samples did not exceed 3–7 GPa. The microstructure of copper changed under the simultaneous action of high-velocity deformation and temperature increase. The formation of cellular dislocation structures, systems of microtwins, dynamic polygonization subgranular structures, and new recrystallized grains was observed. After two passes, the major part of a sample had a structure that consisted of thin fibers containing submicrodisperse (50–100 nm) grains.     

Assessing the structure and function of single biomolecules with scanning transmission electron and atomic force microscopes

The scanning transmission electron microscope (STEM) and the atomic force microscope (AFM) have provided a wealth of useful information on a wide variety of biological structures. These instruments have in common that they raster-scan a probe over a sample and are able to address single molecules. In the STEM the probe is a focused electron beam that is deflected by the scan-coils. Detectors collecting the scattered electrons provide quantitative information for each sub-nanometer sized sample volume irradiated. These electron scattering data can be reconstituted to images of single macromolecules or can be integrated to provide the mass of the macromolecules. Samples need to be dehydrated for such quantitative STEM imaging. In contrast, the AFM raster-scans a sharp tip over a sample surface submerged in a buffer solution to acquire information on the sample's surface topography at sub-nanometer resolution. Direct observation of function-related structural changes induced by variation of temperature, pH, ionic strength, and applied force provides insight into the structure-function relationship of macromolecules. Further, the AFM allows single molecules to be addressed and quantitatively unfolded using the tip as nano-tweezers. The performance of these two scanning probe approaches is illustrated by several examples including the chaperonin GroEL, bacterial surface layers, protein crystals, and bacterial appendices.     

An electron diffraction and high-resolution transmission electron microscopy study of defect structure in silicon doped with transition metal impurities

Features of defect formation upon the decomposition of a supersaturated solid solution of a transition metal in silicon were studied. Zinc was used as the transition metal impurity. The silicon was doped with zinc by high-temperature diffusion annealing with subsequent quenching. Microstructures of this material were studied by electron diffraction and high-resolution X-ray transmission electron microscopy combined with X-ray energy-dispersion microanalysis. It was established that the studied material was a quite perfect single crystal but contained chaotically distributed dislocations.     

Scanning transmission X-ray microscopic analysis of purified melanosomes of the mouse iris

Melanosomes are specialized intracellular membrane bound organelles that produce and store melanin pigment. The composition of melanin and distribution of melanosomes determine the color of many mammalian tissues, including the hair, skin, and iris. However, the presence of melanosomes within a tissue carries potentially detrimental risks related to the cytotoxic indole–quinone intermediates produced during melanin synthesis. In order to study melanosomal molecules, including melanin and melanin-related intermediates, we have refined methods allowing spectromicroscopic analysis of purified melanosomes using scanning transmission X-ray microscopy. Here, we present for the first time absorption data for melanosomes at the carbon absorption edge ranging from 284 to 290 eV. High-resolution images of melanosomes at discrete energies demonstrate that fully melanized mature melanosomes are internally non-homogeneous, suggesting the presence of an organized internal sub-structure. Spectra of purified melanosomes are complex, partially described by a predominating absorption band at 288.4 eV with additional contributions from several minor bands. Differences in these spectra were detectable between samples from two strains of inbred mice known to harbor genetically determined melanosomal differences, DBA/2J and C57BL/6J, and are likely to represent signatures arising from biologically relevant and tractable phenomena.     

Characterization and scanning electron microscopic investigation of crosslinked freeze dried gelatin matrices for study of drug diffusivity and release kinetics

Drug delivery is a promising technique to enhance the therapeutic efficacy of the drug. However, properties of carrier materials require intense improvement for effective transport of drug molecules. In the current study, attempts have been made to develop freeze dried gelatin matrices cross linked with genipin at various temperatures (5°C, 15°C and 25°C) prior to freeze-drying (-80°C). The freeze dried matrices thus obtained at the said temperatures are characterized for crosslinking density, compression strength, swelling behaviors. The matrix crosslinked at 25°C showed highest Flory-Rehner crosslinking density (467 ± 46) (p<0.05), highest compressive strength (12.36 ± 0.12) (p<0.05) and lowest equilibrium water content. In this context, scanning electron microscopy (SEM) was performed to study the surface morphology (size and shape of pores) of the crosslinked matrices. These images were further processed for quantitative analysis of morphological features, viz., areas, radius, ferret diameter, length of major and minor axis and eccentricity using MATLAB toolboxes. These quantitative analyses correlate transport and the release kinetics of model anti-inflammatory drug (indomethacin) from crosslinked matrices in vitro to tune as a controllable delivery system. The diffusional exponent (n) for all constructs ranging from 0.61 to 0.69 (p<0.05) (0.45相似文献   

A comparative study of nanoparticles in premixed flames by scanning mobility particle sizer, small angle neutron scattering, and transmission electron microscopy

Scanning mobility particle sizer (SMPS) and transmission electron microscopy (TEM) studies were conducted for TiO₂ and soot particles. The TiO₂ particles were produced from a premixed stagnation ethylene-oxygen-argon flame (? = 0.36) doped with titanium tetraisopropoxide. Soot was generated from a burner-stabilized premixed ethylene-oxygen-argon flame (? = 2.5). The close agreement among SMPS, TEM, and X-ray diffraction results for TiO₂ nanoparticles demonstrates that the probe sampling/mobility measurement technique is accurate for on-line analysis of the size distribution of particles as small as 3 nm in diameter. In the case of soot, notable disagreement between the SMPS and TEM sizes was found and attributable to the fact that the soot taken from the flame studied herein is liquid-like and that upon deposition on the TEM grid, the primary particles do not retain their sphericity. This interpretation is supported by measurements with photo ionization aerosol mass spectrometry, small angle neutron scattering, and thermocouple particle densitometry.     

Dose-limited spectroscopic imaging of soft materials by low-loss EELS in the scanning transmission electron microscope

Spectroscopic imaging in the scanning transmission electron microscope (STEM) using spatially resolved electron energy-loss spectroscopy (EELS) provides one of the few ways to quantitatively measure the real-space nanoscale morphology of soft materials such as polymers and biological tissue. This paper describes the basic principles of this technique and outlines some of the important attributes that define the achievable spatial resolution. Many soft materials can be differentiated from each other as well as from solvents based on their EELS fingerprints. Applying a multiple least squares (MLS) fitting algorithm using such spectral fingerprints to analyze spatially resolved spectrum datasets enables the quantitative mapping of the different components in a specimen. However, in contrast to TEM studies of many inorganic materials where the spatial resolution is limited principally by the spherical aberration of the objective lens, the spatial resolution associated with the imaging of radiation-sensitive soft materials is limited by the total electron dose to which they can be exposed before suffering irrevocable chemical or structural damage. The Rose criterion provides a simple guide to enhance the so-called dose-limited spatial resolution relevant to soft-materials imaging. By using the low-loss portion of an EELS spectrum where the inelastic scattering cross-sections are highest together with improvements in data-collection efficiency and post-acquisition data processing, the dose-limited resolution in spectrum images of solvated polymers has moved into the sub 10nm regime. This resolution is sufficient to solve important applications-oriented problems associated with hetero interfaces, nanoscale mixing, and nanophase separation.     

从能量的角度讨论两体碰撞问题

从能量角度导出了两体对心碰撞的能量损失公式,重新讨论了恢复系数的物理意义．     

Analysis of top and bottom surface structure in thin (001) Au films by high resolution transmission electron microscopy

Using computer-generated models of the (001) surface of Au a number of image computations were performed for high energy electron diffraction to match experimental transmission electron micrographs. With a multislice dynamical electron diffraction formalism it was possible to generate images from thin films which contained one roughened surface or both top and bottom surfaces roughened. Here, it will be demonstrated that the computer generated micrographs can be used to show both bulk lattice periodicities of 2.03 Å and the surface lattice of 2.86 Å and that these features are separable in real electron micrographs under favorable imaging conditions.     

2D atomic mapping of oxidation states in transition metal oxides by scanning transmission electron microscopy and electron energy-loss spectroscopy

Using a combination of high-angle annular dark-field scanning transmission electron microscopy and atomically resolved electron energy-loss spectroscopy in an aberration-corrected transmission electron microscope we demonstrate the possibility of 2D atom by atom valence mapping in the mixed valence compound Mn3O4. The Mn L(2,3) energy-loss near-edge structures from Mn2+ and Mn3+ cation sites are similar to those of MnO and Mn2O3 references. Comparison with simulations shows that even though a local interpretation is valid here, intermixing of the inelastic signal plays a significant role. This type of experiment should be applicable to challenging topics in materials science, such as the investigation of charge ordering or single atom column oxidation states in, e.g., dislocations.     

Observation of magnetic domain structure in Terfenol-D by scanning electron acoustic microscopy

The magnetic domain structure in oriented Tb_0.3Dy_0.7Fe_1.92 (Terfenol-D) is investigated by scanning electron acoustic microscopy (SEAM) in a wide frequency range from 75 to 530 kHz. Both secondary electron image and electron acoustic image can be obtained in situ simultaneously. By changing the modulation frequencies, the SEAM can be used as an effective nondestructive method to observe not only the surface topography and domain structure but also the subsurface domain structure and defects. The magnetic domain structure is verified by magnetic force microscopy (MFM). Furthermore, magnetic domains can be observed in both linear and nonlinear imaging modes by SEAM. The contributions to the image contrast are related to the signal generation through the piezomagnetic coupling mechanism, magnetostrictive coupling mechanism, and thermal-wave coupling mechanism.     

Analysis of the spatial orientation distribution of building blocks in polycrystals as determined using transmission electron microscopy and a backscattered electron beam in a scanning electron microscope

The advantages and disadvantages of the method of automatic analysis of electron backscattering diffraction (EBSD) patterns for studying spatial orientation distributions are considered as compared to transmission electron microscopy (TEM). A misorientation spectrum in a test alloy (Kh20N80 alloy) having a high content of annealing twins is experimentally studied using both TEM and EBSD, and the results obtained are compared.     

Reconstruction of surface topographies by scanning electron microscopy for application in fracture research

Stereoscopic scanning electron micrographs can be used to reconstruct the microscopic topography of material surfaces. By applying a system for automatic image processing we can obtain Digital Elevation Models (DEMs) of the investigated surface. These DEMs are used to measure the degree of deformation on metallic fracture surfaces. By modelling the deformation the amount of plastic energy that is necessary to shape the microductile fracture surface can be calculated. These values are compared with experimentally obtained results.     

复杂结构沿面闪络产生发展阶段模拟研究

以天光Ⅱ-A装置X-pinch负载腔为例,采用包含场致发射、二次电子倍增模型的三维模拟软件OPAL,对复杂结构中真空绝缘体沿面闪络的产生与发展阶段进行了模拟研究。模拟结果表明,阳极产生的二次电子在平行于绝缘体表面的电场分量的作用下从阴极座向大半径的运动,是导致沿面闪络的主要原因。并提出了阻断沿面闪络的方法及其原理。采用阻断沿面闪络的措施后,后续多次X-pinch负载腔放电实验证明,正常的回流电流增加了近20%,真空绝缘体上的沿面闪络得到了抑制。;     

复杂结构沿面闪络产生发展阶段模拟研究

以天光Ⅱ-A装置X-pinch负载腔为例,采用包含场致发射、二次电子倍增模型的三维模拟软件OPAL,对复杂结构中真空绝缘体沿面闪络的产生与发展阶段进行了模拟研究。模拟结果表明,阳极产生的二次电子在平行于绝缘体表面的电场分量的作用下从阴极座向大半径的运动,是导致沿面闪络的主要原因。并提出了阻断沿面闪络的方法及其原理。采用阻断沿面闪络的措施后,后续多次X-pinch负载腔放电实验证明,正常的回流电流增加了近20%,真空绝缘体上的沿面闪络得到了抑制。;     

Hypokinetic stress and neuronal porosome complex in the rat brain: the electron microscopic study

Porosomes are the universal secretory machinery in cells, where membrane-bound secretory vesicles transiently dock and fuse to release intravesicular contents to the outside of the cell during cell secretion. Studies using atomic force microscopy, electron microscopy, electron density and 3D contour mapping, provided rich nanoscale information on the structure and assembly of proteins within the neuronal porosome complex in normal brain. However it remains uncertain whether pathological conditions that alter process of neurotransmission, provoke alterations in the porosome structure also. To determine if porosomes are altered in disease states, the current study was undertaken for first time using high resolution electron microscope. One of pathologies that produce subtle alteration at the presynaptic terminals has been demonstrated to be hypokinetic stress. The central nucleus of amygdale is the brain region, where such alterations are mostly expressed. We have examined the width and depth of the neuronal porosome complex and their alterations provoked by chronic hypokinetic stress in above mentioned limbic region. Specifically, we have demonstrated that despite alterations in the presynaptic terminals and synaptic transmission provoked by this pathological condition in this region, the final step/structure in neurosecretion--the porosome--remains unaffected: the morphometric analysis of the depth and diameter of this cup-shaped structure at the presynaptic membrane point out to the heterogeneity of porosome dimensions, but with unchanged fluctuation in norm and pathology.     

Ion scattering spectroscopy and scanning tunneling microscopy: A powerful combination for surface structure analysis

Low-energy ion backscattering and scanning tunneling microscopy (STM) have been used in combination to get better insight into the field of surface crystallography. The synergic effectiveness resulting from the complementing character of the two methods has been exemplified at clean NiAl(111) and for oxygen and nitrogen adsorption on Cu(110). The position of the atom cores is accessible by the low-energy noble gas impact collision ion scattering spectroscopy with neutral detection (NICISS). As a technique averaging over a macroscopic area of the sample, NICISS is better suited to supply information on features of completely developed phases, either on clean or adsorbate saturated surfaces. Additional information, on the other hand, can be gained by scanning tunneling microscopy (STM), which as a powerful local probe may be used to image surfaces with atomic resolution and to monitor defects, steps and the growth kinetics of e.g. adsorption-induced phase changes.     

重复频率强流电子束的产生和传输实验研究

电子束真空二极管重复频率运行时,它将表现出与单次运行时不同的特点。在电子束产生过程中,屏蔽半径应尽可能地小,且击穿延时时间较短,故选择石墨作为阴极材料。实验结果表明：在重复频率运行时,当环型阴极环厚较薄时,阴极的发射电流密度较大,因此对阴极的加热效应也加强,等离子体的膨胀速度加快,从而使得二极管阻抗减小,最后几次输出的电子束的电流较大,而电压减小;当重复频率较高时,由于加热效应使得阴极等离子体膨胀速度加快,最后几个脉冲阴极发射能力增强,波形重复性变差;当引导磁场强度增大时,阴极等离子体受到较大的磁场力约束,横向膨胀速度减慢,从而使得电子发射面积减小,总发射电流减小,二极管的阻抗增大。最后取引导磁场为1.5 T,阴极环厚为1 mm,得到重复频率100 Hz、束压827 kV、束流8.22 kA、脉冲波形之间重复性很好的均匀电子束输出。