Characterization of ultrafine coal fly ash particles by energy-filtered TEM

In this study, energy-filtered transmission electron microscopy is demonstrated to be a valuable tool for characterizing ultrafine coal fly ash particles, especially those particles encapsulated in or associated with carbon. By examining a series of elemental maps (K-edge maps of C and O, and L-edge maps of Si, Al, Ti and Fe) recorded using the three-window method, considerable numbers of titanium and iron species with sizes from several nanometres to submicrometre were shown to be present, typically as oxides dispersed in the carbonaceous matrix. Crystalline phases, such as rutile and iron-rich oxide spinel, were also identified from electron diffraction patterns and high-resolution TEM images. Information about these ultrafine coal fly ash particles regarding their size, morphology, elemental composition and distribution, and crystalline phases, which has not been available previously in conventional ash studies, should be useful in toxicological studies and related environmental fields.     

Application of recording and processing of energy-filtered image sequences for the elemental mapping of biological specimens: Imaging-Spectrum

Computerized energy-filtered transmission electron microscope (EFTEM) permits the recording and the processing of energy-filtered images, allowing a part of an electron energy-loss spectrum for each picture element to be obtained. This method, called ‘Imaging-Spectrum’, uses a Zeiss CEM902 coupled to several image analysis systems. The actual configuration records sequences of 48 images, 256 × 256 pixels, in steps of the energy loss, ΔE. Processing these sequences results in part of a core-loss EELS-spectrum for each pixel. This approach produces elemental maps with a short processing time. We have implemented three kinds of background calculation for the image subtraction. The influence of the irradiation dose and of the energy selecting slit width on the quality of the spectra is investigated. The method is applied to the analysis of some biological specimens (pericellular coat behaviour during adhesion between macrophages and red blood cells and location of calcite microcrystals in dental pulp cells). The Imaging-Spectrum method appears to be suitable for the analysis of large areas.     

Comparison of EFTEM and STEM EELS plasmon imaging of gold nanoparticles in a monochromated TEM

We present and compare two different imaging techniques for plasmonic excitations in metallic nanoparticles based on high energy-resolution electron energy-loss spectroscopy in a monochromated transmission electron microscope. We demonstrate that a recently developed monochromated energy-filtering (EFTEM) approach can be used in addition to the well established scanning technique to directly obtain plasmon images in the energy range below 1 eV. The EFTEM technique is described in detail, and a double experiment performed on the same, triangular gold nanoparticle compares equivalent data acquired by both techniques, respectively.     

Determination of the Fe content of embedded Cu-rich particles in ferritic alloys using energy-filtered TEM

A novel technique for the quantification of the iron content of copper precipitates in ferritic steels is presented. Energy-filtered (EF) imaging has been used to extract elemental maps with high spatial resolution. These maps contain enough information to attempt the quantification of the signal produced by the precipitates when either a line profile is measured across them or the whole image signal is integrated. Assumptions such as sphericity of the precipitates and composition variations are discussed. Special attention to the assessment of drift on the information extracted from EF images has been taken. Minimum detectability and optimum acquisition conditions are discussed.     

Zero-loss energy-filtered imaging of frozen-hydrated proteins: model calculations and implications for future developments

Energy-filtered transmission electron microscopes operating in zero-loss mode are used increasingly to study biological material in frozen-hydrated conditions. The contrast enhancement and improved structural resolution obtainable by this method have been studied using Monte-Carlo model calculations for the scattering processes occurring in such samples. Three models representing typical situations have been analysed, each normalized to minimal beam damage. It is shown that for proteins in thin layers of ice an optimal signal-to-noise ratio is achieved in the 80–120-keV electron energy range. For proteins which have to be embedded in thicker ice layers, a considerably higher acceleration voltage is required. In particular, electron energies above 200 keV would be desirable for electron diffraction work on microcrystals.     

Retrieval of absorptive potential variation in electron beam sensitive specimens using a single energy-filtered bright-field TEM image

A method is presented for retrieving the variation of the absorptive potential in electron beam sensitive soft material. The absorptive potential is directly related to the variations in atomic density and in chemical composition fluctuation. In our approach only a single zero-loss energy-filtered bright-field transmission electron microscopy (TEM) image is sufficient to obtain this information. The accuracy and the effectiveness of this proposed method has been tested using both simulation and experiment. As an experimental example of soft (organic) material, the variation in absorptive potential in an unstained tissue sample of zebrafish gill has been determined.     

Structural characterization of TiN/NbN multilayers: X-ray diffraction, energy-filtered TEM and Fresnel contrast techniques compared

Two TiN/NbN multilayers with wavelength 13.6 and 6.15 nm have been characterized by X-ray diffraction (XRD), Fresnel contrast analysis (FCA) and energy-filtered transmission electron microscopy (EFTEM). Good agreement between the composition profile obtained by FCA and EFTEM is obtained if the lower resolution of the EFTEM images is taken into account. The relative advantages and disadvantages of the techniques are discussed. Used together the two TEM techniques provide a quantitative characterization that is consistent with, and for some parameters provides more precise values than, that from XRD. The analysis shows that the multilayers have narrow interfaces (< 1 nm) and a composition amplitude close to 95% for the longer wavelength.     

Chemical mapping of a block copolymer electrolyte by low-loss EFTEM spectrum-imaging and principal component analysis

Energy-filtered transmission electron microscopy spectrum-imaging (EFTEM SI) in the low electron energy-loss range is a valuable technique for probing the chemical structure of a material with nanoscale spatial resolution using a reduced electron dose. By analyzing EFTEM SI datasets using principal component analysis (PCA), the constituent chemical phases of the material can be identified in an efficient manner without prior knowledge of the specimen. We implement low-loss EFTEM SI together with PCA to investigate thin films of the block copolymer electrolyte poly(styrene-block-ethylene oxide) (PS-b-PEO) blended with a sodium salt. PCA identifies three main phases, the first and second phases corresponding to the two blocks of the copolymer and a third phase corresponding to the salt. The low-loss spectra for these phases are extracted from a noise-reduced EFTEM SI dataset and used to generate a chemical map of the material by multiple linear least square fitting. We validate the results of the low-loss EFTEM SI/PCA technique by applying the method to a control PS-b-PEO sample that does not contain the sodium salt, and by conducting spatially resolved X-ray energy-dispersive spectrometry on the salt-containing PS-b-PEO thin film.     

A simple algorithm for measuring particle size distributions on an uneven background from TEM images

Nanoparticles have a wide range of applications in science and technology. Their sizes are often measured using transmission electron microscopy (TEM) or X-ray diffraction. Here, we describe a simple computer algorithm for measuring particle size distributions from TEM images in the presence of an uneven background. The approach is based on adaptive thresholding, making use of local threshold values that change with spatial coordinate. The algorithm allows particles to be detected and characterized with greater accuracy than using more conventional methods, in which a global threshold is used. Its application to images of heterogeneous catalysts is presented.     

基于粒子滤波的移动机器人同时定位和环境模型的建立

介绍了一种基于粒子滤波的移动机器人同时定位与地图创建方法。通过旋转超声传感器获得环境信息，利用贝叶斯规则更新栅格地图，然后利用粒子滤波对机器人进行定位，之后地图更新和机器人定位交替进行，直到将整个环境探测完毕。仿真结果表明机器人能较好的完成环境探测的任务。     

Element specific imaging with high lateral resolution: an experimental study on layer structures

Planar defects and individual layers in ceramic material are chemically imaged by high resolution energy-filtering TEM using a post-column imaging electron energy filter. Objects are barium layers in the cuprate superconductor NdBa₂Cu₃O_7−δ (isostructual to YBa₂Cu₃O_7−δ) as well as planar defects and precipitates of β-WB in tungsten- and chromium-doped TiB₂. The barium layers with a spacing of 0.42 nm in the cuprate are resolved in jump-ratio images using the Ba_N edge. In the boride system the β-WB precipitates with thickness of 0.8 nm can be chemically imaged in elemental maps of B_K, Ti_L ,Cr_L and W_M. The B as well as the Ti map show a decrease in intensity at the precipitates, whereas in the W map an increase in intensity is observed. The boron-deficient layers with a spacing of 0.38 nm in the β-WB precipitate can be resolved in boron jump-ratio images. Additionally, defects containing single boron-deficient layers are chemically imaged. Hence structures in the dimension of interatomic distances can be imaged with respect to their elemental constituents. Although high resolution electron spectroscopic images contain strong interference contrast from elastic scattering, after normalization or background subtraction the element specific images are dominated by chemical contrast.     

TEM cross-section preparation with minimal ion milling time

The production of high quality thin film TEM cross-sections suitable for microanalysis is often a difficult and time-consuming task. This is particularly so in cases where there exists a large difference between the sputtering rate of the film and that of the substrate. The problem is further exacerbated when the levels of internal stress in the film are high enough to cause the substrate to distort during the thinning process. This paper describes some modifications to existing techniques which allow a greater degree of mechanical thinning prior to the ion etching stage. Consequently, ion milling times are drastically reduced, typically by a factor of at least 5 and by as much as 25 in some cases.     

ESI contrast analysis: a new approach for element analysis with energy-filtering transmission electron microscopy (EFTEM)

Element microanalysis with energy-filtering transmission electron microscopy can be performed in different ways. Electron energy-loss spectroscopy (EELS) records the intensity as a function of the energy loss from selected regions. Elemental mapping with electron spectroscopic imaging (ESI) uses energy-filtered images at an element-specific energy loss from which a background image has to be subtracted. A combination of these two approaches is Image-EELS, which records a series of energy-filtered images, each at a different energy loss and measures the intensity of selected regions as a function of the energy loss. As an additional procedure ESI contrast analysis is introduced; with this we can investigate the image contrast as a function of the energy loss. The contrast can be measured for the total image or for selected regions as the standard deviation of the grey levels divided by the mean grey level. This procedure is added as a new feature to the existing Image-EELS program, so that EELS intensity spectra and the contrast can be directly compared. Alternatively, the contrast can be calculated step by step from individually recorded electron spectroscopic images, so that only simple equipment for image analysis is sufficient to realize this new method. Inner shell ionizations produce characteristic, but often weak element edges in energy-loss spectra which can be detected more sensitively and reliably as a rapid increase in contrast. Regional analysis of the contrast as a function of the energy loss, combination of data from different regions and the possibility to increase the intensity during recording of the images expand the application range of this new analytical method which bridges the gap between ESI and EELS analysis. With ESI contrast analysis it is possible to discriminate between faint element signals and artefacts in elemental mapping. This new approach for element detection is especially advantageous for biological objects which usually contain very small amounts of the interesting elements in heterogeneous and complex objects. As an example, nervous tissue of a fish was analysed after cytochemical precipitation of endogenous calcium.     

实现半闭环控制磨削加工的数控改造

数控磨削加工的难点在于,由于砂轮在磨削过程中是不断磨损的,因此使得被磨工件的加工尺寸不能恒定。在普通磨床上采用特殊的数控改造方式,同时采用特殊结构的数控加工程序编制,在磨削过程中可以实现砂轮的修整,达到了半闭环控制的磨削加工效果。在保证被磨工件的尺寸精度的基础上,提高了被磨工件的几何加工精度和生产效率。     

在AutoCAD中应用Autolisp实现轴承参数化绘图

以深沟球轴承的参数化绘图为示例,介绍了用Autolisp对AutoCAD图形进行的参数化绘图程序设计。实践表明,Autolisp语言功能强大,易学易用,是AutoCAD二次开发的重要工具。     

Electron spectroscopic imaging of antigens by reaction with boronated antibodies

Two small homogeneous markers for electron spectroscopic imaging (ESI) containing eight dodecaborane cages linked to a poly-α,ε- l -lysine dendrimer were synthesized; one of these was made water soluble by the attachment of a polyether. The markers were coupled to the sulfhydryl group of (monovalent) antibody fragments (Fab') by a homobifunctional cross-linker. While the coupling ratios of the poorly water-soluble compound did not exceed 20%, the polyether-containing variant reacted quantitatively. Its suitability for immunolabelling was tested in a study of the mechanism of the transcellular transport of an administered heterologous protein (bovine serum albumin, BSA) through ileal enterocytes of newborn piglets by endocytotic vesicles in comparison to conventional immunogold reagents. The post-embedding technique was employed. The boronated Fab' gave rise to considerably higher tagging frequencies than seen with immunogold, as could be expected from its form- and size-related physical advantages and the dense packing of BSA in the vesicles. The new probe, carrying the antigen-combining cleft at one end and the boron clusters at the opposite end of the oval-shaped conjugate, add to the potential of ESI-based immunocytochemistry.     

Elemental mapping with elastically scattered electrons

We describe a technique for efficient, quantitative, standardless elemental mapping using a high-angle annular detector in a scanning transmission electron microscope (STEM) to collect elastically scattered electrons. With a single crystal specimen, contrast due to thickness variations, diffraction, and channelling effects can be avoided, so that the resulting image contrast quantitatively reflects variations in impurity concentration. We compare a number of simple analytical approximations to the elastic scattering cross sections and show that a standardless analysis is possible over a wide range of atomic number and inner detector angle to an absolute accuracy of better than 20%.     

Preparation of thin ceramic monofilaments for TEM observation with novel embedding processes

An applicable method to prepare transmission electron microscopy specimens from ceramic fibers for longitudinal and cross-sectional observations is investigated. The method includes novel embedding processes to fix fibers, a polishing process using a self-manufactured device to get uniformly low thickness (40 μm for L-fiber, 60 μm for C-fiber), a one-side dimpling process to grind the specimen to near electron transparency (about 5 μm in thickness for both L-fiber and C-fiber) and an efficient ion milling process using calculated parameters. These techniques are reliable to accomplish the preparation with high quality in a relatively short time. Many factors related to the preparation processes are discussed.     

A TEM phase plate loading system with loading monitoring and nano-positioning functions

We present a phase plate loading system developed for a commercial transmission electron microscope (TEM). Our system can be installed without modifying the optical design of the TEM. This system is equipped with a loading monitoring set that allows users to easily and safely locate the phase plate between the pole pieces, and also comes with an airlock that permits quick loading of a phase plate without the need to re-vent the TEM column. The system uses a home-made three-axis nano-positioner to precisely position the phase plate hole at the desired location. Our system has a precision of ∼10 nm, an improvement of one order of magnitude compared with the precision of a phase plate holder modified from an objective aperture. We demonstrate the successful installation and the use of the loading system to place a phase plate at the desired position. Our phase plate loading system can be used to accommodate various types of phase plates and thus provides a good way to greatly speed up the development of TEM phase plates.     

Advances and problems with TEM characterization of Cr/CrN multilayer coatings

Multilayer Cr/CrN/Cr/Cr(N,C) and Cr/CrN with 8 and 32 layer coatings were deposited on austenite substrates using pulsed laser deposition (PLD) technique. The microstructure observations were performed using Philips CM20?, TECNAI G² F20 – TWIN? and JEOL EX4000? transmission microscopes. The performed experiments indicated that lowering the argon flow from 60 to 30 cm³/s during chromium ablation changes buffer layers microstructure from nearly amorphous to nano‐crystalline. The nitride or carbo‐nitride layers turned out to be less sensitive to changes in nitrogen flow during deposition. The columnar microstructure of Cr layers is coarser than those in CrN ones under the same deposition condition. This observation proved also that relying on PLD technique as thin as 30 nm layers might be formed within multilayer Cr/CrN coatings.