高分辨率原位环境透射电镜的发展与应用

材料受周围环境的影响而产生的结构或成分变化一直都是材料科学和工业研发领域最关注的方向之一。随着材料研究的纳米化,外场导致的材料在亚纳米或原子尺度上的结构变化越来越成为认知材料宏观和纳米材料特性之根本。在诸如纳米催化剂的催化机制,材料的氧化-还原机制,纳米材料的生长或受力形变,电、磁场对材料纳米尺度结构的影响及微量气体探测等很多研究中有许多问题都需要一种特殊的电子显微镜即高分辨率原位环境电镜来帮助寻求答案。本文简要地回顾了环境透射电镜技术的发展思路,对于现代气体环境透射电镜的主流技术作了初步介绍,特别强调了高分辨率环境电镜的重要性以及在环境电镜中实现高分辨率所需要关注的一些技术环节,并力图通过具体实验实例使读者充分了解高分辨率原位环境电镜在材料科学研究中的重要性。     

缸内直喷汽油机高压喷油器驱动电路的设计

为了实现缸内直喷汽油机(GDI)喷油量、喷油正时和喷油速率的精确控制,对喷油嚣驱动电路提出更高的要求.设计了一种GDI发动机喷油器驱动电路,该电路由BOOST升压、高端自举驱动和电流分段控制电路等模块组成,采用双电源供电,以硬件控制方式实现三段驱动反馈电流控制,节省了软件资源.实验表明,该电路可以有效减小喷油器的开启时...     

Development of a technique for in situ high temperature TEM observation of catalysts in a highly moisturized air atmosphere

To clarify the influence of moisture on the structural changes of heated nano materials, in situ high temperature transmission electron microscopy (TEM) has been carried out using a conventional analytical TEM combined with a gas injection-specimen heating holder. Air with high moisture content, above 94% relative humidity (RH), from a humidifier was directly injected onto the heated platinum catalyst dispersed on carbon black (Pt/CB), and the morphological changes of the specimens were observed at high magnification dynamically. The result of the experiment was compared with a result obtained from an experiment using air with a low moisture content, 34% RH. Active movement of the Pt particles, leading agglomeration and grain growth, occurred prior to degradation of the CB support at high moisture content. In contrast, the degradation of the CB support leading agglomeration and grain growth of the Pt particles occurred before the displacement of the Pt particles on the CB supports in a low humidity environment.     

Resonance suppression in a TEM cell

All TEmnp resonances in a TEM cell have been suppressed by cutting the cell walls longitudinally. The TMmnp resonances and propagating TEM mode were not affected. The suppressed resonances have a residual interaction with a biological body inside the cell. Because of this, the modified cell can only be used for bioeffects dosimetry studies at a small number of frequencies above the upper limit for the original cell. Where an accuracy of only +/- 5 dB is required, such as in some EMC studies, the effective bandwidth of the modified cell is twice that of the original cell.     

Development of a stage-scanning system for high-resolution confocal STEM

A stage-scanning system is composed of a specially designed transmission electron microscopy specimen holder equipped with a piezo-driven specimen stage, power supplier and control software. This system enables the specimen to be scanned three-dimensionally, and therefore confocal scanning transmission electron microscopy (STEM) can be performed with a fixed electron-optics configuration. It is demonstrated that stage-scanning confocal STEM images can be obtained with the lateral atomic resolution and the specimen can be moved three-dimensionally with high precision.     

利用TEM研究叶蛇纹石晶胞参数随温压条件的变化特征

对不存在特征变质矿物的蛇纹岩进行温压条件的限定是一个难题,因为其中的主要矿物叶蛇纹石可以在约400~700℃,1.0~5.0 GPa以上的温压范围内稳定存在。天然样品观察和高压实验结果都表明,叶蛇纹石的a轴晶胞参数与温度、压力相关,对温度、压力条件具有一定的指示意义。本文使用TEM测量全岩体系(各种化学成分都含有的体系)下通过高压实验得到的叶蛇纹石的晶体结构,与前人在Mg O-SiO_2-H_2O(MSH)体系下高压合成的叶蛇纹石的晶体结构进行对比,探讨全岩体系下叶蛇纹石的a轴晶胞参数对应的m值与温度、压力的相关关系。本次研究表明:(1)叶蛇纹石的m值随着压力的升高而升高;(2)叶蛇纹石中铝含量的升高使得m值往高温方向迁移;(3)温度升高,叶蛇纹石的m值变小,含水量相对升高。     

Conformal mapping analysis of a modified TEM cell

A modification procedure in which the inner conductor of the usual TEM cell is symmetrically finned with a pair of small vertical plates is proposed to obtain a more suitable uniform field. In such modified TEM cells, a fairly uniform field can be established just above the inner surface of the rectangular-shaped shield instead of in the central portion of the separation between the septum and the shield, and this uniform field can be used for EMC measurements without dielectric equipment support or on a ground screen. The usefulness of the proposed modification is illustrated by the conformal mapping analysis of a special modified TEM cell. A similar modification can also be made in a general TEM cell and GTEM cell for the aforementioned uses. Conclusions and discussions are given, and further work is suggested     

High pressure high temperature cell for electrical conductivitymeasurements of Earth-type materials

A high-pressure high-temperature cell has been constructed and used to determine the temperature dependence of the electrical conductivity of various geological materials at a frequency of 60 Hz. Test conditions in the cell approximate an in situ environment by means of a variable uniaxial confining pressure and a separately variable pore pressure. A wide array of constituents of typical oil bearing formations have been examined at temperatures up to 240°C     

Circular TEM cell for generating standard electromagnetic fields

A circular TEM (CTEM) cell for achieving the radiated EMC test without any rotation of the equipment under test is proposed. The authors also analyse field uniformity inside the cell and characteristic impedance by using a moment method (MM) which can determine the number of segments per line efficiently     

Beam alignment and related problems of spherical aberration corrected high-resolution TEM images

For spherical aberration corrected transmission electron microscopes recently developed, the Scherzer resolution in proportion to C(s) 1/4 lambda 3/4 is still inevitably limited by the influence of some other electron optical factors, such as chromatic aberration coefficient of objective lens (C(c)), beam divergence and alignment, incident electron energy spread (deltaE), and the instability of accelerating voltage (deltaV) and of lens current (deltaI). Depending on the image resolution guaranteed by C(s) correction, the defocus spread caused by C(c), deltaV, deltaI and deltaE would need to be reduced. The effect of beam alignment as a phase shift in contrast transfer function is also studied for the C(s) corrected microscopes with different values of C(s), defocus and spatial frequency. There is a relationship between the phase shift and defocus that allows us to find a series of 'alignment-free' focal conditions. A triangular relation among C(s), defocus and lattice spacing is established for proper image contrast and 'alignment-free' imaging with the C(s) corrected microscope.     

Development of new TEM specimen holder for cathodoluminescence detection

A simple, new TEM specimen holder to detect cathodoluminescence (CL) in a transmission electron microscope has been developed. This holder accommodates a flat light-collecting reflector below the specimen and CL signals are guided to an optical spectrometer outside of the microscope through a quartz optical fibre. The compact system requires no modification of the microscope itself and allows large-angle specimen tilting and easy combination with other associate analytical tools. Test data are presented to aid the future application of the holder.     

A high luminance high-resolution cathode-ray tube for special purposes

For those applications where light sources of high radiance or displays of high resolution are necessary, miniature cathode-ray tubes have been developed with monocrystalline luminescent screens. These newly developed screens consist of cerium-doped yttrium-aluminum garnet (YAG), epitaxially grown on commercially available YAG substrates; they have an excellent heat conductivity and are optically clear. The construction of the tube and its performance in two modes of operation are described. When the tube is operated with a continuous undeflected beam, the luminance of the spot is limited by thermal quenching of the phosphor material. Under these circumstances, the maximum luminance of 1.9 × 10⁸cd/m²(0.55 × 10⁸FTL or 4 × 10⁵W/m²sr) is reached at a power of 70 mW in a 3.5-µA 20-kV beam, focussed to a spot of 9 µm diameter. Equipped with appropriate deflection coils and scanned with an interlaced field of 575 active lines and 25-Hz repetition frequency, the tube can handle up to 20 W of beam power in a 12 × 16 mm²image area. In this mode, the luminance is limited by the design of the electron gun and the desired resolution. At 20 kV and 100 µA (i.e., at 7500 cd/m²) the tube has a half-intensity linewidth of 60 µm, which is equivalent to 500-TV limiting response lines in the same 12 × 16 mm²area.     

高钒高速钢中碳化钒的电镜分析

在轧钢轧辊及粉磨行业的锤头、颚板等耐磨件的生产应用中 ,高钒高速钢材料的耐磨性比高铬铸铁提高 3～ 5倍。高钒高速钢中碳化物类型较多 ,主要硬质相是钒的碳化物。以往研究多停留在光学显微镜、扫描电镜及X射线等手段分析高钒高速钢凝固结晶相组成及耐磨机制 ,未见用透射电镜电子衍射及衍衬方法对高钒高速钢中各类型碳化物晶型、形态及内部精细结构的分析工作的详细报道。本工作利用透射电镜对高钒高速钢中具有简单结构间隙相 碳化钒及M7C3 型碳化物形态及精细结构进行研究。高钒高速钢的化学成分 (wt.% ) :C 2 98,V 9 8,Cr 4 2 5 ,…     

Electromagnetic fields with arbitrary wave impedances generatedinside a TEM cell

It is shown that arbitrary electromagnetic fields and wave impedances can be generated inside a transverse electromagnetic (TEM) cell for RF susceptibility testing. This is achieved by simply exciting one port and terminating the other port with appropriate loads. Thus, TEM cells are not limited to producing a planar field environment with the free-space impedance of 377 Ω, but can also be used to generate high-impedance or low-impedance fields for special testing needs. Experimental results for only three load impedances are described. In principle, many other loads including reactive terminations could be used to create a particularly desired field and wave impedance inside the TEM cell     

FDTD analysis of a gigahertz TEM cell for ultra-wideband pulse exposure studies of biological specimens

Gigahertz transverse electromagnetic (GTEM) transmission cells have been previously used to experimentally study exposure of biological cells to ultra-wideband (UWB), monopolar, electromagnetic pulses. Using finite-difference time-domain (FDTD) simulations we examine the time-dependent electric field waveforms and energy dose spatial distributions within a finite volume of biological cell culture medium during these experiments. The simulations show that when one or more flasks containing cell culture media are placed inside the GTEM cell, the uniform fields of the empty GTEM cell are significantly perturbed. The fields inside the cell culture medium, representing the fields to which the biological cells are exposed, are no longer monopolar and are spatially highly nonuniform. These effects result from a combination of refraction and distortion of the incident wave, combined with excitation of resonant eigenmodes within the cell culture medium volume. The simulations show that these distortions of the incident waveform may be mitigated by supporting the sample on a high permittivity pedestal and modifying the incident waveform to more closely approximate a Gaussian pulse. Under all simulated conditions, the estimated maximum temperature rises are completely negligible, ensuring that any experimentally observed unusual cell function or histopathology can be associated with nonthermal effects.     

Development of panel structure for a high-resolution 21-in-diagonalfull-color surface-discharge plasma display panel

Plasma display panel (PDP) structure has been investigated to develop a 21-in-diagonal color plasma display with a high-resolution of 0.22-mm subpixel pitch. To realize a high-resolution display, a stripe alignment of three primary color elements such as red, blue, and green, was introduced. Four kinds of panel structures are compared and finally stripe rib and stripe phosphor structures were introduced for the three electrode surface discharge plasma display. The 21-in-plasma display developed with the structure has firstly been put into the market with sufficient performance, such as a wide operating voltage margin, a high luminance, and a wide viewing angle of more than 60 V, 200 cd/m² , and 160°, respectively     

高压冷冻技术及其在植物细胞超微结构中的应用

冷冻固定技术可以将生物组织和细胞内所有结构和成分同时固定。因此避免了因化学渗透固定而引起的各种假象。通常,在常压下冷冻技术仅能使生物样品表面１０～３０μｍ厚度得以充分固定,而高压冷冻技术则能使样品有效固定厚度增加至６００μｍ。尽管植物组织细胞具有特殊的结构－厚壁和含大量水分的液泡,使冷冻固定较为困难,但利用高冷冻技术仍能使２００μｍ厚度的样品得到充分固定,而且能够捕获近似自然状态的细胞超微结构。本     

Development of a miniature pressure transducer for biomedical applications

Miniature absolute pressure transducers are needed for biomedical implant applications. The design parameters are: 1) sensitivity, 2) size, 3) hysteresis, 4) temperature coefficient, 5) long-term stability, and 6) biocompatibility. The present devices cannot meet all the requirements, particularly in size, long-term stability, and biocompatibility. The results of a development program on implantable and indwelling pressure transducers are reported with emphasis on the study of long-term stability and reproducibility associated with reduced size. The sensor is a resistive bridge diffused on a     

Measuring the radiated emissions from a family of microprocessorsusing a 1-GHz TEM cell

This paper presents a series of measurements of the radiated emissions from 8 and 16 bit microprocessors. The radiated emissions were measured using a 1-GHz TEM cell that incorporates the device under test (DUT) into the cell structure itself. For the 16 bit processor, samples from each of the manufacturer's identified process corners were measured and compared. Two separate fabrication lines were compared for process variability. The spatial location on the wafer was measured for emissions variation. In addition, emissions were measured for a 16 bit processor as a function of the operating temperature. Finally a comparison was made between discrete implementations of a module digital core and the same circuit implemented as an multichip module (MCM)     

Advanced FIB sample preparation techniques for high resolution TEM investigations of HEMT structures

In this paper advanced sample preparation techniques based on focused ion beam (FIB) optimized for TEM investigation of high electron mobility transistor (HEMT) structures are presented. It is shown that the usage of an innovative in-situ lift-out method combined with X2 window and backside milling techniques as well as live thickness control and end point detection can significantly improve the quality of electron transparent samples required for high resolution TEM investigations. This advanced preparation flow is evaluated and demonstrated at GaN HEMT structures for atomic resolution TEM investigation.