SEM electron channelling patterns as a technique for the characterization of ion-implantation damage

Electron channelling patterns (ECPs) formed in back-scattered images in the scanning electron microscope (SEM) have been used occasionally to confirm surface amorphization during ion implantation. In order to place such observations on a more quantitative basis, the study reported here has explored the variation of ECP appearance with both specimen damage levels (and thus subsurface structures) and SEM accelerating voltage (i.e. sampled depth). Polished and annealed (0001) single crystal sapphire discs were implanted to various damage levels up to both subsurface and full surface amorphization. Damage levels were measured independently by Rutherford back-scattering (RBS). Selected-area ECPs were obtained in a Jeol-840 electron microscope operating over the range 5–40 kV in 5-kV steps. Progressive ECP degradation—in terms of high-order line disappearance—was observed with increasing dose, culminating in total pattern loss when full surface amorphization occurred. However, ECP information could still be obtained from the damaged near-surface material even when a subsurface amorphous layer was present, thus demonstrating the shallow retrieval depth of information from the ECP technique. Indeed, because the spatial distribution of damage from ion implantation is both calculable and measurable, these experiments have also allowed us, for the first time, to explore and demonstrate the shallow sample depths from which the majority of ECP contrast originates (< 150 nm in sapphire at an accelerating voltage of 35 kV), even when the beam penetration is considerable by comparison (～ 5 μm). Furthermore, the way in which this sampled depth varies with SEM accelerating voltage is both demonstrated and shown to be a powerful diagnostic technique for studying the distribution of near-surface structural damage.     

Magnetic field emission gun with zirconiated emitter

A magnetic-field-superimposed field emission gun with low aberrations and equipped with a zirconiated tungsten emitter has been developed for applications where very stable high probe currents are required. It has been tested on a conventional electron microscope at 10 kV and on an electron beam testing system at 1 kV. Probe current i = 250 nA in a probe size d = 0.4 μm is obtained at 10 kV; at 1 kV the resolution is 0.1 μm with i = 5 nA, and 0.4 μm with i = 30 nA. For these probe currents, the spatial broadening effect due to electron–electron interactions in the beam is the preponderant factor limiting the probe size.     

Applications of medium-voltage STEM for the 3-D study of organelles within very thick sections

Scanning transmission electron microscopy at 300 kV enables the visualization of nucleolar silver-stained structures within thick sections (3–8 μm) of Epon-embedded cells at high tilt angles (–50°; + 50°). Thick sections coated with gold particles were used to determine the best conditions for obtaining images with high contrast and good resolution. For a 6-μm-thick section the values of thinning and shrinkage under the beam are 35 to 10%, respectively. At the electron density used in these experiments (100e^—/Å₂/s) it is estimated that these modifications of the section stabilized in less than 10 min. The broadening of the beam through the section was measured and calculations indicated that the subsequent resolution reached 100 nm for objects localized near the lower side of 4-μm-thick sections with a spot-size of 5·6 nm. Comparing the same biological samples, viewed alternately in CTEM and STEM, demonstrated that images obtained in STEM have a better resolution and contrast for sections thicker than 3 μm. Therefore, the visualization of densely stained structures, observed through very thick sections in the STEM mode, will be very useful in the near future for microtomographic reconstruction of cellular organelles.     

Surface and internal structure correlation: high-voltage and scanning electron microscopies of wholemount alveolar walls of human lung

We found that the high-voltage electron microscope (HVEM) operating at 1–5 MeV was able to transilluminate and form a focused transmission image of whole-mounts of alveolar walls from human lung, a tissue sufficiently thin to require no embedment and sectioning. Resultant micrographs resembled a composite of scanning and transmission electron microscope images: surface and internal structure of the alveolar wall were visualized in a single micrograph. Although the scanning electron microscope extracts some subsurface information in the secondary electron mode, the HVEM produced better images of both surface and subsurface features. Lungs were fixed, dehydrated, critical point dried, and metal coated as for conventional scanning electron microscopy, then individual alveolar walls were excised by hand and mounted on transmission electron microscope grids. Regions of the alveolar wall up to 10 μm thick were delineated with the high-voltage electron microscope. Cell surface characteristics were correlated with cell type as identified by underlying cell internal structure. Whole white blood cells within capillaries of the alveolar wall were identified by the configuration of their nuclei. Features of the nucleus and surface of alveolar type II cells were recorded simultaneously. Whole red blood cells were imaged within intact capillaries that branched and wove from one alveolar surface to the other. HVEM analysis of excised alveolar septa allows definitive correlation of surface and underlying structures in single micrographs of broad portions of the alveolar wall and is an alternative to embedment, microtomy and serial section reconstruction for this uniquely thin tissue.     

RB-SiC亚表面损伤检测及其旋转超声磨削亚表面损伤特征

分别采用截面抛光法(包括以硅片作陪衬与以聚酯作陪衬两种形式)和界面黏接法检测了反应烧结碳化硅(Reaction Bonded SiC,RB-SiC)旋转超声磨削加工的亚表面损伤。为确定其中的最佳检测形式,采用表面破碎层深度、最大破碎层深度、平均裂纹深度、最大裂纹深度4个亚表面损伤评价指标对两种方法分别检测到的RB-SiC旋转超声磨削亚表面损伤进行对比分析。结果显示:截面抛光法(硅片作陪衬)检测到的4个指标值依次为3.30μm、6.59μm、8.64μm、17.44μm;截面抛光法(聚酯作陪衬)检测到的4个指标值依次为5.71μm、14.33μm、15.36μm、54.82μm;而界面黏接法检测到的4个指标值依次为9.19μm、19.45μm、13.04μm、32.20μm。试验结果表明,截面抛光法(硅片作陪衬)检测的精度更高,检测的亚表面损伤更符合实际情况。最后,基于此方法,对旋转超声磨削RB-SiC材料的亚表面损伤特征进行了总结。     

可调谐声光调Q CO2激光器

摘要：利用调Q脉冲激光器速率方程计算了自行设计的声光调Q小型CO2激光器的主要技术参数,分析了影响声光调Q CO2激光器输出的主要因素,提出了优化设计的途径和方法,实验结果与理论计算基本一致。经优化设计的激光器脉冲重复频率达1Hz～50kHz, 1kHz时在获得脉宽180ns,峰值功率4062w的激光输出,并利用光栅实现了激光输出波长的连续调谐,波长调谐范围9.2μm～10.8μm,该激光器在激光测距、环境探测及空间通讯等领域具有广泛的用途。     

A method for estimating the fibre length in fibre‐PLA composites

Wood pulp fibres are an important component of environmentally sound and renewable fibre‐reinforced composite materials. The high aspect ratio of pulp fibres is an essential property with respect to the mechanical properties a given composite material can achieve. The length of pulp fibres is affected by composite processing operations. This thus emphasizes the importance of assessing the pulp fibre length and how this may be affected by a given process for manufacturing composites. In this work a new method for measuring the length distribution of fibres and fibre fragments has been developed. The method is based on; (i) dissolving the composites, (ii) preparing the fibres for image acquisition and (iii) image analysis of the resulting fibre structures. The image analysis part is relatively simple to implement and is based on images acquired with a desktop scanner and a new ImageJ plugin. The quantification of fibre length has demonstrated the fibre shortening effect because of an extrusion process and subsequent injection moulding. Fibres with original lengths of >1 mm where shortened to fibre fragments with length of <200 μm. The shortening seems to be affected by the number of times the fibres have passed through the extruder, the amount of chain extender and the fraction of fibres in the polymer matrix.     

Sectioning and imaging hard mineral fibres in biological tissues

A technique is described which overcomes the problems associated with sectioning biological tissue containing hard mineral fibres. 0·2–0·5 μm thick sections were cut with a diamond knife, placed in a folding grid, conventionally stained with uranyl acetate and lead citrate and viewed at an accelerating voltage of 200 kV in the scanning transmission mode.     

晶体已加工表面频率特征对亚表层温度场的影响

为了更加准确地分析表面形貌对KH2PO4(KDP)晶体元件激光损伤和使用性能的影响，通过功率谱密度和连续小波变换对KDP晶体已加工表面存在的实际频率特征进行提取和重构。利用波动光学理论分析经入射波长1.064 μm、功率20 MW/μm2的激光束照射1 ns后，表面频率特征对KDP晶体亚表层光场及温度场的影响。结果表明，当表面频率特征的波长越接近入射光波长1.064 μm，KDP晶体亚表层的光场畸变现象越严重，会造成局部聚焦，温度越高；当波长超过20 μm时，在振幅不变的情况下，最高温度随着波长的增加基本不变。通过切削实验获得的KDP晶体已加工表面上明显存在的波长分别为14 μm、50 μm和140 μm，对KDP晶体亚表层造成的温升分别为56 K、22 K和12 K。当波长相同时，KDP晶体的最高温度与表面频率幅值成线性关系。随着表面频率波长的增加，温度最高点的位置向KDP晶体内部延伸。     

Acoustic imaging of high-temperature superconducting materials

A new method of microstructure examination, acoustic microscopy, was used to study high-temperature superconducting materials. The high-resolution images obtained (up to 0.4 μm resolution) visualize the specimen topography, variations in local acoustic properties, in particular surface and subsurface defects such as cracks, twins, phase and structural discontinuities and film peeling. For bulk specimens a quantitative characteristic was obtained: a local Rayleigh wave velocity (within an area of 10 × 10 μm), which makes it possible, in particular, to characterize individual crystallites in ceramics.     

High-power switches based on reversely switched-on dynistors for high-voltage pulse technologies

The results of comparative investigations of commercially produced reversely switched-on dynistors (RSDs) with an operating voltage of 2 kV and 76-mm-diameter structures are presented. The studies were performed in the mode of switching current pulses with an amplitude of 200 kA and a duration of 300 μs. The electric scheme of the power circuit of the generator of high-power high-voltage pulses with a switch on the basis of an assembly of RSDs is considered. RSD switches with an operating current of 250 kA and operating voltages of 12 and 24 kV are described. Some results of using RSD switches in high-voltage pulse technologies are presented.     

A new confocal scanning beam laser MACROscope using a telecentric,f-theta laser scan lens

A new confocal scanning beam system (MACROscope) that images very large-area specimens is described. The MACROscope uses a telecentric, f-theta laser scan lens as an objective lens to image specimens as large as 7·5 cm × 7·5 cm in 5 s. The lateral resolution of the MACROscope is 5 μm and the axial resolution is 200 μm. When combined with a confocal microscope, a new hybrid imaging system is produced that uses the advantages of small-area, high-speed, high-resolution microscopy (0·2 μm lateral and 0·4 μm axial resolution) with the large-area, high-speed, good-resolution imaging of the MACROscope. The advantages of the microscope/MACROscope are illustrated in applications which include reflected-light confocal images of biological specimens, DNA sequencing gels, latent fingerprints and photoluminescence imaging of porous silicon.     

基于混合材料模型的颗粒增强钛基复材高速磨削温度研究

针对颗粒增强钛基复合材料（Particulate reinforced titanium matrix composites,PTMCs）高速磨削加工,建立一种三维混合材料磨削温度场有限元仿真计算模型,既考虑了Ti-6Al-4V基体材料特性,又包含了材料内部的TiC增强颗粒,由此分析了高速磨削过程中温度场特征及其演变规律。结果表明：基于三维混合材料模型的PTMCs磨削温度预测值与试验值相差小（为8%以下）,而基于普通均质材料模型的磨削温度预测值与试验值相差大（为16%以上）。PTMCs工件表面磨削温度随着磨削用量的增加逐渐上升。当砂轮线速度为120 m/s、工件进给速度为6 m/min时,磨削深度从20 μm增加到100 μm,PTMCs工件表面磨削温度从346℃增加到987℃,温度梯度值从1 070~624℃/mm增加到1 570~1 310℃/mm。磨削温度及其分布梯度对PTMCs亚表层显微组织变化层深度存在显著影响,磨削深度从40 μm上升到80 μm,显微组织变化层深度从22 μm增大到40 μm;当磨削深度进一步从80 μm增加到100 μm时,显微组织变化层深度增加到53 μm。     

High-current pulse switching by thyristors triggered in the impact-ionization wave mode

The operation of a thyristor switch triggered in the impact-ionization wave mode was investigated. The switch contained two series-connected Т253-800-24 thyristors of the tablet design with a semiconductor- structure diameter of 56 mm. When a triggering pulse is applied to the switch at a voltage rise rate dU/dt of more than 1 kV/ns, the transition time of the thyristors to the conducting state was shorter than 1 ns. It was shown that the maximum amplitude of the no-failure current increases with an increase in dU/dt at the triggering stage. The possible mechanism of the influence of the dU/dt value on the thyristor breakdown current is discussed. In the safe operating mode at dU/dt = 6 kV/ns (3 kV/ns per single thyristor), the switch discharged a storage capacitor with a capacitance of 1 mF, which was charged to a voltage of 5 kV, through a resistive load of 18 mΩ. The following results were obtained: the discharge-current amplitude was 200 kA, the initial current rise rate was 58 kA/μs, the pulse duration (FWHM) was 25 μs, and the switching efficiency of 0.97.     

KDP晶体加工表面的亚表面损伤检测与分析

采用截面显微法和择优蚀刻法分别对磷酸二氢钾(KDP)晶体从线切割样品制备到磨削、抛光亚表面损伤进行检测,利用OLYMPUS MX40光学显微镜对表面腐蚀现象与亚表面裂纹形状进行观测,并对裂纹深度进行测量。结果表明,由线切割产生的亚表面损伤裂纹形状以"斜线状"为主,裂纹深度最大值为85.59 μm;由#600砂轮磨削产生的亚表面损伤深度最大值为8.55 μm。在(001)晶面出现了四方形的分布密度较高的位错腐蚀坑;而在三倍频晶面上出现的是密度较低、形状类似梯形的位错腐蚀坑。该研究为KDP晶体亚表面损伤提供了一种检测与分析手段。     

光栅平动式光调制器光学特性分析

提出了一种基于微光机电系统的可用于投影显示及相关器件的新型光栅光调制器,介绍了其结构、工作原理和加工流程.对器件进行光学分析,优化和仿真,得出器件结构参数与光学特性之间关系.器件的可动光栅占空比e=0.5,光栅常数d=6 μm,长度L=39 μm,宽度w=36 μm,边距w0=1.5 μm时,理论上±1级衍射效率η=37.0%,对比度V=625;可动光栅与下电极在开态和关态时间距分别为0.65 μm和0.78 μm,器件单像素尺寸为51 μm×51 μm.     

微通道结构带状电极电火花加工方法研究

针对大厚度、高深宽比金属微通道结构加工的难题,提出一种带状电极电火花加工方法,利用厚度30～100 μm的带状电极,在金属基体上高效制造微通道结构。研究了带状电极电火花加工机理,建立了带状电极在加工间隙中的运动模型,分析了影响带状电极运动的主要因素,搭建了带状电极电火花加工装置,开展了微通道结构带状电极加工实验研究,获得了带状电极电火花加工基础工艺规律。利用带状电极电火花加工方法成功加工出的具有200条微通道的反应器结构和44×45微换热器阵列结构,表明带状电极电火花加工可以实现窄宽度(100 μm以下)、大厚度(35 mm以上)、高深宽比(10以上)和高精度(缝宽标准差3 μm以内)的大批量微通道结构的高效加工,相关方法和技术有望在微模具、微散热器、微反应器等领域获得推广和应用。     

X-ray microanalytical resolution in frozen-hydrated biological bulk samples

In coated frozen-hydrated gelatin gels the backscattered electron yield does not increase during electron irradiation as it does in uncoated samples. Neither is the backscattered electron yield greater from coated frozen-hydrated gels than that from more conductive organic samples. This is interpreted as indicating that a significant distortion of the electron interaction volume, due to the development of a space charge, does not occur in electron irradiated frozen-hydrated gelatine gels when they are coated with a conducting coat. The depth resolution as estimated from models of biological samples in the form of frozen-hydrated photographic film and frozen-hydrated sections of gelatine gel is consistent with that computed from X-ray depth distribution curves, i.e. close to 2.0 μm at 15 kV. Lateral resolution was estimated from photographic film to be close to 2.0 μm also, at 15 kV.     

An injector of charged liquid particles

The design of an injector of charged liquid particles with diameters of 1–10 μm that move at velocities of up to 1400 m/s is described. The injector stably operates at a potential difference of 5–20 kV between the needle, on which charged droplets form, and the focusing electrode with a distance between the electrodes of 5–20 mm. The diameter of the metal needle was varied from 0.1 to 10 μm. Experiments showed that, depending on the needle length, the source can stably operate in two modes: at a needle length of ≤1.7 and ≥2.7 mm. The experimental technique and results are presented. The dependences of the characteristics of accelerated particles on the voltages across the plates of the electrostatic particle accelerator are determined. The experimental results are in good agreement with the computer simulation results.     

A procedure for increasing the contrast of biological specimens in edge-projection TEM

Rotary shadowing has been used to increase the image contrast of biological specimens during edge-projection imaging in the transmission electron microscope (TEM). In this imaging mode, biological specimens are adsorbed from aqueous solution onto a highly curved substrate and observed in a direction parallel to its surface. High contrast TEM images are obtained at 200 kV when a 1–3 nm layer of tungsten is thermally evaporated onto the substrate at an angle of about 9°. Individual adsorbates are clearly delineated by the smooth, continuous, and fine-grained tungsten layer that surrounds them. TEM images obtained with this technique can provide a unique view of biological adsorbates on metal, insulator or semiconductor substrates.