Simulation study on image contrast and spatial resolution in helium ion microscope

We performed Monte Carlo simulation of helium (He) ion induced secondary electron (SE) emission in order to compare the secondary electron image characteristics between He and gallium (Ga) scanning ion microscopes (SIM) and scanning electron microscope (SEM). For 10-50 keV He ion bombardment SE yield increases gradually with increasing the atomic number, Z2, of the target, as well as for the electron bombardment. However, for 30 keV Ga ion bombardment, SE yield shows an opposite Z2 dependence. The calculated SE yield is much larger than that for both electron and Ga ion bombardment. The incident angle dependence of the SE yield approximately obeys the inverse cosine law even at high angles of 85 degrees and more. On the other hand, for electron bombardment, the incident angle dependences are much weaker for low energy and high Z2. These indicate that the image contrast on He-SIM is clearer than those of SEM. Among the electron excitations by incident He ions, recoiled target atoms and excited electrons, the first one having narrow excitation volume dominates the SE yield, so that the spatial image resolution in SIM using zero-diameter He beams with the energies of 10-50 keV is prospected to be smaller or better (<0.1 nm) than for 30 keV Ga ion and 1 keV electron beams.     

Comparative study of depth and lateral distributions of electron excitation between scanning ion and scanning electron microscopes

In order to study the contrast difference between scanning ion microscopes (SIM) and scanning electron microscopes (SEM), the depth and lateral distributions of secondary electrons escaped from surfaces of 17 metals with atomic numbers, Z2, of 4-79 were calculated for bombardment with 30 keV Ga ions and for 10 keV electrons. For both projectiles, the excitation depth generally decreased with increasing Z2, while showing the same periodic change as the secondary-electron yield. However, an opposite trend in Z2 dependence between the Ga ion and electron bombardments was calculated with the lateral distribution of secondary electrons escaped from the surface. Except for low Z2 metals, the lateral distribution, which is much narrower for 30 keV Ga ions than for 10 keV electrons, indicates that the spatial resolution of the secondary-electron images is better for SIM than for SEM, if zero-sized probe beams are assumed. Furthermore, the present calculation reveals important effects of electron excitation by recoiled material atoms and reflected electrons on the lateral distribution, as well as the secondary-electron yield, for the Ga ion and electron bombardments, respectively.     

Monte Carlo simulation of topographic contrast in scanning ion microscope

Topographic contrast of secondary-electron (SE) images in a scanning ion microscope (SIM) using a focused gallium (Ga) ion beam is investigated by Monte Carlo simulation. The SE yield of heavy materials, in particular, due to the impact of 30 keV Ga ions increases much faster than for the impact of electrons at < or =10 keV as a function of the angle of incidence of the primary beam. This indicates the topographic contrast for heavy materials is clearer in a SIM image than in a scanning electron microscope (SEM) image; for light materials both contrasts are similar to each other. Semicircular rods with different radii and steps with large heights and a small wall angle, made of Si and Au, are modeled for comparison with SE images in SEM. Line profiles of the SE intensity and pseudo-images constructed from the profiles reveal some differences of the topographic contrast between SIM and SEM. We discuss not only the incident-angle effect on the contrast, but also the effects of re-entrances of primary particles and SEs to the neighboring surface, the effect of a sharp edge on the sample surface, and the effects of pattern size and beam size.     

绝缘膜负带电时的表面局部电场与二次电子返回特性

为分析IC多层版图扫描电镜(SEM)对准检测所利用的负带电成像原理,采用Mott弹性散射截面和修正的Bethe非弹性碰撞公式,对点照射入射电子在绝缘膜中的散射过程进行了Monte Carlo模拟,得到负带电绝缘物表面的局部电位分布.在此基础上计算了二次电子从表面出射后在局部场作用下的运动轨迹,获得了SEM像的二次电子信号电流.结果表明,在弱负带电条件下,照射点处表面电位越低,返回表面的二次电子就越多,对应的二次电子信号电流越弱.此结果与SEM实验中图像亮度随照射时间的变化规律相符     

Time of flight spectrometer for scanning electron microscope

Experimental results which show the feasibility of use a time-of-flight spectrometer to obtain energy information of emitted electrons in a scanning electron microscope (SEM) are presented. The method is able to simultaneously display the energy distribution of emitted electrons over their entire energy range, from elastic backscattered electrons down to the low energy secondary electrons, and is thus predicted to have major signal-to-noise benefits for topographic, material, and voltage contrast in an SEM.<>     

A virtual scanning electron microscope. 4. Simulator-based implementation

A virtual scanning electron microscope (VSEM), which is based on a simulator of information, obtained on a real scanning electron microscope (SEM), is described. A semiempirical generation model of images in a SEM, operating in the low-voltage mode and high-voltage mode during recording backscattered and secondary slow electrons, forms the basis of a virtual SEM. A method of comparing real and virtual images is proposed. Examples of operation of the virtual SEM are given for elements of structures which are located both far from the edges of the structure and near these edges.     

扫描电子显微学中二次电子发射过程的蒙特卡洛模拟

利用蒙特卡洛模拟固体中电子散射轨迹的计算方法，系统地研究了扫描电镜中二次电子信号的发射过程。该模拟电子与固体相互作用的蒙特卡洛模型包含了级联二次电子产生的过程，并且采用光学介电函数方法描述电子的能量损失和相伴的二次电子激发。由于模拟计算可以给出背散射电子和二次电子的绝对产额，以及它们随加速电压和样品的原子序数的变化关系，因此可以用于模拟元素衬度和形貌衬度像。还计算得到了关于二次电子产生和发射的其它分布，并与实验结果作了比较。     

电子显微镜的现状与展望

本文扼要介绍了电子显微镜的现状与展望，透射电子显微镜方面主要有：高分辨电子显微学及原子像的观察，像差校正电子显微镜，原子尺度电子全息学，表面的高分辨电子显微正面成像，超高压电子显微镜，中等电压电镜，１２０ｋＶ，１００ｋＶ分析电镜，场发射枪扫描透射电镜及能量选择电镜等，透射电镜将又一次面临新的重大突破，扫描电子显微镜方面主要有：分析扫描电镜和Ｘ射线能谱仪，Ｘ射线波谱仪和电子探针仪，场发射枪扫描电镜和     

Applying secondary ion mass spectrometry to the analysis of elements in goblet cells of conjunctiva

We investigated the location of elements in the goblet cells of rat conjunctiva by analyzing ion images produced by secondary ion mass spectrometry (SIMS) and comparing them with those produced by energy dispersive X-ray analyser (EDX). Conjunctivas of normal Spraque-Dawley rats were quenched in propane prechilled liquid nitrogen. Semi-thin sections were made with a cryo-ultramicrotome, freeze-dried, carbon-coated and observed under a light microscope, SIMS and scanning electron microscope (SEM). In the element analysis by SIMS, images of positive ions were examined with an O2+ primary ion source and images of negative ions with a Ga+ ion source. The same sections were observed and analysed with SEM-EDX. Morphological features and images of elements with SIMS and EDX were compared. Na, Mg, K, and Ca were detected as positive ions and OH, CN, P, S, and Cl as negative ions with SIMS, but C, N, O, Na, Mg, P, S, Cl, K, and Ca were detected with EDX. The spatial resolution of SIMS in element location was higher than that of EDX. Many elements were clearly located in the goblet cells on ion images by SIMS. Element ion images were demonstrated more densely in goblet cells than in other parts within conjunctiva and by SIMS compared to EDX. SIMS is a useful method for the detection of elements and their locations in ocular tissues and cells.     

The potential of the scanning low energy electron microscopy for the examination of aluminum based alloys and composites

When studying the physical properties and technological parameters of aluminum-based alloys and composites, some partial tasks, connected with the microstructure of the material bulk, pose a problem for established microscopic techniques. The topography and distribution of sub-micrometer sized precipitates and of segregations on the particle/matrix interface, for example, are difficult to observe by conventional methods of transmission and scanning electron microscopy. The introduction of a high-resolution low-energy mode into the scanning electron microscope, relying on the deceleration of an already formed and focused primary beam just in front of the specimen, enables one to browse over the full electron energy range with great ease. This method offers added value consisting of the diminished interaction volume of electrons, the favorable combination of secondary and backscattered electron signals emitted at increased yields and collected at extremely high efficiency and the availability of unconventional contrasts excited by slow electrons. Demonstration experiments have been performed on structures based on the Al-Mg-Si alloy, and oriented towards examination of the Mg-Si precipitates in the alloy and sub-micrometer spinel crystals growing on the matrix-ceramic interface in a composite filled with alumina particles.     

RF磁控溅射和氨化法制备GaN纳米棒和纳米颗粒

利用射频磁控溅射法分别溅射ZnO中间层和Ga2O3薄膜到Si(111)衬底上,然后ZnO/Ga2O3薄膜在管式石英炉中常压下通氨气进行氨化,高温下ZnO在氨气气氛中被还原生成Zn而升华,而在不同的氨化时间下Ga2O3和氨气反应合成出GaN纳米棒和纳米颗粒。X射线衍射(XRD)测量结果表明,利用该方法制备GaN纳米棒和颗粒具有沿c轴择优取向生长的六方纤锌矿结构。利用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、傅里叶红外透射谱(FTIR)及选区电子衍射(SAED)观测和分析了样品的形貌、成分和晶格结构。研究分析了此种方法合成GaN纳米结构的反应机制。     

聚焦离子束制备透射电子显微镜样品的两种厚度判断方法

透射电镜样品的厚度是透射电镜(TEM)表征中一个重要参数,快速准确地判断样品厚度是制备高质量样品的前提.本文通过使用聚焦离子束(FIB)制备了带有厚度梯度的透射电镜样品(Si、SrTiO3和LaAlO3),并提出两种制样过程中快速判断厚度的方法.第一种通过扫描电子显微镜(SEM)的衬度变化经验地判断样品的厚度;第二种是用FIB在样品边缘切一个斜边,通过SEM测量斜边侧面的宽度用几何方法推断样品的厚度.这两种方法都通过会聚束电子衍射(CBED)和电子能量损失谱(EELS)测量的厚度作为检验标准.对比认为,样品较薄时用SEM衬度测厚比较合适;样品比较厚时用几何方法测量比较直接.     

High Purity and Large-scale Preparation of β-Ga2O3 Nanowires and Nanosheets by CVD and Their Raman and Photoluminescence Characteristics

Ga2O3 nano-structures,nanowires and nanosheets are produced on Au pre-coated(111) silicon substrates with chemical vapor deposition(CVD) technique.By evaporating pure Ga powder in the H2O atmosphere under ambient pressure the large-scale preparation of β-Ga2O3 with monoclinic crystalline structure is achieved.The crystalline structures and morphologies of produced Ga2O3 nano-structures are characterized by means of scanning electron microscope(SEM),X-ray diffraction(XRD),selected area electron diffraction(SAED) and transmission electron microscope(TEM).Raman spectrum reveals the typical vibration modes of Ga2O3.The vibration mode shifts corresponding to Ga2O3 nano-structures are not found.Two distinguish photoluminescence(PL) emissions are found at about 399 nm and 469 nm owing to the VO-VGa excitation and VO-VGa-O excitation,respectively.The growth mechanisms of Ga2O3 nanowires and nanosheets are discussed with vapor-liquid-solid(VLS) and vapor-solid(VS) mechanisms.     

High Purity and Large-scale Preparation of β-Ga2O3 Nanowires and Nanosheets by CVD and Their Raman and Photoluminescence Characteristics

Ga2O3 nano-structures, nanowires and nanosheets are produced on Au pre coated（111） silicon substrates with chemical vapor deposition（CVD） technique. By evaporating pure Ga powder in the H2O atmosphere under ambient pressure the large-scale preparation of β-Ga2O3 with monoclinic crystalline structure is achieved. The crystalline structures and morphologies of produced Ga2O3 nano-structures are characterized by means of scanning electron microscope（SEM）, X-ray diffraction（XRD）, selected area electron diffraction （SAED） and transmission electron microscope（TEM）. Raman spectrum reveals the typical vibration modes of Ga2O3 The vibration mode shifts corresponding to Ga2O3 nano-structures are not found. Two distinguish photoluminescence（PL） emissions are found at about 399 nm and 469 nm owing to the VO-VGa excitation and VO-VGaO excitation, respectively. The growth mechanisms of Ga2O3 nanowires and nanosheets are discussed with vapor liquid-solid（VLS） and vapor-solid（VS） mechanisms.     

离子束沉积PdC_x纳米结构及其输运性能

采用离子束沉积方法制备了PdCx纳米结构,并对材料的电子输运性能进行了研究。利用扫描电子显微镜(SEM)和X射线能谱仪(EDX)分析了材料的微观结构和组成,利用原子力显微镜(AFM)分析了纳米结构的尺寸大小,利用高分辨率透射电子显微镜(HRTEM)分析了材料的原子结构。采用电阻桥测试了PdCx纳米结构的电阻,在低温保持器(OXFORD2)中对其电子传输性能进行了测试。X射线能谱仪(EDX)检测结果表明,该纳米结构金属含量低,表现出非金属性。高分辨率透射电子显微镜(HRTEM)检测结果表明,其为PdCx多晶纳米结构,与所观测到的电子输运性能结果一致。     

A virtual scanning electron microscope. 3. A semiempirical model of the SEM signal generation

Experiments are analyzed on scanning electron microscopes (SEMs) with test objects having a trapezoidal profile and large tilt angles of the side walls. Based on the analysis, a semiempirical generation model of images in a SEM, operating in the low-voltage mode and high-voltage mode during recording back-scattered and secondary slow electrons (SSEs), is proposed. The model is intended for application in a virtual SEM (VSEM).     

低能电子束照射集成电路芯片时的静态电容衬度分析

在研究低能电子束照射绝缘物时在二次电子返回特性的基础上,通过绝缘物表面照射微区和衬底之间的有效电容,获得了表面电位和二次电子信号电流在表面电荷积累过渡过程中随照射条件的变化关系,建立了电子束照射覆盖有绝缘膜的IC芯片时形成静态电容衬度的理论模型.从理论上分析了电子束照射条件和芯片内部形貌、材料参数对静态电容衬度的影响,解释了在扫描电镜实验中的最大衬度现象及其对应的最佳电子照射条件.     

Formation of GaN Nanowires by Ammoniating Ga2O3 Films Deposited on Oxidized Al Layers on Si Substrate

Large quantities of gallium nitride（GaN） nanowires have been prepared via ammoniating the Ga2O3 films deposited on the oxidized aluminum layer at 950℃ in a quartz tube. The nanowires have been confirmed as crystalline wurtzite GaN by X-ray diffraction, X-ray photoelectron spectrometry scanning electron microscope and selected-area electron diffraction. Transmission electron microscope （TEM） and scanning electron microscopy（SEM） reveal that the nanowires are amorphous and irregular, with diameters ranging from 30 nm to 80 nm and lengths up to tens of microns. Selected-area electron diffraction indicates that the nanowire with the hexagonal wurtzite structure is the single crystalline. The growth mechanism is discussed briefly.     

电子束蒸发沉积TiN薄膜的电学特性研究

采用TCP(Transverse coupled plasma)等离子体辅助电子枪蒸镀技术,在玻璃衬底上制备了TiN薄膜。用X射线衍射仪(XRD)、扫描电子显微镜(SEM)和原子力显微镜(AFM)研究了不同工艺条件对薄膜晶体结构和表面形貌的影响;用四探针法测量薄膜的电阻率变化。结果表明,所制备的TiN薄膜在(111)晶面有择优取向。与金属薄膜类似,TiN薄膜的平均表面粗糙度与电阻率之间存在近似线性关系,并且电阻率随残余应力增大而增大。     

Visualization of the interaction between blood vessels and podocytes in the mouse embryonic glomerulus using a barium-infusion method for scanning electron microscopy

The present study revealed three dimensionally the formation of epithelial cells and vascular capillaries in glomeruli of the kidney of the mouse embryo. Barium sulphate was infused through the umbilical vessel of 16.5-17.5-day embryos and the backscattered electron (BSE) image and the secondary electron (SE) image of the identical area of glomeruli were obtained by scanning electron microscopy (SEM). The BSE images directly showed the vascular structure of the glomerulus, while the SE images showed a developmental process of podocytes from epithelial cells. Podocytes were more closely located to the vascular capillary than other epithelial cells. These findings were compared with those obtained in the resin cast model of glomeruli. Thus, the metal infusion-SEM method described here can trace the process of formation of urine filtration barrier in the mouse embryonic glomerulus.