扫描电镜与能谱仪

<正>扫描电镜利用精细聚焦电子束照射在样品表面,该电子束可以是静止或在样品表面作光栅扫描。在这个过程中,电子束与样品相互作用产生各种信号,其中包括二次电子、背散射电子、俄歇电子、特征X射线和不同能量的光子等,这些信号来自样品中的特定区域,分别利用探测器接收,可以提供样品的各种信息,用于研究材料的微观形貌、晶体学特征和微区化学成分。X射线能谱仪是扫描电镜附带的附件,通过检测从样品出射的特征X射线的波长或能量,测定样品元素的组成、相对含量以及分布。     

改革教学方法,提高扫描电镜实验教学效果

针对目前本科生扫描电镜实验教学中存在以理论讲解和教师操作为主,学生主动参与性差,教学效果不理想等情况,建立以提高实验教学效果为目标的教学改革方法。通过精心设计实验教学内容、改进教学方法,以实例教学法加深学生对二次电子和背散射电子像、分辨率及景深等抽象概念的理解,增加学生自制样品观察,突出能谱测试的应用场合。授课方式既有理论讲解,又有实例图示及相关计算,使实验教学更具趣味性,激发学生的求知欲望,体现学生的主体作用,培养学生分析问题、解决问题的能力,切实提高材料专业扫描电镜实验的教学效果。     

背散射电子成像与能谱技术结合用于金属负载型催化剂的分散性研究

扫描电子显微(配备能谱仪附件)技术作为表面微观分析的重要手段之一,可充分展现催化剂的表面形貌和微区成分,对催化剂的研制和开发具有重要意义.本文将背散射电子成像与X射线能谱仪结合,研究了 Au-Ni复合催化剂的表面形貌及活性组分的分散状态,并详细探讨了图像清晰度与扫描速度、工作电压、工作距离等的关系.研究发现,在扫描速度...     

Fe掺杂ZrO_2催化剂上苯酚气相甲基化（英文）

采用共沉淀法制备了Fe掺杂的ZrO_2样品,并采用X射线衍射、N_2吸附-脱附、紫外漫反射光谱、扫描电镜-电子能谱、氨程序升温脱附、X射线光电子能谱和原位红外光谱进行了表征.结果表明,Fe进入ZrO_2晶格中有效稳定了其晶相结构为单一的四方相.这些样品可很好地催化苯酚气相甲基化反应,其催化活性取决于Fe含量,并与样品中L酸有关.     

Nd3+掺杂钙钛锆石(Ca1-3x/2NdxZrTi2O7)晶型转变行为的研究

采用高温固相反应法制备Ca1-3x/2NdxZrTi2O7(0.0≤x≤0.5)系列钙钛锆石样品,借助X射线衍射(XRD)、拉曼光谱(Raman)、背散射电子像(BES)和能谱(EDS)分析,对其晶型转变行为进行了研究.结果 表明:随着Nd3+掺杂量的增加,钙钛锫石-2M(Zirconolite-2M)结构将向钙钛锆石...     

超高性能钕铁硼表面镀渗处理研究

通过磁控溅射进行钕铁硼磁体表面重稀土Tb镀膜,再经过渗扩热处理获得了综合性能近80[H_cj/kOe+(BH)_max/MGOe]的超高性能磁体,分析了其内在机制。借助扫描电镜背散射电子成像技术,研究了热处理温度对磁体磁性能和微观组织的影响,并探讨了晶界扩散法矫顽力提高的机理和微观结构变化规律。结果表明,经镀渗处理后磁体的矫顽力明显提高,剩磁无明显降低,温度稳定性得以显著改进,显微组织结构有了明显的优化,形成连续均匀薄层晶界富Nd相组织有效的包裹主相,能够有效降低相邻晶粒的磁耦合效应。Tb富集在2∶14∶1晶粒的表面区域而不是中心,不仅通过增强局部磁晶各向异性场来增加矫顽力,而且还保持了剩磁。     

研究沸石结构的低剂量高分辨电子显微学方法

介绍了一种研究沸石结构的低剂量高分辨电子显微学方法,该方法可以有效降低电子束对沸石样品的辐照损伤,获得的高分辨像的分辨率优于0．18nm。提出了降低电子辐照损伤的措施,阐述了低剂量高分辨成像技术的技术要点。     

基于扫描电镜和能谱仪的薄膜表面形貌和厚度同时测量研究

扫描电子显微镜通过电子束轰击样品产生的二次电子、背散射电子等实现对样品表面形貌的观测，通过对样品横断面的观测来获得薄膜厚度信息，但难以实现对薄膜表面形貌和厚度的同时观测。通过能谱仪研究各种厚度的薄膜同其激发的特征X射线计数率之间的关系，实现了通过特征X射线计数率来测量薄膜厚度的方法。对于激光吹气系统所需的钨薄膜而言，结果表明，计数率随薄膜厚度的增加先线性增加后趋于稳定，利用该曲线的直线部分作为刻度曲线，可实现对5～19μm范围内钨薄膜表面形貌和厚度的同时测量，精度约为10%,通过增加电子能量可实现对更厚样品的测量。该方法可推广到其他种类的薄膜研究，有助于推动薄膜物理研究的开展。     

扫描电镜技术在高分子表征研究中的应用

扫描电子显微镜(scanning electron microscope,SEM)是表征高分子材料微观结构及其组成信息重要的手段之一，具有操作简便、信号电子种类多样且对样品损伤较小等特点.本文系统阐述了SEM的工作原理，通过与透射电子显微镜(transmission electron microscope,TEM)进行比较，突出了其优势与特色.详细讨论了该技术的测试方法，包括样品制备、仪器参数设定、操作技巧与图像处理，并揭示了获得高质量SEM图像的关键技术.介绍了SEM不同的信号电子成像、SEM与其他仪器联用及SEM原位分析技术在高分子材料表征中的应用与进展.最后，对SEM的发展趋势进行了展望.     

聚苯乙烯/顺丁橡胶共混过程中的相结构

利用激光背散射装置结合密炼机对聚合物共混过程进行了在线分析．以典型完全不相容体系聚苯乙烯／顺丁橡胶为共混体系，对不同共混速度下结构参数随共混时间及共混条件如剪切速率等的变化进行了详细讨论．利用扫描电镜与激光背散射在线分析对聚合物共混过程结构参数变化进行了比较，结果显示聚苯乙烯／顺丁橡胶共混物处于熔融态与处于固态时结构基本相同．     

Electron Backscattering from Real and In-Situ Treated Surfaces

 Significant differences in backscattered electron (BSE) yields exist between the surfaces cleaned by methods used in electron microscopy and spectroscopy. These differences have been observed for Au, Cu and Al specimens, and are interpreted on the basis of simulated BSE yields. Composition and thickness of the surface contamination layers, responsible for the differences, are estimated. The results (7 nm of carbon on Au or 3 nm of oxide on Al) remain within expectation and indicate that the BSE yield measurements and BSE images should be interpreted cautiously. Peculiar results are obtained for Cu, perhaps due to a different cleaning procedure. A new concept of an information depth for the BSE signal is introduced as a depth within which the total BSE yield can be modelled as composed of the yields of layers proportional to their thickness weighted by the escape depths. This concept proved satisfactory for thin surface layers and brought the information depth values 2 to 4 times smaller than first estimated, i.e. half the penetration depth.     

扫描电子显微镜运行和管理的实践与探索

扫描电子显微镜常用于观察样品的内部结构以及化学组成,是材料学领域不可缺少的现代分析测试仪器. 绍兴文理学院使用扫描电子显微镜已十多年,年平均运行有效机时在1 000 h以上,是学校利用率最高的仪器设备之一. 结合大型仪器设备管理运行中的经验以及目前存在的一些问题,从检测技术提升、仪器共享、评价体系等方面对仪器的管理制度进行探讨.     

Closed-cell foam skin thickness measurement using a scanning electron microscope

Closed cell polymer foam skin thickness can be assessed by taking backscatter electron (BSE) images in a scanning electron microscope (SEM) at a series of accelerating voltages. Under a given set of experimental conditions, the electron beam mostly passes through thin polymer skin cell walls. That cell appears dark compared to adjacent thicker-skinned cells. Higher accelerating voltages lead to a thicker skin being penetrated. Monte Carlo modeling of beam-sample interactions indicates that at 5 keV, skin less than ～0.5 μm in thickness will appear dark, whereas imaging at 30 keV allows skin thicknesses up to ～4 μm to be identified. The distribution of skin thickness can be assessed over square millimeters of foam surface in this manner. Qualitative comparisons of the skin thicknesses of samples can be made with a simple visual inspection of the images. A semiquantitative comparison is possible by applying image analysis. The proposed method is applied to two example foams. Characterizing foam skin thickness by this method is possible using any SEM that is capable of collecting useful BSE images over a range of accelerating voltages. Imaging in low vacuum, where an electrically conductive metal coating is not required, leads to more sensitivity in skin thickness characterization.     

加氢精制催化剂表面纳米棒束的电子显微镜研究

利用场发射扫描电镜(SEM)、高分辨透射电镜(HRTEM)、X射线能谱仪(EDX)和选区电子衍射(SAED)分析,对实验室硫化态加氢精制催化剂外表面上的纳米棒束的形貌、化学成分、晶体结构进行研究.SEM结果表明,该纳米棒束普遍分布于催化剂外表面并向外生长,纳米棒束形态较为规整,长度为500～1 500 nm,直径为20...     

Characterization of the morphology of co-extruded, thermoplastic/rubber multi-layer tapes

Tapes with alternating semi-crystalline thermoplastic/rubber layers with thicknesses varying from 100 nm up to several μm were prepared by multi-layer co-extrusion. The variation in layer thickness was obtained by varying the thermoplastic/rubber feed ratio. A systematic study on the use of various microscopy techniques to visualize the morphology of the layered systems is presented. The relatively large length scales and the sample preparation make optical microscopy (OM) unsuitable to study the morphology of the multi-layer tapes. Although excellent contrast between the thermoplastic and rubber layers can be obtained, the usually applied, relatively large magnifications limit the use of transmission electron microscopy (TEM) and atomic force microscopy (AFM) to small sample areas. The large range of applicable magnifications makes scanning electron microscopy (SEM) the most suitable technique to study the morphology of the multi-layer tapes. The sample preparation for SEM with a secondary electron (SE) detector is often based on the removal of one of the components, which may induce changes in the morphology. SEM with a back-scattered electron (BSE) detector is a very convenient method to study the morphology over a wide range of length scales, where the contrast between the different layers can be enhanced by chemical staining. Finally, the nucleation behavior (homogeneous versus heterogeneous) of the semi-crystalline layers, as probed by differential scanning calorimetry (DSC), provides valuable information on the layered morphology. The use of relatively straightforward DSC measurements shows a clear advantage with respect to the discussed microscopy techniques, since no sample preparation is required and relatively large samples can be studied, which are more representative for the bulk.     

Electron microscopy methods for studying polymer blends—comparison of scanning electron microscopy and transmission electron microscopy

The possibility of using a scanning electron microscope (SEM) for studying the morphology of mechanical polymer blends was investigated. Compounds of SBS/EPDM, and both filled and unfilled NBR/EPDM were tested. OsO₄-stained thin-sections were also examined in a transmission electron microscope (TEM) and the results were compared.It seemed to be quite possible to use atomic number contrast detection in combination with OsO₄ staining for visualizing the morphology of the blends in SEM. Domains as small as 0·1 μm were clearly seen. This was done by means of a Robinson backscattered electron detector. Sample preparation was easy, 2 mm thick rubber plates were cut on dry ice to obtain a smooth surface. After staining, the samples were coated with a thin conductive carbon layer.The inner structures of SBS and the carbon black particles were not resolved in SEM but were easily seen in TEM.     

Improving in situ liquid SEM imaging of particles

This work presents in situ imaging of synthesized boehmite (γ-AlOOH) particles ranging from 20 to 100 nm, suspended in liquid, in a vacuum compatible microfluidic sample holder using a scanning electron microscopy (SEM) under the high vacuum mode and highlights the advantage of in situ liquid imaging of colloids. Nanometer-sized boehmite particles in high-level radioactive wastes at the Hanford site are known to be difficult to dissolve and cause rheological problems for processing in the nuclear waste treatment plant. Therefore, it is important to characterize boehmite particles and understand how they form aggregates in the liquid state. Several technical advancements are made to optimize in situ liquid SEM chemical imaging resulting in the improved ability to obtain secondary electron (SE), backscattered electron (BSE) images, and energy dispersive X-ray spectroscopy (EDX) spectra. Moreover, our results show mixed particles could be studied and identified based on the particle shape and elemental composition using in situ SEM imaging and EDX. Thus, we provide a new and improved approach to observe the evolution of particle dispersion and stability in liquid under conditions similar to those in the waste tank.     

Ultrastructure, histochemistry, and mineralization patterns in the ecdysial suture of the blue crab, Callinectes sapidus.

The ecdysial suture is the region of the arthropod exoskeleton that splits to allow the animal to emerge during ecdysis. We examined the morphology and composition of the intermolt and premolt suture of the blue crab using light microscopy and scanning electron microscopy. The suture could not be identified by routine histological techniques; however 3 of 22 fluorescein isothiocyanate-labeled lectins tested (Lens culinaris agglutinin, Vicia faba agglutinin, and Pisum sativum agglutinin) differentiated the suture, binding more intensely to the suture exocuticle and less intensely to the suture endocuticle. Back-scattered electron (BSE) and secondary electron observations of fracture surfaces of intermolt cuticle showed less mineralized regions in the wedge-shaped suture as did BSE analysis of premolt and intermolt resin-embedded cuticle. The prism regions of the suture exocuticle were not calcified. X-ray microanalysis of both the endocuticle and exocuticle demonstrated that the suture was less calcified than the surrounding cuticle with significantly lower magnesium and phosphorus concentrations, potentially making its mineral more soluble. The presence or absence of a glycoprotein in the organic matrix, the extent and composition of the mineral deposited, and the thickness of the cuticle all likely contribute to the suture being removed by molting fluid, thereby ensuring successful ecdysis.     

Nanocrystalline Domain Identification in Gold Films, by Backscattered Electron Imaging and Energy-Filtered Transmission Electron Microscopy

Gold nanocrystallites dispersed in an inhomogeneous gold matrix are detected by high-resolution scanning electron microscopy using a field emission source and backscattered electron detection in the composition mode, as well as by energy-filtered transmission electron microscopy in the plasmon energy region. The identity of the nanocrystalline domains was established by observing the same evaporated gold film samples but using bright-field, dark-field, electron diffractogram, and electron energy loss spectroscopy images in the transmission electron microscope. Comparison of these images shows that backscattered electron and plasmon energy detection can be used to identify crystalline domains in an otherwise chemically uniform sample. Copyright 2001 Academic Press.     

Molecular and elemental characterisation of mineral particles by means of parallel micro-Raman spectrometry and Scanning Electron Microscopy/Energy Dispersive X-ray Analysis

The “fingerprinting” of a molecular structure obtained by micro-Raman spectroscopy (MRS) can be successfully complemented by means of X-ray spot analysis through the application of scanning electron microscopy equipped with an X-ray detector (SEM/EDX). The elemental composition revealed by SEM/EDX is essential for a correct interpretation of the collected Raman spectra. The results presented here illustrate how the two techniques can be combined to characterize geological samples, especially in the case of individual particles. The samples involved in the experiments were Zr- and Ti-bearing sand from South Africa (with major minerals such as zircon and rutile) and U mine tailings from Hungary (rich with feldspars, quartz and sulphate minerals). Mineral phases detected by MRS were identified according to their respective main Raman shifts, with a spatial resolution up to 1 μm, depending on the parameters set. Some unusual and sometimes inexplicable Raman activity was observed, which was ascribed to and rationalized by the presence of accompanying elements as detected with EDX. The relocation of a particle by means of the two instruments was facilitated with TEM grids. Although the limitations of the sequential use of SEM/EDX and MRS, such as different beam sizes, probing depth and surface topography, should be considered in their application to the analysis of individual geological particles, the two methods appeared to be complementary. Not only do they provide correlated chemical information about the sample, but also enable chemical characterization that would be otherwise incomplete when analyzed on a stand-alone basis.