电子显微镜观察高聚物断面样品的制备方法

本文采用液氮冷却脆断,离子切割和超薄切片等制样手段制备高聚物样品的断面,通过扫描电镜或透射电镜观察其断面结构,提出适合维持高聚物样品断面原貌的制样方法。     

常温条件制备金属薄膜样品

一文在上海交通大学产电解双喷制样仪上,通过电解液高氯酸和冰醋酸,对几种金属材料进行了常温下,透射电镜薄膜样品的制备,并获得成功。     

改良游离细胞扫描电镜制样方法适用于凋亡细胞观察

利用常规游离细胞扫描电镜制样方法制备的凋亡细胞样品,镜下凋亡检出率较低,细胞容易脱落变形,不能满足观察要求。本文采用200μmol／L双氢青蒿素作用前列腺癌PC-3细胞48h,诱导细胞凋亡;通过改良的制样方法制样并观察凋亡细胞超微结构。结果显示,凋亡细胞和凋亡小体阳性率明显提高,细胞贴附紧密、分布均匀,凋亡细胞超微结构比透射电镜更直观形象。     

烟草单个花粉原生质体透射镜样品制备及其超微结构观察

本文介绍了烟草花粉原生质体作试验材料，用自制微吸管手工预先挑选单个花粉原生质体，戊二醛微滴固定，然后用低熔点琼脂糖或明胶预包埋，小塑料管顶和包埋单个花粉原生质体，进行透射电镜样品制备，初步建立了单个原生质体电镜制样的技术流程，通过电镜观察，与群体制样法比较，结果是令人满意的。此项技术的建立，为今后植物性细胞超微结构的研究，提供了一项精细的操作方法。     

磷钨酸乙醇染色法在嗜铬颗粒电镜X射线显微分析中的应用

通过比较常规透射电镜制样法、快速冷冻固定－冷冻超薄切片法及磷钨酸乙醇（EPTA）染色法在嗜铬颗粒透射电镜X射线显微分析中的应用，发现磷钨酸乙醇染色法能使嗜铬颗粒电子着色，从而较好地显示嗜铬颗粒的超微结构。同时磷钨酸乙醇染色法也以在一定程度上原位保留生物样品中元素，可以应用于检测样品元素含量的变化或比较样品元素含量的组间差别，提示磷钨酸乙醇染色法是一种可应用于透射电镜X射线显微分析的经济简便的生物样品制备方法。     

烟草单个花粉原生质体透射电镜样品制备及其超微结构观察

本文介绍了烟草花粉原生质体作试验材料，用自制微吸管手工预先挑选单个花粉原生质体，戊二醛微滴固定，然后用低熔点琼脂糖或明胶预包埋，小塑料管顶扣包埋单个花粉原生质体，进行透射电镜样品制备，初步建立了单个原生质体电镜制样的技术流程，通过电镜观察，与群体制样法比较，结果是今人满意的。此项技术的建立，为今后植物性细胞超微结构的研究，提供了一项精细的操作方法。     

薄膜材料透射电镜截面样品的简单制备方法

针对薄膜材料透射电镜截面样品制备过程复杂、制样成功率低的问题,本文详细介绍了一种操作简单、实用性强的制备方法,采用该方法可以成功制备出脆性衬底上薄膜材料的TEM截面样品。     

智能卡芯片产品失效分析样品制备技术

以智能卡芯片产品为例,介绍了四类失效分析样品制备技术,可用于指导失效分析制样种类选取和制样方法选取,能够满足大部分的失效分析制样需求。     

扫描电镜生物制样的改进

扫描电镜生物制样的改进李庚午，朱命炜，张根发（河南师范大学生物系，新乡４５３００２）利用ＳＥＭ观察生物材料，因生物材料不导电而必须在观察前进行一系列处理，在这些过程中以固定、脱水、干燥、喷镀几个环节尤为重要，加之生物材料种类繁杂，其制样方法各环节的种...     

InGaN/GaN岛形量子阱样品透射电镜制样与表征方法

本文研究了氮化物半导体三维岛形结构的透射电镜制样技术,减小了样品在制样过程中的结构损伤,并对In Ga N/Ga N量子阱进行了结构、成分和发光特性的表征。通过对三维Ga N小岛非极性小面微观结构的分析,确定了侧壁小面皆为半极性面,说明小面生长的In Ga N/Ga N量子阱受到较小的极化效应影响。该岛形量子阱的结构特征,有效地增强了量子阱的发光效率,同时由于不同小面的存在,实现了同一小岛的多波长白光发射。     

聚焦离子束技术制备与样品表面平行的TEM样品

制备目标材料的高质量TEM样品对TEM测试表征和结果分析具有决定性作用.聚焦离子束（FIB）技术由于其微观定位选区制样的优势在TEM样品制备上已有一定应用.本文介绍了FIB/SEM双束系统制备与样品表面平行的TEM样品的方法（“V-cut”）,并与传统的FIB制备TEM样品的方法（“U-cut”）进行比较,分析了该方法对实现某些特殊研究目的的独特性和适用性.     

EPMA在热镀锌钢板镀层组织分析中的应用

本文介绍了应用EPMA-1600型电子探针测定热镀锌钢板镀层成分和元素重量百分比,并结合光学显微镜金相分析确定镀层中相结构的方法。结果表明,该方法能准确、快速地原位测定镀层中元素含量和组织结构,是镀层与钢基结合性能评价的重要检测手段。     

TEM specimen preparation of a phase-change optical disk

It has been popular to use transmission electron microscopy (TEM) observation for investigating the microstructure of a phase-change optical disk. In the present work, a new method to prepare a plan-view TEM sample from a disk has been developed. In this method, a copper mesh is placed on a specific area of interest in the disk in advance and then the material is thinned down. By employing this procedure, it becomes possible for the first time to obtain foils that contain the specific area. Furthermore, an advanced method to prepare a cross-sectional TEM sample has also been developed, in which elimination of the polymer substrate is followed by ion milling. With this method, it is possible to prepare cross-sectional foils for high-resolution and analytical electron microscopy observations.     

Local thickness and composition analysis of TEM lamellae in the FIB

High-resolution TEM image quality is greatly impacted by the thickness of the TEM sample (lamella) and the presence of any surface damage layer created during FIB–SEM sample preparation. Here we present a new technique that enables measurement of the local thickness and composition of TEM lamellae and discuss its application to the failure analysis of semiconductor devices. The local thickness in different device regions is accurately measured based on the X-ray emission excited by the electron beam in the FIB–SEM. Examples using this method to guide FIB–SEM preparation of high quality lamellae and to characterise redeposition are shown for Si and III–V semiconductor devices.     

一种气相沉积薄膜TEM样品制备技术——改进的可溶盐基片法

本文对可溶盐基片方法制备薄膜TEM样品进行了改进。改进后不仅保持了原可溶盐基片法方便、高效和快捷的特点,还可以根据表征需要获得薄膜在不同生长阶段微结构的样品。     

基于FIB-SEM制备尖晶石微米颗粒的球差校正透射电镜样品

针对尖晶石微米颗粒材料,利用聚焦离子束扫描电镜双束系统(FIB-SEM),在传统透射电镜样品制备方法的基础上进行技术性改进,成功制备了高质量的球差校正透射电镜样品.并利用球差校正透射电镜成功观察到了尖晶石颗粒的截面原子结构,为更深入地研究尖晶石材料的结构和性能奠定了基础.     

FIB-SEM双束技术简介及其部分应用介绍

聚焦离子束( FIB)与扫描电子显微镜( SEM)耦合成为FIB-SEM双束系统后,通过结合相应的气体沉积装置,纳米操纵仪,各种探测器及可控的样品台等附件成为一个集微区成像、加工、分析、操纵于一体的分析仪器。其应用范围也已经从半导体行业拓展至材料科学、生命科学和地质学等众多领域。本文介绍了双束系统中的一些关键概念及基本原理并综述了其在材料科学领域的一些典型应用,包括透射电镜( TEM)样品制备,微纳尺度力学测试样品制备以及材料三维成像及分析。     

TEM样品制备辅助研究介质层可靠性失效机理

研究了TEM样品制备条件对Cu/低k制程ILD TDDB失效样品及含更低介电常数(k=2.7)介质层样品的TEM成像质量的影响,发现在一定的样品制备条件下低介电常数介质的疏松特性可在TEM成像时得到增强显示,进而揭示了某Cu/低k制程ILD TDDB可靠性失效样品的失效机理为芯片制造过程中介质层沉积温度异常导致其疏松特性增强,介电常数降低,从而导致其电绝缘性能下降而引起TDDB可靠性测试项目失效.     

透射电子显微镜原位磁场双倾样品杆的研制

本文简述了透射电镜磁场双倾样品杆的设计方案,展示了Philips/FEI透射电镜磁场双倾样品杆的研制成果.利用该样品杆可以产生100 Oe的连续磁场,也可以产生140 Oe以上的瞬间磁场.通过“U”型磁组件和样品杯的巧妙设计,尽可能的减小了电子束在横向磁场中的偏移量.     

Back-etch method for plan view transmission electron microscopy sample preparation of optically opaque films

Back-etch methods have been widely used to prepare plan view transmission electron microscopy (TEM) samples of thin films on membranes by removal of the Si substrate below the membrane by backside etching. The conventional means to determine when to stop the etch process is to observe the color of the light transmitted through the sample, which is sensitive to the remaining Si thickness. However, most metallic films thicker than 75 nm are opaque, and there is no detectable color change prior to film perforation. In this paper, a back-etch method based on the observation of an abrupt change of optical reflection contrast is introduced as a means to determine the etch endpoint to prepare TEM samples for these films. As the acid etchant removes the Si substrate material a rough interface is generated. This interface becomes a relatively smooth and featureless region when the etchant reaches the membrane (film/SiO2). This featureless region is caused by the mirror reflection of the film plane (film/SiO2 interface) through the optically transparent SiO2 layer. The lower etch rate of SiO2 (compared with Si) gives the operator enough time to stop the etching without perforating the film. A clear view of the morphology and control of Si roughness during etching are critical to this method, which are discussed in detail. The procedures of mounting wax removal and sample rinsing are also described in detail, as during these steps damage to the membrane may easily occur without appropriate consideration. As examples, the preparation of 100-nm-thick Fe-based amorphous alloy thin film and 160-nm-thick Cu-thin film samples for TEM imaging is described.