"楔形"TEM样品的机械研磨制备技术

介绍了一种用机械研磨法制备集成电路TEM楔形样品的技术,讨论了该制样技术所需注意的关键点,并给出了判断样品薄区是否满足TEM分析要求的两种方法。楔形样品减薄技术兼具制样速度快和样品质量好的优点。该技术既可用于制备非定点TEM样品,也可用于制备定点的TEM样品。给出了用该技术制备的定点失效的MOS器件TEM照片。熟练的技术人员可以用此方法在半小时内完成一个样品的制备。     

FinFET芯片TEM样品制备及避免窗帘效应方法

制备高质量纳米尺度芯片透射电子显微镜(TEM)样品对于探索半导体器件结构设计、材料分布与芯片性能之间的关系具有重要的意义。使用聚焦离子束(FIB)/扫描电子显微镜(SEM)双束系统制备14 nm鳍式场效应晶体管(FinFET)截面TEM样品,制备过程中从技术角度提出了两种自下而上制样方案来抑制窗帘效应。为扩大样品的可表征视场范围,在避免样品弯曲的前提下,提出了一种薄片提取方法。结果表明,离子束流越大,窗帘效应越严重,自下而上方法能有效规避窗帘效应;离子束电压30 kV时采用清洗截面(CCS)模式、5 kV/2 kV时采用矩形模式,样品台倾斜补偿角度为1.5°～3.5°,进行交叉减薄,且最终铣削长度控制在1μm时减薄效果最好;新的薄片提取方法改变了样品的铣削方向,在避免窗帘效应破坏感兴趣结构和样品弯曲的前提下,将样品的可表征视场范围扩大了5倍。研究结果对优化TEM样品制备方法以及芯片失效分析提供了参考。     

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.     

薄膜的截面TEM样品制备

薄膜材料的厚度仅为微米量级或者更薄，对其微结构的研究十分困难，许多表征方法难以采用。透射电子显微分析（TEM）是薄膜材料微结构研究最重要的手段之一。尽管采用TEM平面样品研究薄膜的微结构在样品制备方面相对容易，但由于薄膜依附于基材生长，且通常具有择优取向和柱状晶生长等微结构特征，因而采用截面样品从薄膜生长的横断面进行观察和研究，可以得到更多的材料微结构信息。但是薄膜的TEM截面样品制备过程较为繁杂，难以掌握。已有的文献主要介绍了Si基片上生长薄膜的TEM截面样品制备方法，对金属基片薄膜截面样品的制备方法介绍不多。     

铌的透射电子显微镜样品的制备技术

一种新的大面积TEM样品制备技术——背面防护漂浮减薄法,已在原始厚度约为半微米的共蒸Nb_3Ge薄膜和扩散Nb_3Sn薄膜上,成功地制备出大面积TEM样品。本文报导,将这种方法应用于原始厚度约为15微米的Nb箔,同样也能够制备出大面积TEM样品。这种TEM制样技术不需要复杂的减薄装置或设备,方法简便,易于掌握。预期可在原始厚度约为几十微米的其它样品上,推广使用。     

电镀包埋制备可减薄粉末样品的研究

为了获取更多的粉末颗粒样品内部结构细节信息 ,需要对其进行减薄 ,但常规的由块状样品制备薄膜的方法[1] ,不能解决粉末颗粒的减薄问题。而采用电镀方法[2 ] ,使粉末包埋在金属膜中 ,则是一种可行的方案。本文采用一种电镀包埋法制备ＴＥＭ薄膜样品 ,得到满意的效果。实验方法1 若粉末颗粒度较大 ,则先用玛瑙研钵研磨一下 ,使颗粒的平均粒度达到 30 μｍ左右即可。以乙醇作分散介质均匀分散已处理的微颗粒试样 ,然后滴到事先已清洗干净的金属Ｎｉ片上。待分散介质挥发至半干时 ,Ｎｉ片连同样品水平放置在电镀槽底作阴极。2 配制以下成分的…     

NiSi_2外延单晶薄膜TEM分析样品的制备方法——两步局部化学减薄法

由于自身的特点,通常制备供TEM分析用超薄样品的方法,不适合于NISi_2外延单晶薄膜.为此,提出了一种新的适合于NiSi_2外延单晶薄膜TEM分析样品的制备方法——两步局部化学减薄法.这一方法也适用于制备硅薄膜的TEM分析样品.     

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。     

非晶层占比对TEM样品成像的影响

研究了非晶层占比对半导体器件透射电子显微镜(TEM)样品成像的影响。聚焦离子束(FIB)是制备TEM样品的重要工具,在TEM样品制备过程中,离子束损伤会在样品表面产生非晶层而使TEM图像产生畸变失真。在28 nm技术节点以下半导体器件TEM样品制备中,传统的制备方法会使样品在TEM下呈现非晶像或者图像质量不佳而不再适用。制备了一种楔形样品并使用平面转截面的样品制备方法研究了TEM呈晶格像时和非晶层临界占比的关系。实验表明,当样品中非晶层的占比超过0.66时,其在TEM下的成像为非晶像;当低于这一数值时,其在TEM下的成像为晶格像。针对非晶层对样品成像的影响,使用了一种低电压减薄的制备方法,通过降低非晶层占比可以显著优化表面成像,提高TEM样品的质量。     

矿物材料TEM样品的几种制备方法

矿物材料的TEM样品制备历来是个难题，采用常规方法成功率很低，限制了TEM在矿物研究中的应用。以下探索出的几种矿物材料TEM样品制备方法，希望能对扩展TEM在矿物研究中的应用有所帮助。     

A high-throughput approach for cross-sectional transmission electron microscopy sample preparation of thin films

Cross-sectional transmission electron microscopy (XTEM) is a very useful technique to study the interfacial diffusion and reactions and the grain growth of thin films. However, the preparation of XTEM samples of thin films is tedious and challenging. Difficulties may include the delamination of films from the substrate, fracture of brittle substrates and differential milling rates of the substrate and the film. This paper describes an improved technique using a combination of tripod polishing and focused ion beam milling to prepare XTEM samples of thin films. The technique can be widely used for high-throughput production of samples having varying film and substrate properties. Two different geometries are introduced. The first one is suitable for XTEM sample preparation of most films at a high yield rate, but with a limited view area. The other geometry is able to give a larger view area and is more suitable for thicker films. The technique is illustrated by an example of the sample preparation of Fe/Pt multilayer films on SiO2/Si substrates.     

飞秒脉冲激光沉积Si基a轴择优取向的钛酸铋铁电薄膜

在钛酸铋(Bi4Ti3O12)薄膜的制备过程中容易获得晶粒c轴垂直于基片表面的薄膜,而压电和铁电存储器主要利用a轴的自发极化分量,因而制备a轴择优取向的Bi4Ti3O12铁电薄膜具有特别的意义。采用飞秒脉冲激光作用在钛酸铋陶瓷靶上,采用Si(111)作为衬底,制备了a轴择优取向的钛酸铋薄膜。采用X射线衍射(XRD)的薄膜附件和场发射扫描电镜(FSEM)研究了薄膜的结构和形貌;采用傅里叶红外光谱仪测量了室温(20℃)下在石英基片上沉积的样品的光学特性;室温下沉积的钛酸铋薄膜呈c轴择优取向,晶粒的平均大小为20 nm,其光学禁带宽度约为1.0 eV。在500℃沉积的钛酸铋薄膜呈a轴择优取向,晶粒大小在30~300 nm之间,薄膜的剩余极化强度Pr为15μC/cm2,矫顽力Er为48 kV/cm。     

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.     

Principle and applications of an autocharge-compensated sample andhold circuit

This paper describes an autocharge-compensated sample and hold circuit (ACC-SH) for thin film transistor active matrix liquid-crystal displays (TFT-AM-LCD's, TFT-LCD's, or LCD's). The operating principle and actual application problems for TFT-LCD's are also discussed. The applicability of the ACC-SH is verified not only by circuit simulation but also by experimental circuit die measurement     

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.     

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.     

Preparation of Photoelectric Material--Pyrite(FeS_2) Thin Film

The preparation methods of simultaneous electro-deposition for pyrite (FeS2) thin film are introduced from aqueous solution of FeSO4 and Na2S2O3. Electrical process is studied in detail in the paper. From the experiment result, the best way of drying the sample is to dry it in vacuum. Electro-deposition method for the preparation of pyrite thin film is a safe, simple and low-cost method.     

Evaluation of scanning capacitance microscopy sample preparation by focused ion beam

Due to the continuous reduction of the critical dimensions of semiconductor devices, it becomes very important to know the two dimensional (2D) doping profile for electrical performance of devices. Scanning Capacitance Microscopy (SCM) is a powerful technique for qualitative analysis of 2D doping species distribution, measuring small capacitance variations with high spatial resolution. For 2D carrier profiling, the region of interest must be accessible to the profiling instrument. SCM samples require cross-sectioning to expose the inner sample at a visible surface. In some analysis, the failure is localized at a very accurate address up to hundreds of nanometers. With the traditional polishing method of sample preparation it is very difficult to reach the exact location. For this reason we are investigating a new way to prepare SCM sample with Focused Ion Beam (FIB) and plasma etch in order to accurately choose the scanning zone. This paper presents a method to obtain SCM scans after a sample preparation by FIB and the influence of the FIB and the Plasma etcher on cross-sectioned SCM samples.     

钢和铸铁的激光表面合金化研究

1.试验条件及方法 试样材料为45~#钢和高磷铸铁。高磷铸铁试样按空化腐蚀试验要求做成如图1所示的特殊试样。在试样表面采用火焰、等离子喷涂或手工涂层等方法喷涂一层厚为0.1～0.2mm厚的Ni基合金粉末,粉末成分见表1。