纳米级长度扫描电镜测量的现状和展望

1前言 “纳米科技”是20世纪80年代末快速崛起的一门新兴学科,由于它的发展前景广阔,实用价值较大,引起了世界各国的重视,成为科技界争相研究的领域。我国政府和科研机构都积极支持和发展纳米科技。     

微米、纳米尺度测量环境的温度测量和控制技术

真空法和空调法是精密测量环境温度高稳定度和均匀度的主要构建方法.讨论了多热源温场控制的解耦问题,考虑到空气温度控制模型的复杂性和非精确性,依靠先验知识的不完全解耦方法仍将在工程应用中居于主流地位.高精度温度测量一般依赖于测量精度高的铂电阻等温度传感器完成,但自然对流条件下的空气流动性差,应考虑热电阻工作中的自热现象.热电偶和石英温度传感器可能是该条件下温度测量的一种可考虑的选择.     

扫描电镜测量微米级长度的不确定度评定

对扫描电镜测量微米级长度的不确定度进行了评定。对引起不确定度性的许多因素，如扫描电镜的分辨率、测量的重复性以及标尺的标定误差等作了分析和计算，特别对输入变量相关时的合成问题作了研究。最后得到了S-4200型扫描电镜微米级测量长度的不确定度。     

纳米尺度线宽的测量与Nano1国际关键比对

现代集成电路制造业、数据存储工业和微机电系统等行业的不断发展,对纳米尺度线宽的测量提出了越来越高的要求.目前的一些测量方法分别存在各自的缺点与不足,在缺少更高准确度计量标准的情况下,往往采用比对的方法使计量结果趋于一致.国际计量局在1998年把纳米尺度线宽计量确定为纳米尺度基本特征国际关键比对项目之一.文章对它的主要研究内容以及进展情况作了介绍.     

论纳米光栅测量技术

作者及其同事们经过20多年努力将计量光栅技术提高到了纳米量级和亚纳米量级，并进行了大面积推广应用，形成了一整套纳米光栅测量技术，该文为对这套技术的综合论述．首先回顾了刻线技术的发展历史，指出中国古代曾作出杰出贡献．归纳了发展计量光栅技术的5个阶段和4项内容．给出纳米光栅的定义和两个特点，并通过作者和同事们的光栅制造过程说明，纳米光栅实质上是一种刻录、固化到光栅基体上的光波波长．它为纳米测量领域提供了一种新途径、新方法，与激光干涉仪等现有纳米测量方法相比，具有自己独特的优点．文中讨论了纳米光栅的读取技术与信号处理技术，提出了纳米光栅细分误差的错位测量法．还讨论了与纳米光栅相关的纳米机械，介绍了作者和同事们的科研成果，圆柱、导轨等的机械精度已经进入了纳米量级．最后讨论了纳米光栅与激光干涉仪以及高等级量块的比对结果．     

纳米制造和测量技术产业化的研究

从加工尺度的连续性和加工技术的完整性这一新的角度,分析了纳米加工产业化面临的问题,并提出了相应的解决方案一多离子柬聚焦投影技术。多离子柬聚焦投影技术将填补传统微机加工技术和半导体图形技术之间0．5～5μm的加工空白,并会在1～100nm尺度间实现自上至下技术和自下至上技术的有机结合。纳米测量技术产业化的研究中,以提高扫描探针技术的样品质量作为出发点。在聚焦离子束和扫描电镜平台上集成Ar离子束的“三束”显微镜能有效降低样品的损伤,大大推动了纳米测量技术的发展。     

微纳米尺寸测量技术

随着精密和超精密加工技术的迅速发展,亚微米和纳米级的测量方法不断出现,本文对近年几种常见的微纳米计量技术的基本测量原理和方法作了简单的介绍。     

纳米粉末样品制备方法对扫描电镜成像的影响

制备出分散良好的电镜样品对准确观察纳米粉末的形貌和尺寸尤为重要.以导电类铂和不导电类钒酸钇纳米粉末为研究对象,分别采用直接固定法和铜网碳载膜固定法制备样品,并对比这两种方法对扫描电镜成像的影响.结果表明:采用铜网碳载膜固定制备法可以有效改善纳米粉末样品的分散性,杜绝纳米颗粒与导电胶发生溶合,易获得纳米粉末样品扫描电镜真实像,明显提高扫描电镜观察的准确性和检测效率.     

纳米尺度线宽的测量与Nanol国际关键比对

现代集成电路制造业、数据存储工业和微机电系统等行业的不断发展，对纳米尺度线宽的测量提出了越来越高的要求。目前的一些测量方法分别存在各自的缺点与不足，在缺少更高准确度计量标准的情况下，往往采用比对的方法使计量结果趋于一致。国际计量局在1998年把纳米尺度线宽计量确定为纳米尺度基本特征国际关键比对项目之一。文章对它的主要研究内容以及进展情况作了介绍。     

小型微纳米图形电子束曝光制作系统(英文)

为了满足科学实验过程中对制作半导体器件和微纳米结构的需要,同时避免受到昂贵的工业级电子束曝光(electron beam lithography,EBL)机的条件制约,构建了一种基于普通扫描电子显微镜(scanning electron microsco-py,SEM)的桌面级小型电子束曝光系统.建立了以浮点DSP为控制核心的高速图形发生器硬件系统.利用线性计算方法实现了电子束曝光场的增益、旋转和位移的校正算法.在本曝光系统中应用了新型压电陶瓷电机驱动的精密位移台来实现纳米级定位.利用此位移台所具有的纳米定位能力,采用标记追逐法实现了电子束曝光场尺寸和形状的校准.电子束曝光实验结果表明,场拼接及套刻精度误差小于100 nm.为了测试曝光分辨率,在PMMA抗蚀剂上完成了宽度为30 nm的密集线条曝光实验.利用此系统,在负胶SU8和双层PMMA胶表面进行了曝光实验;并通过电子束拼接和套刻工艺实现了氮化物相变存储器微电极的电子束曝光工艺.     

SEM/EDS分析纳米TiN颗粒在SiC陶瓷中的分布状况

采用水基喷雾造粒技术制备SiC/纳米TiN复合粉体,并借助二步成型和无压烧结技术制备SiC/纳米TiN复合陶瓷,利用场发射扫描电镜结合能谱分析(SEM/EDS)研究了纳米TiN颗粒在SiC/纳米TiN复合粉体、素坯及烧结体过程中的分布状态,借此评价制备工艺。     

Optimisation of secondary electron detector for variable pressure SEM with Monte Carlo method

A computer programme for numerical modelling of electron flow in vacuum instruments is presented. The programme allows to simulate trajectories of charged particles in both high and low vacuum of the order of tens milibars. It combines a commercially available packet SIMION 3D v.7.0 destined for tracing trajectories of charged particles in electric and magnetic fields, and a Monte Carlo programme modelling phenomena accompanying electron collisions with gas molecules. The programme was applied for analysis and optimisation of a novel secondary electron detector for a variable-pressure scanning electron microscopy.     

Hydrogen-acetylene gas ratio and catalyst thickness effect on the growth of uniform layer of carbon nanotubes

Effect of catalyst thickness (2, 4, and 6 nm) and acetylene-hydrogen gas ratio (1/4, 2/4, and 3/4) on the synthesis of carbon nanotubes is reported in this article. Synthesized nanotubes are characterized by X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy, and Raman effect. From SEM results, nanotubes growth is less for higher thickness, as at higher thickness catalyst nanoparticles agglomerate which suppress the growth of nanotubes. Raman spectroscopy results reveal that at higher thickness defects density increases. Nanotube of better crystallinity and graphitic outer walls grows for lower acetylene-hydrogen gas ratio and at smaller thickness of catalyst layer. The sheet resistance of carbon nanotube thin film is measured by using Hall effect measurement systems. Smallest sheet resistance among synthesized multi-walled carbon nanotubes sample is obtained for nanotubes grown on 2 nm thick catalyst film and is 0.9 kΩ/square.     

Effect of Cu on Microstructures of Manganese Steel by EDXA and SEM

In order to investigate the distribution of Cu and Mg, and the effect of Cu on the microstructure of steels, manganese steels containing various Cu contents were annealed at 1260, 1100 and 1000℃, respectively, for I h and subsequently cooled to room temperature in the furnace to simulate the pre-rolling anneal. The results indicate that Cu is not microscopically segregated in the annealed steels. The scanning electron microscopy （SEM） observation shows that the main microstructure consist of ferrite and pearlite; the percentage of pearlite in the steels increases with increasing Cu content. The grain size reduces with the decrease of the annealing temperature. The results of energy dispersive X-ray analysis （EDXA） suggest that Cu content in pearlite is higher than that in ferrite, demonstrating that the microstructure-segregation of Cu occurred. However, the cast specimens show that Cu content in MnS and S-rich phases is high. In addition, Cu of 0.2%-0.4% could improve the distribution of MnS and S-rich inclusions. The optimal Cu content in steels and the optimal annealing temperature between 1100-1200℃ were determined.     

基于AFM的纳米级表面加工中切屑形成的影响因素

以原子力显微镜（AFM）为加工工具进行了纳米级加工实验,对不同加工条件下的材料去除过程和切屑形态进行了研究．切屑形态通过扫描电子显微镜（SEM）进行观察,分析了不同垂直载荷、循环次数和针尖加工方向下铝铜被加工表面的切屑形成过程．实验结果表明：低栽下切屑呈细小断屑,散布在加工区域周围;随着垂直载荷的增加,切屑逐渐变成连续的带状切屑．不同循环次数、针尖加工面时切屑形成都有很大影响．在此基础上,对比分析了相同实验条件下,不同力学性能材料的切屑形成过程．最后,通过检测被加工表面得出被加工表面质量与切屑的数量和形态之间的关系,提出了改善被加工表面质量的方法,以帮助人们更好地理解基于AFM的纳米级加工技术．     

Influence of Cl-, Br-, NO 3 - and SO 4 2- ions on the corrosion behaviour of 6061 Al alloy

The effects of anions like Cl^-, Br^-, NO ₃ ^- and SO ₄ ^2- on the anodic dissolution of the monolithic Al 6061 alloy have been investigated at neutral pH through immersion testing and electrochemical techniques like potentiodynamic polarization and a.c. impedance spectroscopy. Scanning electron microscopy was employed to characterize the corroded surface and to observe the extent of pitting in different media. From the evaluated corrosion parameters it was found that the dissolution of the matrix was extensively reduced in presence of aqueous solutions containing Br^-, NO ₃ ^- and SO ₄ ^2- ions while Cl^- ions aggravated corrosion by penetrating into the barrier oxide film on the surface of the material. Pronounced effect of pitting was observed in presence of Cl^- and the level of pitting in NO ₃ ^- and Br^- were mild. In presence of SO ₄ ^2- ions passivity was extended over a wide potential range and breakdown of passivity occurs when the material was polarized beyond pitting potential. The departure of capacitive behaviour towards resistive behaviour was clearly observed through impedance measurements when investigations were conducted in Cl^- media and in presence of the other electrolytes. Corrosion rates were, however, controlled during prolonged exposure in the electrolytic media, specially in case of chloride media, due to the predominance of film repair kinetics.     

扫描探针显微镜下微纳结构深度测量的校准方法

扫描探针显微镜(SPM)是微纳结构三维测量中的一项重要技术。然而,在测量过程中台阶或沟槽样品的边缘附近会出现不准确的轮廓,这就造成了深度测量的精度损失。为了避免深度测量的精度损失,分别建立了机械探针和光学探针的两个分析模型,描述了不准确轮廓、样品深度和探针形状之间的耦合关系;在此基础上,提出了一种具有良好精度的深度测量标定方法。与现有的国际深度测量标准(W/3规则)进行比较,该方法提供了一个明确的边界来确定测量结果是否有效;此外,它还可以指导用户在执行测量之前选择适当的探针。     

Enhanced field emission characteristics of nitrogen-doped carbon nanotube films grown by microwave plasma enhanced chemical vapor deposition process

Nitrogen-doped carbon nanotube (CNT) films have been synthesized by simple microwave plasma enhanced chemical vapor deposition technique. The morphology and structures were investigated by scanning electron microscopy and high resolution transmission electron microscopy. Morphology of the films was found to be greatly affected by the nature of the substrates. Vertically aligned CNTs were observed on mirror polished Si substrates. On the other hand, randomly oriented flower like morphology of CNTs was found on mechanically polished ones. All the CNTs were found to have bamboo structure with very sharp tips. These films showed very good field emission characteristics with threshold field in the range of 2.65-3.55 V/μm. CNT film with flower like morphology showed lower threshold field as compared to vertically aligned structures. Open graphite edges on the side surface of the bamboo-shaped CNT are suggested to enhance the field emission characteristics which may act as additional emission sites.