High-voltage nano-oxidation in deionized water and atmospheric environments by atomic force microscopy

This study used atomic force microscopy (AFM), metallic probes with a nanoscale tip, and high-voltage generators to investigate the feasibility of high-voltage nano-oxidation processing in deionized water (DI water) and atmospheric environments. Researchers used a combination of wire-cutting and electrochemical etching to transform a 20-μm-thick stainless steel sheet into a conductive metallic AFM probe with a tip radius of 60 nm, capable of withstanding high voltages. The combination of AFM, high-voltage generators, and nanoscale metallic probes enabled nano-oxidation processing at 200 V in DI water environments, producing oxides up to 66.6 nm in height and 467.03 nm in width. Oxides produced through high-voltage nano-oxidation in atmospheric environments were 117.29 nm in height and 551.28 nm in width, considerably exceeding the dimensions of those produced in DI water. An increase in the applied bias voltage led to an apparent logarithmic increase in the height of the oxide dots in the range of 200-400 V. The performance of the proposed high-voltage nano-oxidation technique was relatively high with seamless integration between the AFM machine and the metallic probe fabricated in this study.     

Tip radius effect of AFM probe on K4Nb6O17·3H2O nanosheets groove machining accuracy

This paper presents a technique for groove machining of potassium niobate nanosheets using an atomic force microscope (AFM). Groove machining operations are performed using super sharp silicon (SSS) probes. The tip radius of these probes is less than 5 nm and is one-third that of a conventional silicon (Si) probe. The results obtained using these probes are compared with those obtained using a Si probe, in order to examine the tip radius effects of the AFM probe on groove machining accuracy, i.e., coarseness of the machined groove. These results show that the degree of coarseness of the machined groove for varying machining loads with the SSS probe was much worse than that with the Si probe. Thus, groove machining with the SSS probe was more difficult to control with varying machining loads. We propose a groove fabrication model that considers the stochastic energy and difference in tip radius of the AFM probe. Using our groove fabrication model, changes in the coarseness of the machined groove for varying machining loads can be predicted.     

Simulation-aided design and fabrication of nanoprobes for scanning probe microscopy

We proposed and demonstrated a flexible and effective method to design and fabricate scanning probes for atomic force microscopy applications. Computer simulations were adopted to evaluate design specifications and desired performance of atomic force microscope (AFM) probes; the fabrication processes were guided by feedback from simulation results. Through design-simulation-fabrication iterations, tipless cantilevers and tapping mode probes were successfully made with errors as low as 2% in designed resonant frequencies. For tapping mode probes, the probe tip apex achieved a 10 nm radius of curvature without additional sharpening steps; tilt-compensated probes were also fabricated for better scanning performance. This method provides AFM users improved probe quality and practical guidelines for customized probes, which can support the development of novel scanning probe microscopy (SPM) applications.     

Analysis of simulated scanning of atomic-scale silicon surface by atomic force microscopy

This study constructs a contact-mode atomic force microscopy (AFM) simulation measurement model with constant force mode to simulate and analyze the outline scanning measurement by AFM. The simulation method is that when the probe passes the surface of sample, the action force of the atom of sample received by the atom of the probe can be calculated by using Morse potential. Through calculation, the equivalent force on the cantilever of probe can be acquired. By using the deflection angle equation for the cantilever of probe developed and inferred by this study, the deflection angle of receiving action force can be calculated. On the measurement point, as the deflection angle reaches a fixed deflection angle, the scan height of this simulation model can be acquired. By scanning in the right order, the scan curve of the simulation model can be obtained. By using this simulation measurement model, this study simulates and analyzes the scanning of atomic-scale surface outline. Meanwhile, focusing on the tip radii of different probes, the concept of sensitivity analysis is employed to investigate the effects of the tip radius of probe on the atomic-scale surface outline. As a result, it is found from the simulation on the atomic-scale surface that within the simulation scope of this study, when the tip radius of probe is greater than 12 nm, the effects of single atom on the scan curve of AFM can be better decreased or eliminated.     

Improvement of Local Surface Quality by Using Single Abrasive Abrasion Process

AFM-based wear process actually is single abrasive abrasion process. It is widely employed in the surface micro/nano machining for fabrication of structures at the nanometer scale exhibiting high removing ability of nanometer scale materials. In this study, application of AFM-based single abrasive abrasion process in the local surface quality (surface roughness) improvement was studied. Merged holes were fabricated using an AFM diamond tip with different wear parameters on the surface of germanium (Ge) machined by conventional ultra-precision diamond turning. Results showed that cracks left by diamond turning can be removed and the local surface quality can be improved. Also effects of the wear parameters on the surface roughness were investigated. The optimized parameters of the abrasion process for improving the surface quality were provided. It is verified that AFM-based single abrasive abrasion process is a novel approach to modify or repair local surface on the surface of parts manufactured by other methods.     

Fundamental Investigation of the Wear Progression of Silicon Atomic Force Microscope Probes

Atomic force microscopy (AFM) is a key instrument in nanotechnology; however, AFM probe wear is a critical concern with AFM-based technologies. In this work, the wear progression of silicon AFM probes with different radii was thoroughly explored under various normal forces and sliding speeds. The results showed that the initial wear coefficient increased as the normal force increased. However, after a certain sliding distance, the wear coefficient was stable due to the flattening of the probe even with increasing normal force. It was also observed that the wear coefficient decreased with increasing probe radius and the wear of the probe increased as the sliding speed increased. From the overall results, it was concluded that the contact pressure plays a significant role in wear progression and may be responsible for a lower wear coefficient even with increasing adhesion forces due to wear. The wear rate was found to have an exponential dependence on contact stress, as proposed in recent literatures.     

High-resolution constant-height imaging with apertured silicon cantilever probes

We present high-resolution aperture probes based on non-contact silicon atomic force microscopy (AFM) cantilevers for simultaneous AFM and near-infrared scanning near-field optical microscopy (SNOM). For use in near-field optical microscopy, conventional AFM cantilevers are modified by covering their tip side with an opaque aluminium layer. To fabricate an aperture, this metal layer is opened at the end of the polyhedral probe using focused ion beams (FIB). Here we show that apertures of less than 50 nm can be obtained using this technique, which actually yield a resolution of about 50 nm, corresponding to λ/20 at the wavelength used. To exclude artefacts induced by distance control, we work in constant-height mode. Our attention is particularly focused on the distance dependence of resolution and to the influence of slight cantilever bending on the optical images when scanning at such low scan heights, where first small attractive forces exerted on the cantilever become detectable.     

基于AFM的化学机械抛光磨粒模拟研究

当前的化学机械抛光(CMP)磨损模型中大多数都缺少微观试验数据的支持。为进步揭示CMP中纳米磨粒对材料表面的磨损机制,提出了采用原子力显微镜(AFM)来模拟CMP中的单个磨粒的试验方案,并验证该模拟试验方案的可行性。结果表明:采用AFM探针来模拟CMP过程中单个磨粒对芯片表面的磨损与相互作用的试验方案是完全可行的;可以通过AFM探针对芯片表面的相互作用与磨损,模拟得出单个磨粒对芯片表面的作用与磨损状况,并可以在此微观试验数据的基础上建立起新的CMP磨损模型。     

Surface modification of AFM silicon probes for adhesion and wear reduction

Tip wear of silicon probes used for an atomic force microscope (AFM) is a critical issue. Wear can result in an increase of tip radius and adhesion between tip and sample, thus reducing the image resolution and introducing artifacts. In order to reduce adhesion, friction, and wear so as to reduce tip related artifacts, liquid lubricant (Z-TETRAOL), self-assembled monolayers (pentafluorophenyltriethoxysilane (PFPTES)), and fluorocarbon polymer (Fluorinert™) were applied on the silicon probe. A comprehensive investigation of adhesion, friction, and wear of the uncoated/coated tips in both ambient air and various humidity levels as well as the influence of the coatings on the image resolution was performed. Experiments showed that the coatings reduced the adhesion, friction, and wear of the silicon tip, improved the initial image resolution, and exhibited less deterioration as compared to that of uncoated tip in the long-term test.     

掩模偏转方向对硅尖形状影响的研究

为制备高纵横比的纳米硅尖,研究了掩模的偏转方向对硅尖形状的影响。设计了硅尖制备的工艺流程,采用KOH溶液湿法各向异性腐蚀制备硅尖,将实验和{411}晶面模型相结合,分析了硅尖的成型机理,讨论了掩模偏转方向对硅尖形状的影响,得到制备高纵横比纳米硅尖的工艺参数。实验结果表明：硅尖侧壁是由与(100)面夹角为76.37°的{411}晶面组成;利用正方形掩模的偏转,可以制备出八面体和四面体的硅尖。当正方形掩模边缘沿<110>晶向时,在78℃、浓度40%的KOH溶液中腐蚀的硅尖,经980℃氧化削尖,可以得纵横比大于2的八面体纳米硅尖阵列。     

Effects of scratching directions on AFM-based abrasive abrasion process

AFM-based single abrasive abrasion process is widely employed in the surface micro/nanomachining for fabrication of structures at the nanometer scale. The wear depth and roughness are significantly important in the application of these structures. To study effects of scratching directions on the wear depth and roughness within the wear mark, single groove scratching test and wear test on the surface of polished single crystal silicon were carried out using AFM with a pyramidal diamond tip. Single groove scratching tests indicated that tip geometry leads to different removal states such as cutting and plowing. At the same load, deeper wear depth and rougher surface were produced by using the scratching direction perpendicular to the long axis of the cantilever rather than parallel to the long axis of the cantilever. Surface roughness decreases with respect to the feed scratching perpendicular to the long axis of the cantilever, whereas while scratching along the long axis of the cantilever, the surface roughness is rougher at the small feed. This is attributed to the different stiffness of the cantilever along different scratching directions and different removal states between the tip and sample.     

AFM变载荷刻划硅基底的分子动力学研究

基于改进的分子动力学模型,研究了原子力显微镜(AFM)探针在硅表面变载荷刻划的形变特性。利用结构辨认算法显示非晶层的形成,并建立切屑分布的定量评价指标。在此基础上考察刻划速度、针尖半径和探针锥角对刻划效果的影响。结果表明:(1)当刻划速度小于0.3 nm/ps或大于等于1.5 nm/ps时,基底表面的切屑较少,刻划速度对沟槽表面的影响不大;(2)当针尖半径小于等于1 nm时,探针会发生磨损,当针尖半径大于等于1.5 nm时,探针发生弹性形变,针尖半径为2~3.5 nm能达到最佳刻划效果;(3)较大的锥角有利于减少基底表面的切屑分布。     

Direct deformation study of AFM probe tips modified by hydrophobic alkylsilane self-assembled monolayers

The in-use wear of atomic force microscopy (AFM) probe tips is crucial for the reliability of AFM measurements. Increase of tip size for several nanometers is difficult to monitor but it can already taint subsequent AFM data. We have developed a method to study the shape evolution of AFM probe tips in nanometer scale. This approach provides direct comparison of probe shape profiles, and thus can help in evaluation of the level of tip damage and quality of acquired AFM data. Consequently, the shape degradation of probes modified by hydrophobic alkylsilane self-assembled monolayers (SAMs) was studied. The tip wear length and wear volume were adopted to quantitatively verify the effectiveness of hydrophobic coatings. When compared with their silicon counterparts, probes modified by SAM materials exhibit superior wear-resistant behavior in tapping mode scans.     

基于单片机的AFM纳米机械性能测试系统

摘要：目的：为解决采用AFM系统进行纳米机械性能测试中存在的不能够直接获得载荷——压深曲线以及不能够随意改变加载、保载、卸载时间等问题,对AFM系统进行改造。方法：开发了一套基于单片机的信号输入输出模块。将该模块与AFM控制系统相联,形成新的纳米机械性能测试系统。结果：该系统可以实现动态改变垂直载荷,并依据相应算法,可以实现载荷——压深曲线的实时获得。通过单片机设置模拟信号的输出速率可以实现加载、保载和卸载速率的改变。并结合二维微动精密工作台,可以实现较大范围内点阵的压痕测试。结论：通过在聚碳酸酯、聚二甲基硅氧烷等材料表面进行试验测试表明：该系统可以进行高速高精度的测量样品的纳米机械性能参数,包括对样品进行纳米压痕测试和对样品的纯弹性变形过程进行检测如聚二甲基硅氧烷或者各种微梁等微小构件。     

Imaging and nano-dissection of tobacco mosaic virus by atomic force microscopy

Tobacco mosaic virus (TMV) has been deposited on freshly cleaved mica substrates. The topography was investigated by contact, non-contact and lateral-force microscopy under ambient conditions in air. The results were in accord with known dimensions of TMV (i.e. 18 nm in diameter and 300 nm in length). However, convolution of tip shape with TMV morphology resulted in an apparent width of 80–140 nm in the lateral plane, a factor of 4–7 greater than the known diameter. Other artefacts - broadening and double images - were observed and ascribed to tip anomalies. High force loadings and slow repetitive scanning resulted in controlled removal of parts of the TMV structure. Accordingly, it was possible to reveal and image the central core channel of the TMV. The precision and resolution of dissection induced by AFM is currently limited by the shape of the tip, having a 40-nm radius of curvature for standard Si₃N₄ tips. It is estimated that sharper tips, with a radius of curvature of less than 10 nm, should be able to resolve, non-destructively, the protein subunits in the non-contact mode, and selectively remove single subunits in the contact mode.     

Nano-mechanical and tribological characteristics of ultra-thin amorphous carbon film investigated by afm

The mechanical as well as tribological characteristics of coating films as thin as a few nm become more crucial as applications in micro-systems grow. Especially, the amorphous carbon film has a potential to be used as a protective layer for micro-systems. In this work, quantitative evaluation of nano-indentation, scratching, and wear tests were performed on the 7nm thick amorphous carbon film using an Atomic Force Microscope (AFM). It was shown that AFM-based nano-indentation using a diamond coated tip can be feasibly utilized for mechanical characterization of ultra-thin films. Also, it was found that the critical load where the failure of the carbon film occurred was about 18μN by the ramp load scratch test. Finally, the wear experimental results showed that the quantitative wear rate of the carbon film ranged 10^-9~10^-8 mm³/N cycle. These experimental methods can be effectively utilized for a better understanding the mechanical and tribological characteristics at the nano-scale.     

In situ metal tip sharpening of scanning probe microscopes

This article demonstrated a new approach for fabrication and sharpening of metal tips of scanning probe microscopes. Experimentally, a metal tip was heated and melted by a focused laser light. The tip was then sharpened by a strong electric field and consolidated as the laser was turned off. With a low‐vacuum and a high‐voltage source, a 25‐µm indium‐coated platinum wire was sharpened to a tip with diameters below 50 nm. The minimal tip radius by this method is estimated to be below 1 nm. With this technique, in situ tip sharpening for SPM would be possible. SCANNING 34: 76–79, 2012. © 2011 Wiley Periodicals, Inc.     

湿式机械化学磨削单晶硅的软磨料砂轮及其磨削性能

针对干式机械化学磨削(Mechanical chemical grinding, MCG)单晶硅过程中易产生磨削烧伤、粉尘多、加工环境差等问题,研制一种可用于湿式MCG单晶硅的新型软磨料砂轮,并对砂轮的磨削性能及其磨削单晶硅的材料去除机理进行研究。根据湿式机械化学磨削单晶硅的加工原理和要求,制备出以二氧化硅为磨料、改性耐水树脂为结合剂的新型软磨料砂轮。采用研制的软磨料砂轮对单晶硅进行磨削试验,通过检测加工硅片的表面/亚表面质量对湿式MCG软磨料砂轮的磨削性能进行分析,并与传统金刚石砂轮、干式MCG软磨料砂轮的磨削性能进行对比。采用X射线光电子能谱仪对磨削前后硅片的表面成分进行检测,分析湿式MCG加工硅片过程中发生的化学反应。结果表明,采用湿式MCG软磨料砂轮加工硅片的表面粗糙度Ra值为0.98 nm,亚表面损伤层深度为15 nm,湿式MCG软磨料砂轮磨削硅片的表面/亚表面质量远优于传统金刚石砂轮,达到干式MCG软磨料砂轮的加工效果,可实现湿磨工况下硅片的低损伤磨削加工。在湿式MCG过程中,单晶硅、二氧化硅磨粒与水发生了化学反应,在硅片表面生成易于去除的硅酸化合物,硅酸化合物进一步通过砂...     

散射式太赫兹扫描近场光学显微技术研究

基于散射式近场探测原理,设计并搭建了散射式太赫兹扫描近场光学显微系统(THz s-SNOM),实现了纳米量级空间分辨率的太赫兹近场显微成像测量。该系统以输出频率范围为0.1~0.3THz的太赫兹倍频模块为发射源,通过纳米探针的针尖产生纳米光源与样品相互作用,并将样品表面的倏逝波转化为可在远场测量的辐射波。通过探针逐点扫描样品表面,同时获得了样品表面的形貌图和太赫兹近场显微图。该系统的显微分辨率取决于探针针尖的曲率半径,而与太赫兹波的波长无关。使用该系统测量了金薄膜/硅衬底样品和石墨烯样品的近场显微图,结果表明,近场显微的空间分辨率优于60nm,波长与空间分辨率之比高达λ/26000。     

基于原子力显微镜的线宽粗糙度测量

给出采用原子力显微镜(Atomic force microscope,AFM)测量线宽粗糙度(Line width roughness,LWR)的分析步骤。分析线宽和LWR及其偏差随刻线横截面位置的高度变化的关系,线宽及其偏差和LWR及其偏差随刻线横截面位置的高度值增加而减小。分别采用四种边缘提取算子提取了碳纳米管针尖AFM测量的刻线顶部线宽边缘,计算了刻线顶部线宽和LWR,顶部线宽和LWR测量结果对边缘提取算子不敏感。结合被测单晶硅台阶的顶表面和底表面加工方法,提出采用各扫描线轮廓高度相等的方法校正AFM压电驱动器的z向非线性。比较了采用普通氮化硅探针针尖、超尖针尖以及碳纳米管针尖AFM测量名义线宽为1 000 nm刻线LWR的结果,显示采用三种针尖的LWR测量结果存在差异,但考虑到AFM分辨率,可认为测量结果基本相同。因此,为更精确描述刻线边缘,必须提高AFM分辨率。