基于硅悬臂高阶谐振的动态原子力显微镜的快速扫描

利用原子力显微镜(AFM)硅悬臂器件具有多阶谐振模态的特性,提出了基于硅悬臂高阶谐振特性构建动态AFM来实现快速扫描的方法,并研制了可工作于一阶模态和高阶模态的AFM。介绍了高阶谐振AFM系统的基本结构和工作原理,从理论上证明了利用硅悬臂梁高阶谐振特性实现快速扫描的可行性。以自制的AFM为研究对象,分析了影响动态AFM扫描速度的主要因素,对系统各模块的响应时间进行了分析、测试,并通过实验证明了AFM在二阶谐振模态下的稳定时间明显小于一阶谐振模态下的稳定时间。最后,分别用一阶、二阶谐振模态对光栅试样在同一区域的表面形貌进行了扫描测试,测试数据表明:在相同条件下,AFM的扫描速度在二阶谐振模态下约是一阶模态下的3.3倍。理论分析和实验结果证明了利用高阶谐振探针提高AFM扫描速度的可行性和有效性。     

Dual frequency atomic force microscopy on charged surfaces

The cantilever is mechanically driven at two resonant frequencies in a bimodal atomic force microscope (AFM). To generate the feedback signal for topography measurement the deflection signal is demodulated at one frequency and for compositional surface mapping at the other. In particular, the second mode amplitude and phase signals are used to map surface forces such as the van der Waals interaction. On electrically charged surfaces both, van der Waals forces and electrostatic forces contribute to the second eigenmode signal. The higher eigenmode signal in bimodal AFM reflects the local distribution of electrical charges. Mechanically driven bimodal AFM thus also provides a valuable tool for compositional mapping based on surface charges.     

Analysis of dynamic cantilever behavior in tapping mode atomic force microscopy

Tapping mode atomic force microscopy (AFM) provides phase images in addition to height and amplitude images. Although the behavior of tapping mode AFM has been investigated using mathematical modeling, comprehensive understanding of the behavior of tapping mode AFM still poses a significant challenge to the AFM community, involving issues such as the correct interpretation of the phase images. In this paper, the cantilever's dynamic behavior in tapping mode AFM is studied through a three dimensional finite element method. The cantilever's dynamic displacement responses are firstly obtained via simulation under different tip‐sample separations, and for different tip‐sample interaction forces, such as elastic force, adhesion force, viscosity force, and the van der Waals force, which correspond to the cantilever's action upon various different representative computer‐generated test samples. Simulated results show that the dynamic cantilever displacement response can be divided into three zones: a free vibration zone, a transition zone, and a contact vibration zone. Phase trajectory, phase shift, transition time, pseudo stable amplitude, and frequency changes are then analyzed from the dynamic displacement responses that are obtained. Finally, experiments are carried out on a real AFM system to support the findings of the simulations. Microsc. Res. Tech. 78:935–946, 2015. © 2015 Wiley Periodicals, Inc.     

Scan speed limit in atomic force microscopy

The scan speed limit of atomic force microscopes has been calculated. It is determined by the spring constant of the cantilever k, its effective mass m, the damping constant D of the cantilever in the surrounding medium and the stiffness of the sample. Techniques to measure k, k/m and D/m are described. In liquids the damping constant and the effective mass of the cantilever increase. A consequence of this is that the transfer function always depends on the scan speed when imaging in liquids. The practical scan speed limit for atomic resolution in vacuum is 0·1 μm/s while in water it increases to about 2 μm/s due to the additional damping of cantilever movements. Sample stiffness or damping of cantilever movements by the sample increase these limits. For soft biological materials imaged in water at a desired resolution of 1 nm the scan speed should not exceed 2 μm/s.     

多模态动态原子力显微镜系统

动态原子力显微镜(atomic force microscope,AFM)是通过检测悬臂谐振状态的变化来对物体表面形貌进行测量的。通过对谐振状态的三种因素即振幅、相位、频率的检测,动态AFM可以分为三种工作模式,即振幅反馈、相位反馈与频率反馈模式,这三种反馈模式有着不同的扫描特点。基于硅悬臂具有高阶谐振的特性,动态原子力显微镜可以在悬臂工作于高阶谐振状态时对物体进行扫描。综合上述工作模式研制了一套多模态动态AFM,可以在三种反馈模式、不同阶谐振状态下对物体进行扫描测量。利用该系统在不同反馈模式、不同阶谐振状态下进行了扫描测试,结果显示,系统在各模式下具有亚纳米分辨力,其中在相位反馈模式,悬臂二阶谐振时可达到最优灵敏度与分辨力,分别为17.5V/μm和0.29nm,在最优灵敏度与分辨力状态下对光栅试样进行了三维扫描,得到光栅的三维形貌图。     

AFM纳米加工系统设计

利用自行研制原子力显微镜开发了一套纳米加工系统,系统利用软件预先读入图形,根据图形控制探针的精确走向,实现复杂图案的矢量式扫描刻蚀,并且对陶瓷管的非线性畸变实现了软件矫正,实验表明系统可加工出精细的纳米图形,为进一步加工出更为精细复杂的纳米器件奠定了基础。     

Scanning electron microscopy studies of protein-functionalized atomic force microscopy cantilever tips

Protein-functionalized atomic force microscopy (AFM) tips have been used to investigate the interaction of individual ligand-receptor complexes. Herein we present results from scanning electron microscopy (SEM) studies of protein-functionalized AFM cantilever tips. The goals of this study were (1) to examine the surface morphology of protein-coated AFM tips and (2) to determine the stability of the coated tips. Based on SEM images, we found that bovine serum albumin (BSA) in solution spontaneously adsorbed onto the surface of silicon nitride cantilevers, forming a uniform protein layer over the surface. Additional protein layers deposited over the initial BSA-coated surface did not significantly alter the surface morphology. However, we found that avidin-functionalized tips were contaminated with debris after a series of force measurements with biotinylated agarose beads. The bound debris presumably originated from the transfer of material from the agarose bead. This observation is consistent with the observed deterioration of functional activity as measured in ligand-receptor binding force experiments.     

Improved estimation of contact compliance via atomic force microscopy using a calibrated cantilever as a reference sample

A method to improve accuracy of surface compliance determination by atomic force microscopy is presented, based on using calibrated cantilevers as the reference samples. During each work session, a 1-D compliance map of a reference cantilever is calculated from force–indentation curves along its axis, by the standard ‘indentation mode’. An independent measurement of local compliance on the reference cantilever is obtained by 2-D imaging in constant deflection and using analytical equations based on its known geometry and material properties, called ‘imaging mode’. A re-mapping of the apparent (‘indentation mode’) to the true (‘imaging mode’) compliance is thus obtained, which is applied on ‘indentation mode’ measurements of an unknown sample. This method demonstrates correction in the right direction for a polystyrene plate and a Teflon foil reference samples. The method is then applied on an unknown sample of flat agarose gel patterned with spots of polylysine protein.     

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.     

Nanostructures in silicon investigated by atomic force microscopy and surface photovoltage spectroscopy

Surface photovoltage spectroscopy (SPS) and conductive atomic force microscopy (C-AFM) have been used for the characterization of nanocrystalline hydrogenated Si (nc-Si:H). This is a promising material both for silicon-based opto-electronics as well as for photovoltaic applications. Notwithstanding its interesting properties many issues regarding the material electronic and optical properties are not completely understood. The present contribution reports microscopic and spectroscopic analyses of nc-Si:H films grown for photovoltaic applications by low-energy plasma-enhanced chemical vapor deposition technique. Electronic levels associated with defect states were investigated by SPS, whereas the conduction mechanism at a microscopic level was investigated by C-AFM.     

基于AFM的微位移测量新方法研究

提出了一种测量物体微位移的新方法。原子力显微镜作为测量工具,样品和扫描器置于待测物体上,物体每移动一定距离就由AFM扫描获得一幅样品图像,由此获得一系列连续的序列图像。采用模板匹配方法检测相邻序列图像的偏移,从而可计算出物体的微位移。实验结果表明,用该方法还可实现物体二维方向的微位移测量,且精度达到纳米量级。     

Localized etching of silicon in water using a catalytically active platinum-coated atomic force microscopy probe

This paper presents a novel atomic force microscopy (AFM)-based nanofabrication technique for Si in water that is based on highly localized catalytic etching with a Pt-coated AFM probe. It has been shown that nanoscale grooves can be fabricated on the Si surface at room temperature via Pt-assisted catalytic chemical etching in water without the addition of any chemicals. Furthermore, dissolved oxygen (O₂) in water has been found to be a key element for driving the chemical reaction of Si with water in the Si removal process. Experimental results have also suggested that an oscillating cantilever of the Pt-coated AFM probe for the stirring of water is essential in order to overcome the oxygen mass-transfer limitations and enhance the Si removal rate. The elementary chemical reactions taking place during the etching of Si has been estimated on the basis of electrochemical theory. It is proposed that in the first step, dissolved oxygen is reduced and forms hydroxide ions (OH⁻) with water molecules (H₂O) on the surface of the Pt-coated tip. In the second step, Si atoms are oxidized on reaction with OH⁻ ions and water soluble silicates are formed. The catalytic reaction taking place on the surface of a Pt-coated tip can be enhanced by the application of an anodic potential to an additional Pt wire electrode, resulting in a dramatic fifty-fold increase in the Si removal rate.     

Effect of cantilevers' dimensions on phase contrast in multifrequency atomic force microscopy

During the past years, different theoretical and experimental works are done to enhance the observables (mostly higher eigenmode's phase contrast) in multifrequency atomic force microscopy methods. In this study, the geometry of rectangular cantilevers is studied and an optimum dimension that can provide maximum phase contrast for a given set of samples is found. The analysis is done both numerically and experimentally. A sensitivity analysis is provided to demonstrate which dimension (length, width, thickness, tip‐radius, and cantilever and sample angle) of the cantilever has a higher effect on the results. The effects of geometrical dimensions are categorized into to: (a) effect on dynamics of the cantilever (b) effects on cantilever's specifications (i.e., spring constant and quality factor). Length and width of the cantilever dominates the static behavior of the cantilever. While thickness (for lower values), tip radius, and approach angle mostly affect the dynamic behavior of the cantilever. Theoretically, it is found as the length increases the phase contrast increase. This relationship is opposite for width. It was also observed that the effect of thickness for a specific range on the phase contrast depends on the 1st eigenmode amplitude setpoint. This study shows for having higher contrast, lower tip‐radius is needed. The optimum angle between cantilever and sample to enhance bimodal atomic force microscopy imaging is also found. Based on the commercially available cantilevers, the optimum cantilever dimension is provided. Three different cantilevers with similar dimensions are experimentally tested and theoretical results are verified.     

Geometric parameters effect of the atomic force microscopy smart piezoelectric cantilever on the different rough surface topography quality by considering the capillary force

Nowadays, the atomic force microscopy (AFM) is widely used in the nanotechnology as a powerful nano‐robot. The surface topography in Nanoscale is by far one of the most important usages of the AFM device. Hence, in this article, the vibration motion of a piezoelectric rectangular cross‐section micro‐cantilever (MC) which oscillates in the moist environment has been examined based on the Timoshenko beam theory. After extracting the MC governing equations according to Hamilton's principle, the finite element method has been used to discretize the motion equations. The surface topography has been simulated for various roughness forms in the tapping and non‐contact modes by considering the effects of the Van der Waals, capillary and contact forces. Also, the experimental results obtained from the glass surface topography have been simulated. The results illustrate that the time delay in higher natural frequencies in the tapping mode is shorter in comparison with the non‐contact mode, especially, for the lower natural frequencies. The sensitivity analysis of the natural frequencies, topography depth and time delay have been simulated. Results indicate that the most effective parameter is the MC length. In the first mode, the first section length has the highest effect on the surface topography time delay, also, in the second vibration mode; the most effective parameter on the time delay is the MC tip length based on the simulation results.     

Wide-range length metrology by dual-imaging-unit atomic force microscope based on porous alumina

A new dual-imaging-unit atomic force microscope (DIU-AFM) was developed for wide-range length metrology. In the DIU-AFM, two AFM units were combined, one as a reference unit, and the other a test one. Their probes with Z piezo elements and tips were horizontally set in parallel at the same height to reduce errors due to geometric asymmetry. An XY scanner was attached to an XY block that was able to move in the X direction with a step of about 500 nm. A standard porous alumina film was employed as the reference sample. Both reference sample and test sample were installed at the center of the XY scanner on the same surface and were simultaneously imaged. The two images had the same lateral size, and thus the length of the test sample image could be accurately measured by counting the number of periodic features of the reference one. The XY block together with the XY scanner were next moved in the X direction for about 1.5 microm and a second pair of reference and test images were obtained by activating the scanner. In this way, a series of pairs of images were acquired and could be spliced into two wide-range reference and test images, respectively. Again, the two spliced images were of the same size and the length of test image was measured based on the reference one. This article presents a discussion about the structure and control of the DIU-AFM system. Some experiments were carried out on the system to demonstrate the method of length calculation and measurement. Experiments show a satisfactory result of wide-range length metrology based on the hexagonal features of the porous alumina with a periodic length of several tens of nanometers. Using this method the DIU-AFM is capable of realizing nanometer-order accuracy length metrology when covering a wide range from micron to several hundreds of microns, or even up to millimeter order.     

Micropatterning of bacteria on two-dimensional lattice protein surface observed by atomic force microscopy

In this study, we characterized the two-dimensional lattice of bovine serum albumin (BSA) as a chemical and physical barrier against bacterial adhesion, using fluorescence microscopy and atomic force microscopy (AFM). The lattice of BSA on glass surface was fabricated by micro-contact printing (muCP), which is a useful way to pattern a wide range of molecules into microscale features on different types of substrates. The contact-mode AFM measurements showed that the average height of the printed BSA monolayer was 5-6nm. Escherichia coli adhered rapidly on bare glass slide, while the bacterial adhesion was minimized on the lattices in the range of 1-3mum(2). Especially, the bacterial adhesion was completely inhibited on a 1mum(2) lattice. The results suggest that the anti-adhesion effects are due by the steric repulsion forces exerted by BSA.     

TectoRNA and 'kissing-loop' RNA: atomic force microscopy of self-assembling RNA structures

RNA molecules have been much less studied by atomic force microscopy (AFM) than have DNA molecules. In this paper, AFM imaging is presented for two different RNA molecules able to self‐assemble into complex supramolecular architectures. The first one is a molecular dimer of a 230‐nt RNA fragment coming from the RNA genome of a murine leukaemia virus. The monomeric RNA fragment, which appears by AFM as an elongated structure with a mean aspect ratio of 1.4, assembles into a dimer of elongated structures through the formation of a ‘kissing‐loop’ RNA interaction. The second one is a large supramolecular fibre formed of artificial self‐assembling RNA molecular units called tectoRNA. The fibre lengths by AFM suggest that there are 50–70 tectoRNA units per fibre. Some methods and limitations are presented for measuring molecular volumes from AFM images.     

Towards quantification of doping in gallium arsenide nanostructures by low-energy scanning electron microscopy and conductive atomic force microscopy

We calculate a universal shift in work function of 59.4 meV per decade of dopant concentration change that applies to all doped semiconductors and from this use Monte Carlo simulations to simulate the resulting change in secondary electron yield for doped GaAs. We then compare experimental images of doped GaAs layers from scanning electron microscopy and conductive atomic force microscopy. Kelvin probe force microscopy allows to directly measure and map local work function changes, but values measured are often smaller, typically only around half, of what theory predicts for perfectly clean surfaces.     

Investigation of nanoparticles by atomic and lateral force microscopy

Metallic nanoparticles have been produced on vitreous carbon substrates by means of thermal evaporation. From pictures of the particles, made by a high-resolution scanning electron microscope (HRSEM), a semispherical shape is suggested due to the total mass of deposited material. Atomic force microscopy (AFM) has been applied to this sample in order to get direct topographic information. The AFM has been operated with normal and super tips, the latter having a smaller cone angle and radius, thus following more precisely the contours of an object. Simultaneously lateral-force microscopic (LFM) images have been recorded. Major differences between the contents of HRSEM- and AFM-images are considered, emphasizing the important influence of the tips' geometry. Both the AFM and LFM line scans have been compared with and have qualitatively agreed with those calculated under simplifying assumptions.