Finite-element vibration analysis of tapping-mode atomic force microscopy in liquid

Investigation of morphology and mechanical properties of biological specimens using atomic force microscopy (AFM) often requires its operation in liquid environment. Due to the hydrodynamic force, the vibration of AFM cantilevers in liquid shows dramatically different dynamic characteristics from that in air. A good understanding of the dynamics of AFM cantilevers vibrating in liquid is needed for the interpretation of scanning images, selection of AFM operating conditions, and evaluation of sample's mechanical properties. In this study, a finite element (FE) model is used for frequency and transient response analysis of AFM cantilevers in tapping mode (TM) operated in air or liquid. Hydrodynamic force exerted by the fluid on AFM cantilevers is approximated by additional mass and hydrodynamic damping. The additional mass and hydrodynamic damping matrices corresponding to beam elements are derived. With this model, numerical simulations are performed for an AFM cantilever to obtain the frequency and transient responses of the cantilever in air and liquid. The comparison between our simulated results and the experimentally obtained ones shows good agreement. Based on the simulations, different characteristics of cantilever dynamics in air and liquid are discussed.     

Harnessing bifurcations in tapping-mode atomic force microscopy to calibrate time-varying tip-sample force measurements

Torsional harmonic cantilevers allow measurement of time-varying tip-sample forces in tapping-mode atomic force microscopy. Accuracy of these force measurements is important for quantitative nanomechanical measurements. Here we demonstrate a method to convert the torsional deflection signals into a calibrated force wave form with the use of nonlinear dynamical response of the tapping cantilever. Specifically the transitions between steady oscillation regimes are used to calibrate the torsional deflection signals.     

Non-optical bimorph-based tapping-mode force sensing method for scanning near-field optical microscopy

A non‐optical bimorph‐based tapping‐mode force sensing method for tip–sample distance control in scanning near‐field optical microscopy is developed. Tapping‐mode force sensing is accomplished by use of a suitable piezoelectric bimorph cantilever, attaching an optical fibre tip to the extremity of the cantilever free end and fixing the guiding portion of the fibre to a stationary part near the tip to decouple it from the cantilever. This method is mainly characterized by the use of a bimorph, which carries out simultaneous excitation and detection of mechanical vibration at its resonance frequency owing to piezoelectric and anti‐piezoelectric effects, resulting in simplicity, compactness, ease of implementation and lack of parasitic optical background. In conjugation with a commercially available SPM controller, tapping‐mode images of various samples, such as gratings, human breast adenocarcinoma cells, red blood cells and a close‐packed layer of 220‐nm polystyrene spheres, have been obtained. Furthermore, topographic and near‐field optical images of a layer of polystyrene spheres have also been taken simultaneously. The results suggest that the tapping‐mode set‐up described here is reliable and sensitive, and shows promise for biological applications.     

日本精工SAP400原子力显微镜性能的改进

日本精工公司(SEIKO)生产的原子力显微镜的功能多、性能好,国内已经有近百台的拥有量。它的信号放大、处理主要由锁相放大器完成。但其内部的锁相放大器灵敏度不够高,外加一台高性能、高灵敏度的锁相放大器,可大大提高其性能。用美国斯坦福公司产的SR830锁相放大器对本实验室的日本SEIKO公司SPA400原子力显微镜进行性能改进,可使其性能有很大提高。     

Cross-talk correction in atomic force microscopy

Commercial atomic force microscopes usually use a position-sensitive photodiode to detect the motion of the cantilever via laser beam deflection. This readout technique makes it possible to measure bending and torsion of the cantilever separately. A slight angle between the orientation of the photodiode and the plane of the readout laser beam, however, causes false signals in both readout channels. This cross-talk may lead to misinterpretation of the acquired data. We demonstrate this fault with images recorded in contact mode on periodically poled ferroelectric crystals and present a simple electronic circuit to compensate for it. This circuit can correct for cross-talk with a bandwidth of approximately 1 MHz suppressing the the false signal to <1%.     

Measurement of thermal expansion coefficient of INVAR foil using atomic force microscopy

The production of organic light emitting diode (OLED) displays depends on the use of the low coefficient of thermal expansion (CTE) of INVAR foils as the shadow mask. The high-resolution of the smartphone displays requires increasingly thin INVAR in a two-step etching process. However, it is difficult to measure CTE for very thin metal foils. A simple method is developed to measure the linear CTE of the INVAR foil using atomic force microscopy (AFM). This method uses a focus-ion-beam (FIB) to etch a 5000 μm trench on the INVAR foil. The thermal drift of the system is calibrated from AFM images, and the average linear CTE of the INVAR foil is then calculated from the displacements of two side end points of the trench on the foil during temperature variation. The linear CTE obtained by the proposed method is quite close to the value of the bulk INVAR provided by the manufacturer.     

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.     

Real-time atomic force microscopy in lubrication condition

We have studied frictional force and wear problem in real-time atomic force microscopy in contact-mode using a resonator type mechanical scanner allegedly reported. The fast scanning may cause wear in the sample surface or the tip, and may deteriorate the image quality. Mineral oil was used to make a lubricious surface on a polycarbonate sample, and it was found that the interfacial frictional force was decreased. A Si tip which was coated with a hydrophobic film by means of chemical modification was confirmed to diminish the frictional force in the fast scanning process. The resultant image quality was improved due to reduced friction and wear.     

Intrinsic dissipation in atomic force microscopy cantilevers

In this paper we build a practical modification to the standard Euler-Bernoulli equation for flexural modes of cantilever vibrations most relevant for operation of AFM in high vacuum conditions. This is done by the study of a new internal dissipation term into the Euler-Bernoulli equation. This term remains valid in ultra-high vacuum, and becomes particularly relevant when viscous dissipation with the fluid environment becomes negligible. We derive a compact explicit equation for the quality factor versus pressure for all the flexural modes. This expression is used to compare with corresponding extant high vacuum experiments. We demonstrate that a single internal dissipation parameter and a single viscosity parameter provide enough information to reproduce the first three experimental flexural resonances at all pressures. The new term introduced here has a mesoscopic origin in the relative motion between adjacent layers in the cantilever.     

Adhesion artefacts in atomic force microscopy imaging

Artefacts that affect contrast and arise from adhesion forces in atomic force microscopy images of aramid fibres (both fresh and plasma-treated) are investigated. It is demonstrated that these stem not only from variations in the chemical composition of the surface but also from certain topographical features (which may appear hidden or enhanced in the images), resulting in changes in the lateral forces that are detected by the cantilever and are comparable to the vertical forces. It is also shown that both types of contribution to the forces can be uncoupled to yield images free from these artefacts, thus allowing more accurate quantitative measurements. These artefactual effects are also generally applicable to many other materials.     

Developments for inverted atomic force microscopy

Atomic force microscopy (AFM) has been used to study a wide range of systems. Chemically and biologically modified probes have extended AFM by coupling chemical and biological information with the physical measurements. In an effort to further expand the capabilities of modified AFM probes, previous studies investigated the use of an inverted AFM design (i-AFM), wherein a microfabricated tip array is used to image a cantilever-supported sample. This report details developments in cantilever and tip array fabrication which are aimed at improving the applicability and performance of this i-AFM design. Using an epoxy-based procedure, commercial cantilevers were modified with a series of standard substrates, including template-stripped gold, highly oriented pyrolytic graphite, and mica. The samples on these cantilevers were imaged with i-AFM, and lateral force images are obtained. This paper demonstrates the first use of i-AFM for measuring friction.     

C-banding visualized by atomic force microscopy

C-banding is a method used for studying chromosome rearrangements near centromeres and for investigating polymorphisms. In human chromosomes, the C-bands are located at the centromere of all the chromosomes and the distal long arm of the Y chromosome. In this study, we aimed to detect the structural changes in chromosomes during the stages of C-banding by atomic force microscopy. We observed crater-like structures in the chromosomes after 2xSSC (saline sodium citrate) treatment and measured the relative difference between the heights of chromatid and centromere of the chromosomes. Results showed that the relative difference was 3 nm in chromosomes 1, 9, 16, and Y, whereas in the other chromosomes this value was 11.6 nm. After Giemsa staining, the relative difference increased by a factor of 16 in chromosomes 1, 9, 16, and Y. The other chromosomes showed no such increase, which is in accordance with our suggestion that nonhiston proteins associated with DNA in constitutive heterochromatin can make the constitutive heterochromatin resistant to C-banding.     

Near-grain-boundary characterization by atomic force microscopy

Characterization of near-grain boundary is carried out by atomic force microscopy (AFM). It has been observed to be the most suitable technique owing to its capability to investigate the surface at high resolution. Commercial purity-grade nickel processed under different conditions, viz., (i) cold-rolled and annealed and (ii) thermally etched condition without cold rolling, is considered in the present study. AFM crystallographic data match well with the standard data. Hence, it establishes two grain-boundary relations viz., plane matching and coincidence site lattice (CSL Σ=9) relation for the two different sample conditions.     

Chemical force microscopy of microcontact-printed self-assembled monolayers by pulsed-force-mode atomic force microscopy

A novel chemically sensitive imaging mode based on adhesive force detection by previously developed pulsed-force-mode atomic force microscopy (PFM-AFM) is presented. PFM-AFM enables simultaneous imaging of surface topography and adhesive force between tip and sample surfaces. Since the adhesive forces are directly related to interaction between chemical functional groups on tip and sample surfaces, we combined the adhesive force mapping by PFM-AFM with chemically modified tips to accomplish imaging of a sample surface with chemical sensitivity. The adhesive force mapping by PFM-AFM both in air and pure water with CH3- and COOH-modified tips clearly discriminated the chemical functional groups on the patterned self-assembled monolayers (SAMs) consisting of COOH- and CH3-terminated regions prepared by microcontact printing (microCP). These results indicate that the adhesive force mapping by PFM-AFM can be used to image distribution of different chemical functional groups on a sample surface. The discrimination mechanism based upon adhesive forces measured by PFM-AFM was compared with that based upon friction forces measured by friction force microscopy. The former is related to observed difference in interactions between tip and sample surfaces when the different interfaces are detached, while the latter depends on difference in periodic corrugated interfacial potentials due to Pauli repulsive forces between the outermost functional groups facing each other and also difference in shear moduli of elasticities between different SAMs.     

光学原子力显微镜中的蒙特卡罗方法

扫描探针显微镜(Scanning probe microscopy,SPM)是显微镜的一个分支,它利用物理探针扫描标本形成样本表面图像.而原子力显微镜(Atomic force microscopy,AFM)是SPM中一种多功能的表面成像和测量工具,对导电、不导电、真空中、空气中或流体中的各种样本均可测量.原子力显微镜最面临的最大挑战之一是评估其在表面测量过程中所伴随的不确定度.本研究通过XYZ Phase的标定,对一台光学原子力显微镜进行了校准.该方法旨在克服在评估一些无法实验确定的不确定部件时遇到的困难,如尖端表面相互作用力和尖端几何.运用蒙特卡罗方法来确定根据相关容差和概率密度函数(PDFs)随机绘制参数而引起的相关不确定度.整个过程遵循《测量不确定度表示指南》(GUM)补编2.经本方法验证,原子力显微镜的评估不确定度为10nm左右.     

Multifrequency high-speed phase-modulation atomic force microscopy in liquids

We have developed a new technique, called multifrequency high-speed phase-modulation atomic force microscopy (PM-AFM) in constant-amplitude (CA) mode based on the simultaneous excitation of the first two flexural modes of a cantilever. By performing a theoretical investigation, we have found that this technique enables the simultaneous imaging of the surface topography, energy dissipation and elasticity (nonlinear mapping) of materials. We experimentally demonstrated high-speed imaging at a scan speed of 5 frames/s for a polystyrene (PS) and polyisobutylene (PIB) polymer-blend thin-film surface in water.     

Intermittency in amplitude modulated dynamic atomic force microscopy

From a mathematical point of view, the atomic force microscope (AFM) belongs to a special class of continuous time dynamical systems with intermittent impact collisions. Discontinuities of the velocity result from the collisions of the tip with the surface. Transition to chaos in non-linear systems can occur via the following four routes: bifurcation cascade, crisis, quasi-periodicity, and intermittency. For the AFM period doubling and period-adding cascades are well established. Other routes into chaos, however, also may play an important role. Time series data of a dynamic AFM experiment indicates a chaotic mode that is related to the intermittency route into chaos. The observed intermittency is characterized as a type III intermittency. Understanding the dynamics of the system will help improve the overall system performance by keeping the operation parameters of dynamic AFM in a range, where chaos can be avoided or at least controlled.     

Topographic and phase-contrast imaging in atomic force microscopy

Phase-contrast imaging in the tapping mode atomic force microscopy (AFM) is a powerful method in surface characterization. This method can provide fine details about rough surfaces, which are normally obscured in topographic imaging. To illustrate some of the capabilities of phase-contrast imaging, AFM studies of Pt/Ti/SiO2/Si and Pb(Zr0.52Ti0.48)O3 (PZT) films were carried out. Phase-contrast imaging revealed fine details of their microstructures, including grain boundaries, triple junctions and twinning, which could not be detected by topographic imaging. The studies showed that phase-contrast imaging is capable of providing superior information about surface characteristics when compared to the standard topographic imaging.     

Application of atomic force microscopy in bacterial research

The atomic force microscope (AFM) has evolved from an imaging device into a multifunctional and powerful toolkit for probing the nanostructures and surface components on the exterior of bacterial cells. Currently, the area of application spans a broad range of interesting fields from materials sciences, in which AFM has been used to deposit patterns of thiol‐functionalized molecules onto gold substrates, to biological sciences, in which AFM has been employed to study the undesirable bacterial adhesion to implants and catheters or the essential bacterial adhesion to contaminated soil or aquifers. The unique attribute of AFM is the ability to image bacterial surface features, to measure interaction forces of functionalized probes with these features, and to manipulate these features, for example, by measuring elongation forces under physiological conditions and at high lateral resolution (<1 Å). The first imaging studies showed the morphology of various biomolecules followed by rapid progress in visualizing whole bacterial cells. The AFM technique gradually developed into a lab‐on‐a‐tip allowing more quantitative analysis of bacterial samples in aqueous liquids and non‐contact modes. Recently, force spectroscopy modes, such as chemical force microscopy, single‐cell force spectroscopy, and single‐molecule force spectroscopy, have been used to map the spatial arrangement of chemical groups and electrical charges on bacterial surfaces, to measure cell–cell interactions, and to stretch biomolecules. In this review, we present the fascinating options offered by the rapid advances in AFM with emphasizes on bacterial research and provide a background for the exciting research articles to follow. SCANNING 32: 74–96, 2010. © 2010 Wiley Periodicals, Inc.     

A complementary-metal-oxide-semiconductor-field-effect-transistor-compatible atomic force microscopy tip fabrication process and integrated atomic force microscopy cantilevers fabricated with this process

A complementary-metal-oxide-semiconductor-field-effect-transistor-compatible process for the fabrication of atomic force microscopy cantilevers with integrated tips has been developed. For the first time, the tips are fabricated after the completion of the regular complementary metal-oxide-semiconductor-field-effect-transistor fabrication process sequence. On-chip circuit components, such as piezoresistive deflection sensors, deflection actuators, and amplifiers, are fabricated on the mirror-polished surface of the wafer, ensuring optimal performance. The tip fabrication process is based on anisotropic silicon etching at low temperature using a tetramethylammonium hydroxide solution. The anisotropic etching process has been optimized to ensure process controllability. Using the described process, complementary-metal-oxide-semiconductor-field-effect-transistor-based cantilevers with piezoresistive deflection sensors and integrated tips have been successfully fabricated. Force-distance curves and scanning images in constant-force mode have been recorded.