Force interactions between substrates and SPM cantilevers immersed in fluids

With the availability of equipment used in Scanning Probe Microscopy (SPM), researchers have been able to probe the local fluid–substrate force interactions with resolutions of pN using a variety of SPM cantilevers. When using such methods, it is essential to differentiate between contributions to the net force on the cantilever. Specifically, the interaction between the cantilever, substrate and fluid, quantified while generating force curves, are discussed and compared with theoretical models for squeeze-film effects and drag on the SPM cantilevers. In addition we have demonstrated a simple method for utilizing the system as a micro-viscometer, independently measuring the viscosity of the lubricant for each test.     

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.     

New tools for force spectroscopy

Force curves using atomic force microscopy have been proposed as a new tool to probe the conformation of adsorbed polymers and interactions between molecules through the analysis of the rupture distributions. We describe an algorithm for the computer-assisted detection of ruptures in force curves. This program allows us to automatically detect the ruptures. The algorithm is based on an analysis of the standard deviation in a sliding window along the length of the force. Automatic detection of ruptures constitutes an important step forward because the time required to analyse the curves is significantly reduced, thus allowing the user to perform multiple experiments. In addition, using these tools we can address the problem of the interpretation of rupture distributions.     

Miniature active damping stage for scanning probe applications in ultra high vacuum

Scanning probe microscope (SPM) experiments demand a low vibration level to minimize the external influence on the measured signal. We present a miniature six-degree of freedom active damping stage based on a Gough-Stewart platform (hexapod) which is positioned in ultra high vacuum as close to the SPM as possible. In this way, vibrations originating from the experimental setup can be effectively reduced providing a quiet environment for the SPM. In addition, the hexapod provides a rigid reference point, which facilitates wiring as well as sample transfer. We outline the main working principle and show that for scanning tunneling microscopy (STM) measurements of a Si(111) 7 × 7 surface, the hexapod significantly improves the stability and quality of the topographic images.     

Design and performance of a combined secondary ion mass spectrometry-scanning probe microscopy instrument for high sensitivity and high-resolution elemental three-dimensional analysis

State-of-the-art secondary ion mass spectrometry (SIMS) instruments allow producing 3D chemical mappings with excellent sensitivity and spatial resolution. Several important artifacts however arise from the fact that SIMS 3D mapping does not take into account the surface topography of the sample. In order to correct these artifacts, we have integrated a specially developed scanning probe microscopy (SPM) system into a commercial Cameca NanoSIMS 50 instrument. This new SPM module, which was designed as a DN200CF flange-mounted bolt-on accessory, includes a new high-precision sample stage, a scanner with a range of 100 μm in x and y direction, and a dedicated SPM head which can be operated in the atomic force microscopy (AFM) and Kelvin probe force microscopy modes. Topographical information gained from AFM measurements taken before, during, and after SIMS analysis as well as the SIMS data are automatically compiled into an accurate 3D reconstruction using the software program "SARINA," which was developed for this first combined SIMS-SPM instrument. The achievable lateral resolutions are 6 nm in the SPM mode and 45 nm in the SIMS mode. Elemental 3D images obtained with our integrated SIMS-SPM instrument on Al/Cu and polystyrene/poly(methyl methacrylate) samples demonstrate the advantages of the combined SIMS-SPM approach.     

Modeling scanning probe microscope lateral dynamics using the probe-surface interaction signal

In this paper, a novel scanning probe microscope (SPM) modeling technique is presented. The novelty of this technique is that it exploits the SPM's probe-surface interaction measurement capabilities [e.g., the topography signal in atomic force microscopy (AFM)] to determine the SPM's lateral positioning dynamics. SPM operation speed is limited due to mechanical vibrations induced by movement of the SPM nanopositioner. In order to facilitate high-speed SPM operation, the dynamics of the SPM can be modeled and used to design feedforward and feedback controllers that reduce nanopositioner vibrations. The proposed technique seeks to develop a transfer function model of the SPM dynamics using only the SPM probe-surface interaction signal obtained while scanning a calibration sample. The technique is presented in the context of an AFM example, errors associated with the method are analyzed, and the method is experimentally verified using a commercial AFM. Experimental modeling results show that the method is capable of modeling the dynamics of SPM systems.     

Note: In situ cleavage of crystallographic oriented tips for scanning probe microscopy

We report an in situ method of preparing tips for scanning probe microscopy (SPM). Oriented single-crystal nickel oxide (NiO) rods were diced, using a wafer saw, to prepare artificial breaking points. Two geometries, a single rod and a two-sided cut rod were fabricated. The cleavable tips were mounted to a force sensor based on a quartz tuning fork and cleaved using the coarse approach of the SPM. Atomically resolved force microscopy images of NiO (001) were taken with these NiO tips.     

General three-dimensional image simulation and surface reconstruction in scanning probe microscopy using a dexel representation

The ability to image complex general three-dimensional (3D) structures, including reentrant surfaces and undercut features using scanning probe microscopy, is becoming increasing important in many small length-scale applications. This paper presents a dexel data representation and its algorithm implementation for scanning probe microscope (SPM) image simulation (morphological dilation) and surface reconstruction (erosion) on such general 3D structures. Validation using simulations, some of which are modeled upon actual atomic force microscope data, demonstrates that the dexel representation can efficiently simulate SPM imaging and reconstruct the sample surface from measured images, including those with reentrant surfaces and undercut features.     

Imaging and Measuring the Molecular Force of Lymphoma Pathological Cells Using Atomic Force Microscopy

Atomic force microscopy (AFM) provides a new technology to visualize the cellular topography and quantify the molecular interactions at nanometer spatial resolution. In this work, AFM was used to image the cellular topography and measure the molecular force of pathological cells from B‐cell lymphoma patients. After the fluorescence staining, cancer cells were recognized by their special morphological features and then the detailed topography was visualized by AFM imaging. The AFM images showed that cancer cells were much rougher than healthy cells. CD20 is a surface marker of B cells and rituximab is a monoclonal antibody against CD20. To measure the CD20‐rituximab interaction forces, the polyethylene glycol (PEG) linker was used to link rituximab onto the AFM tip and the verification experiments of the functionalized probe indicated that rituximab molecules were successfully linked onto the AFM tip. The CD20‐rituximab interaction forces were measured on about 20 pathological cells and the force measurement results indicated the CD20‐rituximab binding forces were mainly in the range of 110–120 pN and 130–140 pN. These results can improve our understanding of the topography and molecular force of lymphoma pathological cells. SCANNING 35:40‐46, 2013. © 2012 Wiley Periodicals, Inc.     

MEMS-based fast scanning probe microscopes

Scanning probe microscopy is a frequently used nanometer-scale surface investigation technique. Unfortunately, its applicability is limited by the relatively low image acquisition speed, typically seconds to minutes per image. Higher imaging speeds are desirable for rapid inspection of samples and for the study of a range of dynamic surface processes, such as catalysis and crystal growth. We have designed a new high-speed scanning probe microscope (SPM) based on micro-electro mechanical systems (MEMS). MEMS are small, typically micrometer size devices that can be designed to perform the scanning motion required in an SPM system. These devices can be optimized to have high resonance frequencies (up to the MHz range) and have very low mass (10⁻¹¹ kg). Therefore, MEMS can perform fast scanning motion without exciting resonances in the mechanical loop of the SPM, and hence scan the surface without causing the image distortion from which conventional piezo scanners suffer. We have designed a MEMS z-scanner which we have integrated in commercial AFM (atomic force microscope) and STM (scanning tunneling microscope) setups. We show the first successful AFM experiments.     

The effect of deformation on the lateral resolution of atomic force microscopy

A computer model based on the elastic properties of rubber is introduced for the evaluation of the lateral resolution in atomic force microscopy of deformable specimens. The computational results show that, if the full width at half-height can be defined as the lateral resolution, it is continuously improved at greater probe forces, at the expense of a reduced molecular height. In fact, even for a probe that is bigger than the molecule, the real size of the molecule can be 'recovered' at about 25% compression. This result demonstrates that for a better lateral resolution, a greater probe force can be beneficial, provided that the molecule is not moved or damaged and the response remains elastic. Measurements on isolated low-density lipoproteins (LDL) show that with 26% vertical compression, the lateral size measured in atomic force microscopy is only about 72% of the value predicted by a simple convolution, and is only slightly larger (≈ 13%) than the known size of LDL. Therefore, the results on LDL provide a direct support for the conclusions of the computational model.     

Atomic and magnetic force microscopy imaging of thin-film recording heads

Investigations on the use of the scanning probe microscope (SPM) in the atomic force microscopy (AFM) mode for topography imaging and the magnetic force microscopy (MFM) mode for magnetic imaging are presented for a thin-film recording head. Results showed that the SPM is suitable for imaging the surface profile of the recording head, determining the width of the pole gap region, and mapping the magnetic field patterns of the recording head excited under current bias conditions of different polarity. For the cobalt sputter-coated tips used in MFM imaging, it was found that the magnetic field patterns obtained under different polarities of the current bias to the recording head were similar. This can be explained by the nature of the thin-film MFM tip, in which the direction of the tip magnetic moment can follow the stray magnetic field of the sample as the current bias to the recording head reverses in direction.     

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.     

Application of scanning probe microscopy to the characterization and fabrication of hybrid nanomaterials

Scanning probe microscopy (SPM) is a widely used experimental technique for characterizing and fabricating nanostructures on surfaces. In particular, due to its ability to spatially map variations in materials properties with nanometer spatial resolution, SPM is particularly well suited to probe the subcomponents and interfaces of hybrid nanomaterials, i.e., materials that are made up of distinct nanometer scale components with distinguishable properties. In addition, the interaction of the SPM tip with materials can be intentionally tuned such that local surface modification is achieved. In this manner, hybrid nanostructures can also be fabricated on solid substrates using SPM. This report reviews recent developments in the characterization and fabrication of hybrid nanomaterials with SPM. Specific attention is given to nanomaterials that consist of both organic and inorganic components including individual biomolecules mounted on inorganic substrates. SPM techniques that are particularly well suited for characterizing the mechanical and electrical properties of such hybrid systems in atmospheric pressure environments are highlighted, and specific illustrative examples are provided. This review concludes with a brief discussion of the remaining challenges and promising future prospects for this field.     

Calibration and examination of piezoresistive Wheatstone bridge cantilevers for scanning probe microscopy

This paper describes the method of determining the force constant and displacement sensitivity of piezoresistive Wheatstone bridge cantilevers applied in scanning probe microscopy (SPM). In the procedure presented here, the force constant for beams with various geometry is determined based on resonance frequency measurement. The displacement sensitivity is measured by the deflection of the cantilever with the calibrated piezoactuator stage. Preliminary results show that our method is capable of measuring the force constant of Wheatstone bridge cantilevers with an accuracy of better than 5% and this is used as feedback for improvement of sensor micromachining process.     

基于相位反馈控制的压电微音叉扫描探针显微镜

压电微音叉具有谐振频率稳定、品质因数高和易于实现音叉臂的振动检测等优点。利用微音叉的这些特性,将其与钨探针结合,构成了压电微音叉扫描探针显微镜(SPM)测头,可实现对微观表面的测量。该测头扫描时,压电微音叉的谐振频率被试样表面原子和钨探针尖端原子间的作用力调制。探针的谐振状态通过锁相环路(PLL)实现,微音叉测头与试样间的恒定测力及测头的Z向定位通过相位反馈控制实现。此外,测量系统可同时获得试样表面的微观轮廓图和相位图。     

Charge Contribution to the Adhesion Performance of Polymeric Microstructures

Strong attachment of many insects with microstructured attachment pads is due to the Van der Waals interactions or/and the capillary forces between the pads and substrates. To establish initial contact between two surfaces a certain normal force should be applied. The presence of the charges on surfaces could facilitate or impede the initial contact formation. In this study, forces appearing due to the contact electrification of microstructured material mimicking beetle adhesive pads were measured and their influence on the contact formation was discussed. The experiments have clearly demonstrated that static charges contribute to an initial contact establishment in materials with the mushroom-shaped microstructure, whereas Van der Waals interactions or/and capillary forces have the main contribution at pull-off. A simple model was successfully used for data analysis and extraction information about the charge distribution. The effect of the jump-in due to the electrostatic interaction has to be considered during the development of further implementation of biologically inspired microstructured adhesives.     

Combining optical tweezers and scanning probe microscopy to study DNA-protein interactions

We present the first results obtained with a new instrument designed and built to study DNA-protein interactions at the single molecule level. This microscope combines optical tweezers with scanning probe microscopy and allows us to locate DNA-binding proteins on a single suspended DNA molecule. A single DNA molecule is stretched taut using the optical tweezers, while a probe is scanned along the molecule. Interaction forces between the probe and the sample are measured with the optical tweezers. The instrument thus enables us to correlate mechanical and functional properties of bound proteins with the tension within the DNA molecule. The typical friction force between a micropipette used as probe and a naked DNA molecule was found to be <1 pN. A 16 micro m DNA molecule with approximately 10-15 digoxygenin (DIG) molecules located over a 90 nm range in the middle of the DNA was used as a model system. By scanning with an antidigoxygenin (alpha-DIG) antibody-coated pipette we were able to localize these sites by exploiting the high binding affinity between this antibody-antigen pair. The estimated experimental resolution assuming an infinitesimally thin and rigid probe and a single alpha-DIG/DIG bond was 15 nm.     

An integrated methodology for data processing in dynamic force spectroscopy of ligand-receptor binding

Dynamic force spectroscopy (DFS), using atomic force microscopy (AFM), is a powerful tool to study ligand-receptor binding. The interaction mode of two binding partners is investigated by exploring stochastic behaviors of bond rupture events. However, to define a rupture event from force-distance measurements is not conclusive or unique in literature. To reveal the influence of event identification methods, we have developed an efficient protocol to manage tremendous amount of data by implementing different choices of peak selection from the force-distance curve. This data processing software simplifies routinely experimental procedures such as cantilever spring constant and force-distance curve calibrations, statistical treatments of data, and analysis distributions of rupture events. In the present work, we took available experimental data from a complex between a chelate metal compound and a monoclonal antibody as a study system.     

Optimal design and fabrication of three-dimensional calibration specimens for scanning probe microscopy

Micro-/nano-scale roughness specimens are highly demanded to synthetically calibrate the scanning probe microscopy (SPM) instrument. In this study, three-dimensional (3D) specimens with controllable main surface evaluation parameters were designed. In order to improve the design accuracy, the genetic algorithm was introduced into the conventional digital filter method. A primary 3D calibration specimen with the dimension of 10 μm × 10 μm was fabricated by electron beam lithography. Atomic force microscopy characterizations demonstrated that the statistical and spectral parameters of the fabricated specimen match well with the designed values. Such a kind of 3D specimens has the potential to calibrate the SPM for applications in quantitative surface evaluations.