Calibration of atomic force microscope cantilevers using piezolevers

The atomic force microscope (AFM) can provide qualitative information by numerous imaging modes, but it can also provide quantitative information when calibrated cantilevers are used. In this article a new technique is demonstrated to calibrate AFM cantilevers using a reference piezolever. Experiments are performed on 13 different commercially available cantilevers. The stiff cantilevers, whose stiffness is more than 0.4 N/m, are compared to the stiffness values measured using nanoindentation. The experimental data collected by the piezolever method is in good agreement with the nanoindentation data. Calibration with a piezolever is fast, easy, and nondestructive and a commercially available AFM is enough to perform the experiments. In addition, the AFM laser must not be calibrated. Calibration is reported here for cantilevers whose stiffness lies between 0.08 and 6.02 N/m.     

Accurate determination of spring constant of atomic force microscope cantilevers and comparison with other methods

We present calibration results of commercial AFM cantilevers using the KRISS nanoforce calibrator (NFC) that can determine traceably spring constants with an uncertainty better than 1%, along with the results obtained from other four calibration methods: the dimensional method, the cantilever-on-cantilever method, the Sader method, and the thermal noise method. Two types (contact and tapping mode) of beam-shaped AFM cantilevers with nominal spring constants of 0.9 N m⁻¹ and 42 N m⁻¹, respectively, were investigated in this study. Because of its small uncertainty, the NFC method was used to assess the uncertainties of other four methods through comparisons between values obtained from other methods and those from the NFC method for the same cantilever. Results from other methods were generally in good agreement with those from the NFC method within the uncertainties of other methods claimed in other literatures, but values obtained from the Sader method were differed by up to 40% from the NFC values, which is 2 times worse than the known uncertainty.     

原子力显微镜在液相环境中的应用研究

简要介绍了原子力显微镜的工作原理 ,着重分析了液相探头的设计 ,并利用该探头进行了液相环境的样品表面形貌测量 ,给出了测量的图像。实验表明 ,该液相探头具有良好的液态环境扫描性能 ,图像稳定 ,分辨力高。     

Nanotribological characterization of digital micromirror devices using an atomic force microscope

Texas Instruments’ digital micromirror device (DMD) comprises an array of fast digital micromirrors, monolithically integrated onto and controlled by an underlying silicon memory chip. The DMD is one of the few success stories in the emerging field of MEMS. In this study, an atomic force microscope (AFM) has been used to characterize the nanotribological properties of the elements of the DMD. An AFM methodology was developed to identify and remove micromirrors of interest. The surface roughness, adhesion, friction, and stiffness properties of the DMD elements were studied. The influence of relative humidity and temperature on the behavior of the DMD element surfaces was also investigated. Potential mechanisms for wear and stiction are discussed in light of the findings.     

Bituminous emulsions and their characterization by atomic force microscopy

We present a new method for observing oil-in-water emulsions with a continuous water phase and a dispersed bitumen phase. The fine polydispersed bitumen micelles were adsorbed to an atomically smooth mica substrate and imaged in solution by atomic force microscopy in a liquid cell. The height of the adsorbed bitumen sheet in wet and dry states can be measured and the homogeneity of film formation by coalescence can be determined. Localization of surfactant onto and between bitumen micelles is also visualized.     

Modulus characterization of cells with submicron colloidal probes by atomic force microscope

Colloidal probes have been increasingly demanded for the characterization of cellular modulus in atomic force microscope because of their well-defined geometry and large contact area with cell. In this work, submicron colloidal probes are prepared by scanning electron microscope/focused ion beam and compared with sharp tip and micron colloidal probe, in conjunction with loading velocity and indentation depth on the apparent elastic modulus. NIM and cartilage cells are used as specimens. The results show that modulus value measured by sharp tip changes significantly with loading velocity while remains almost stable by colloidal probes. Also, submicron colloidal probe is superior in characterizing the modulus with increasing indentation depth, which could help reveal the mechanical details of cellular membrane and the modulus of the whole cell. To test the submicron colloidal probe further, the modulus distribution map of cell is scanned with submicron colloidal probe of 50 nm radius during small and large indentation depths with high spatial resolution. The outcome of this work will provide the effective submicron colloidal probe according to the effect of loading velocity and indentation depth, characterizing the mechanical properties of the cells.     

Effect of multiplicative noise on least-squares parameter estimation with applications to the atomic force microscope

Measurement of the power spectral density of (stochastic) Brownian fluctuations of micro- and nano-devices is used frequently to gain insight into their mechanistic properties. Noise is always present in these measurements and can directly influence any parameter estimation obtained through a least-squares analysis. Importantly, measurements of the spectral density of stationary random signals, such as Brownian motion, inherently contain multiplicative noise. In this article, we theoretically analyze the impact of multiplicative noise on fit parameters extracted using a least-squares analysis. A general analysis is presented that is valid for any fit function with any number of fit parameters. This yields closed-form expressions for the expected value and variance in the fit parameters and provides a rigorous theoretical framework for a priori determination of the effect of measurement uncertainty. The theory is demonstrated and validated through Monte Carlo simulation of synthetic data and by comparison to power spectral density measurements of the Brownian fluctuations of an atomic force microscope cantilever - analytical formulas for the uncertainty in the fitted resonant frequency and quality factor are presented. The results of this study demonstrate that precise measurements of fit parameters in the presence of noise are inherently problematic - individual measurements of the power spectral density are capable of yielding fit parameters that are many standard deviations away from the mean, with finite probability. This is of direct relevance to a host of applications in measurement science, including those connected with the atomic force microscope.     

Distortion in the thermal noise spectrum and quality factor of nanomechanical devices due to finite frequency resolution with applications to the atomic force microscope

The thermal noise spectrum of nanomechanical devices is commonly used to characterize their mechanical properties and energy dissipation. This spectrum is measured from finite time series of Brownian motion of the device, which is windowed and Fourier transformed. Here, we present a theoretical and experimental investigation of the effect of such finite sampling on the measured device quality factor. We prove that if no spectral window is used, the thermal noise spectrum retains its original Lorentzian distribution but with a reduced quality factor, indicating an apparent enhancement in energy dissipation. A simple analytical formula is derived connecting the true and measured quality factors - this enables extraction of the true device quality factor from measured data. Common windows used to reduce spectral leakage are found to distort the (true) Lorentzian shape, potentially making fitting problematic. These findings are expected to be of particular importance for devices with high quality factors, where spectral resolution can be limited in practice. Comparison and validation using measurements on atomic force microscope cantilevers are presented.     

原子力显微镜的力曲线分析与转化

原子力显微镜测定的力曲线需转化为力位移曲线来应用.力位移曲线是以任意点为零点的,当研究粘附或者分子模型对比时,需要知道针尖样品间的作用力或确切的零点位置,这时需将其转化为力-距离曲线.本文首先从力曲线的测定原理得出了典型的力曲线,之后从理论上分析了力曲线、力位移曲线和力-距离曲线间的转化,从中得出了转化过程中需要的两个重要参量:灵敏度和零距离,并提出了确定方法.最后,利用MATLAB实现了曲线的自动转化.     

Note: A scanning electron microscope sample holder for bidirectional characterization of atomic force microscope probe tips

A novel sample holder that enables atomic force microscopy (AFM) tips to be mounted inside a scanning electron microscopy (SEM) for the purpose of characterizing the AFM tips is described. The holder provides quick and easy handling of tips by using a spring clip to hold them in place. The holder can accommodate two tips simultaneously in two perpendicular orientations, allowing both top and side view imaging of the tips by the SEM.     

The comparison between force volume and peakforce quantitative nanomechanical mode of atomic force microscope in detecting cell's mechanical properties

Atomic force microscope (AFM) has been widely used in the biological field owing to its high sensitivity (subnanonewton), high spatial resolution (nanometer), and adaptability to physiological environments. Nowadays, force volume (FV) and peakforce quantitative nanomechanical (QNM) are two distinct modes of AFM used in biomechanical research. However, numerous studies have revealed an extremely confusing phenomenon that FV mode has a significant difference with QNM in determining the mechanical properties of the same samples. In this article, for the case of human benign prostatic hyperplasia cells (BPH) and two cancerous prostate cells with different grades of malignancy (PC3 and DU145), the differences were compared between FV and QNM modes in detecting mechanical properties. The results show measured Young's modulus of the same cells in FV mode was much lower than that obtained by QNM mode. Combining experimental results with working principles of two modes, it is indicated that surface adhesion is highly suspected to be a critical factor resulting in the measurement difference between two modes. To further confirm this conjecture, various weight ratios of polydimethylsiloxane (PDMS) were assessed by two modes, respectively. The results show that the difference of Young's modulus measured by two modes increases with the surface adhesion of PDMS, confirming that adhesion is one of the significant elements that lead to the measurement difference between FV and QNM modes.     

原子力显微镜在DNA领域中研究应用

原子力显微镜(AFM)是研究DNA有力工具,在对DNA研究中有其独特优势。本文概述原子力显微镜DNA研究中应用以及取得进展。虽然原子力显微镜在研究DNA研究中仍有局限性,但随着原子力显微技术及相关技术发展,原子力显微镜在DNA中研究必将不断深入。     

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。     

A novel cleaning method of gold-coated atomic force microscope tips for their chemical modification

For chemical modification of gold-coated AFM tips with thiol or sulfide compounds, a new two-step precleaning procedure was studied. The two-step cleaning procedure involves (i) oxidation of organic contaminants on the AFM tips with ozone treatment and (ii) reduction of the oxidized gold surface by immersing the oxidized tip into pure hot ethanol at ca. 65 degrees C. The chemically modified tips prepared from gold-coated AFM tips precleaned by the two-step procedure gave almost the same tip characteristics as those chemically modified immediately after gold vapor deposition in a factory. The present two-step cleaning procedure can be used widely for chemical modification of commercially available gold-coated AFM tips with thiol or disulfide compounds for chemical force microscopy.     

Note: ferrule-top atomic force microscope. II. Imaging in tapping mode and at low temperature

In a recent paper [D.Chavan et al., Rev. Sci. Instrum. 81, 123702 (2010)] we have demonstrated that ferrule-top cantilevers, obtained by carving the end of a ferruled fiber, can be used for contact mode atomic force microscopy in ambient conditions. Here we show that those probes can provide tapping mode images at both room and cryogenic temperatures (12 K).     

Study of SU-8 photoresist cross-linking process by atomic force acoustic microscopy

In this paper, a method is presented to detect the different phases of epoxy cross-linking process and the subsurface structures of SU-8 thin films by atomic force acoustic microscopy (AFAM). The AFAM imaging of SU-8 thin films was investigated under different exposure and bake conditions. Optimized conditions were obtained for the cross-linking of SU-8 thin film at the exposure does of eight laser pulses with the laser fluence 10 mJ cm^–2 per pulse and the post exposure bake (PEB) time at 90 s. The subsurface structures of undeveloped SU-8 thin films were visible in the AFAM images. This method provides an effective and low-cost way for the determination of different phases of epoxy cross-linking process in nanostructured compounds, for the non-destructive testing of subsurface defects, and for the evaluation of the quality of patterned structures.     

A large-sample atomic force microscope observing in both air and liquid

A large-sample atomic force microscope (AFM) that allows high resolution observation in both air and liquid has been developed. With a unique beam tracking method, laser beam is capable of reflecting off the same spot on the AFM cantilever throughout raster scan over the entire scan area, either operating in air or in liquid environment. Incorporating the stand-alone AFM probe unit with an automated large sample stage, wide-scan-range imaging can be realized with high resolution and slight distortion. In addition, an image stitching method is utilized to build a broad merged image with range up to millimeters while keeping nanometer order resolution. By using a large-volume liquid bath, large and massive sample can be observed in liquid with this AFM system. Several typical experiments have been carried out to demonstrate the imaging ability and stability of this AFM. Topographic structures of gold pattern on a glass substrate are scanned at two different places on the same specimen surface. The porosity of a sheet of filter paper is then characterized in both air and water. Finally, larger-area AFM image of anodic aluminum oxide template in oxalic acid is on spot obtained by merging several individually scanned images together. Experiments show that this AFM system can offer high resolution and wide range AFM images even for large samples with remarkable capabilities in various environments.     

Effect of contact stiffness on wedge calibration of lateral force in atomic force microscopy

Quantitative friction measurement of nanomaterials in atomic force microscope requires accurate calibration method for lateral force. The effect of contact stiffness on lateral force calibration of atomic force microscope is discussed in detail and an improved calibration method is presented. The calibration factor derived from the original method increased with the applied normal load, which indicates that separate calibration should be required for every given applied normal load to keep the accuracy of friction measurement. We improve the original method by introducing the contact factor, which is derived from the contact stiffness between the tip and the sample, to the calculation of calibration factors. The improved method makes the calculation of calibration factors under different applied normal loads possible without repeating the calibration procedure. Comparative experiments on a silicon wafer have been done by both the two methods to validate the method in this article.     

Retrofitting an atomic force microscope with photothermal excitation for a clean cantilever response in low Q environments

It is well known that the low-Q regime in dynamic atomic force microscopy is afflicted by instrumental artifacts (known as "the forest of peaks") caused by piezoacoustic excitation of the cantilever. In this article, we unveil additional issues associated with piezoacoustic excitation that become apparent and problematic at low Q values. We present the design of a photothermal excitation system that resolves these issues, and demonstrate its performance on force spectroscopy at the interface of gold and an ionic liquid with an overdamped cantilever (Q < 0.5). Finally, challenges in the interpretation of low-Q dynamic AFM measurements are discussed.