Wear characteristics of diamond-coated atomic force microscope probe

In atomic force microscope (AFM) applications, the wear of the probe is undoubtedly a serious concern since it affects the integrity of the measurements. In this work, wear tests were performed using an AFM with lateral force monitoring capability with the aim to better understand the wear characteristics of diamond-coated probes. For the assessment of the probe wear, a transmission electron microscope (TEM) as well as a scanning electron microscope were utilized. The degree of the probe wear was quantified using the Archard's wear equation. The structure of the diamond-coated probe was analyzed by using the TEM and Raman spectroscopy. From the experimental results, two different wear characteristics, the gradual wear and the abrupt fracture of the diamond coating, were observed. In the case of gradual wear, the wear coefficient of the diamond-coated probe slid against a silicon nitride specimen was about 10(-5)-10(-6). It was also found that the wear rate significantly decreased with increase in the sliding distance. Raman spectroscopy analysis showed that the difference in the chemical structure of the diamond coating may induce the different wear phenomena. These results may be effectively utilized for fundamental understanding of nano-wear characteristics of AFM probes.     

The number distribution of complex shear modulus of single cells measured by atomic force microscopy

The viscoelastic properties of a large number of mouse fibroblast NIH3T3 cells (n?130) were investigated by combining atomic force microscopy (AFM) with a microarray technique. In the experiments, the cells were arranged and cultured in the wells of a microarray substrate, and a force modulation mode experiment was used to measure the complex shear modulus, G*, of individual cells in a frequency range 0.5–200 Hz. The frequency dependence of G* of the cells exhibited a power-law behavior and similar frequency dependencies have been observed in several cell types cultured on flat substrates. This indicated that the NIH3T3 cells cultured in the wells of a microarray have analogous structural organization to those cells cultured on flat substrates. The number distribution of both the storage and loss moduli of G* fitted well to a log-normal distribution function, whereas the power-law exponent estimated by a power-law structural damping model showed a normal distribution function. These results showed that combining AFM with a microarray technique was a suitable approach for investigating the statistics of rheological properties of living cells without the requirement of cell surface modification.     

High-sensitivity detection of proteins using gel electrophoresis and atomic force microscopy

We have developed a method to detect specific proteins with a high sensitivity using a gel electrophoresis method and force measurement of atomic force microscopy (AFM). Biotinylated proteins were separated by electrophoresis and fixed with cross-linking chemicals on the gel, followed by direct force measurement between the biotinylated proteins on the gel and a streptavidin-modified tip of an AFM cantilever. We were able to achieve a high enough sensitivity to detect the picogram order of the biotinylated proteins by evaluating the frequency of the interaction force larger than 100 pN in the force profile, which corresponds to the rupture force of interaction between streptavidin and biotin.     

Lateral force microscopy of multiwalled carbon nanotubes

Carbon nanotubes are usually imaged with the atomic force microscope (AFM) in non-contact mode. However, in many applications, such as mechanical manipulation or elasticity measurements, contact mode is used. The forces affecting the nanotube are then considerable and not fully understood. In this work lateral forces were measured during contact mode imaging with an AFM across a carbon nanotube. We found that, qualitatively, both magnitude and sign of the lateral forces to the AFM tip were independent of scan direction and can be concluded to arise from the tip slipping on the round edges of the nanotube. The dependence on the normal force applied to the tip and on the ratio between nanotube diameter and tip radius was studied. We show that for small values of this ratio, the lateral force signal can be explained with a simple geometrical model.     

Apparent height in tapping mode of electrostatic force microscopy

We investigate a source of error in electrostatic force microscopy (EFM) measurements. During EFM, the probe performs two scans: the first to obtain the topography in tapping mode and the second at a chosen lift height to measure the electrostatic force. However, during the first scan, the electrostatic force between the probe and sample can cause error in the height measurement. In this work, micron-sized wires are fabricated, and test voltages applied. Experiments demonstrate that attractive electrostatic forces result in erroneous height measurements. A tip–sample interaction model is provided.     

Coupled lateral bending-torsional vibration sensitivity of atomic force microscope cantilever

We study the influence of the contact stiffness and the ration between cantilever and tip lengths on the resonance frequencies and sensitivities of lateral cantilever modes. We derive expressions to determine both the effective resonance frequency and the mode sensitivity of an atomic force microscope (AFM) rectangular cantilever. Once the contact stiffness is given, the resonance frequency and the sensitivity of the vibration modes can be obtained from the expression. The results show that each mode has a different resonant frequency to variations in contact stiffness and each frequency increased until it eventually reached a constant value at very high contact stiffness. The low-order vibration modes are more sensitive to vibration than the high-order mode when the contact stiffness is low. However, the situation is reversed when the lateral contact stiffness became higher. Furthermore, increasing the ratio of tip length to cantilever length increases the vibration frequency and the sensitivity of AFM cantilever.     

High-speed atomic force microscope lithography using a piezo tube scanner driven by a sinusoidal waveform

Improving the throughput of atomic force microscope (AFM) lithography is an important success factor for employing it in nanolithography applications. The conventional motion of the AFM tube scanner is usually driven by triangular-shaped signals, but it is limited in speed due to mechanical instability of the scanner at the turning points. Here, we show that high-speed lithography is achievable using not only a piezo tube driven by a sinusoidal waveform signal but also highly sensitive noble organic resists including a photo acid generator. Cross-linked polymer nanostructures applying sinusoidal waveform driving have also shown improvements in the linearity and uniformity of line patterns.     

Fabrication of carbon nanotube AFM probes using the Langmuir-Blodgett technique

Carbon nanotube (CNT)-tipped atomic force microscopy (AFM) probes have shown a significant potential for obtaining high-resolution imaging of nanostructure and biological materials. In this paper, we report a simple method to fabricate single-walled carbon nanotube (SWNT) nanoprobes for AFM using the Langmuir-Blodgett (LB) technique. Thiophenyl-modified SWNTs (SWNT-SHs) through amidation of SWNTs in chloroform allowed to be spread and form a stable Langmuir monolayer at the water/air interface. A simple two-step transfer process was used: (1) dipping conventional AFM probes into the Langmuir monolayer and (2) lifting the probes from the water surface. This results in the attachment of SWNTs onto the tips of AFM nanoprobes. We found that the SWNTs assembled on the nanoprobes were well-oriented and robust enough to maintain their shape and direction even after successive scans. AFM measurements of a nano-porous alumina substrate and deoxyribonucleic acid using SWNT-modified nanoprobes revealed that the curvature diameter of the nanoprobes was less than 3nm and a fine resolution was obtained than that from conventional AFM probes. We also demonstrate that the LB method is a scalable process capable of simultaneously fabricating a large number of SWNT-modified nanoprobes.     

Lateral force microscope calibration using a modified atomic force microscope cantilever

A proof-of-concept study is presented for a prototype atomic force microscope (AFM) cantilever and associated calibration procedure that provide a path for quantitative friction measurement using a lateral force microscope (LFM). The calibration procedure is based on the method proposed by Feiler et al. [Rev. Sci. Instrum. 71, 2746 (2000)] but allows for calibration and friction measurements to be carried out in situ and with greater precision. The modified AFM cantilever is equipped with lateral lever arms that facilitate the application of normal and lateral forces, comparable to those acting in a typical LFM friction experiment. The technique allows the user to select acceptable precision via a potentially unlimited number of calibration measurements across the full working range of the LFM photodetector. A microfabricated version of the cantilever would be compatible with typical commercial AFM instrumentation and allow for common AFM techniques such as topography imaging and other surface force measurements to be performed.     

Study of the sensitivity of the first four flexural modes of an AFM cantilever with a sidewall probe

The resonant frequency and sensitivity of flexural vibration for an atomic force microscope (AFM) cantilever with a sidewall probe have been analyzed. A closed-form expression for the sensitivity of vibration modes has been obtained using the relationship between the resonant frequency and contact stiffness of cantilever and sample. The results show that a sidewall scanning AFM is more sensitive when the contact stiffness is lower and that the first mode is the most sensitive. However, the high-order modes become more sensitive than the low-order modes as the contact stiffness increases. The resonance frequency of an AFM cantilever is low when contact stiffness is small. However, the frequency rapidly increases as contact stiffness increases. In addition, it can be found that the effects of the vertical extension on the sensitivity and the resonant frequency of an AFM cantilever are significant. Decreasing the length of vertical extension can increase the resonance frequency and sensitivity of mode 1 when the contact stiffness is small. However, the situation is reverse when the contact stiffness becomes large.     

Quantitative characterization of crosstalk effects for friction force microscopy with scan-by-probe SPMs

If the photodetector and cantilever of an atomic force microscope (AFM) are not properly adjusted, crosstalk effects will appear. These effects disturb measurements of the absolute vertical and horizontal cantilever deflections, which are involved in friction force microscopy (FFM). A straightforward procedure is proposed to study quantitatively crosstalk effects observed in scan-by-probe SPMs. The advantage of this simple, fast, and accurate procedure is that no hardware change or upgrade is needed. The results indicate that crosstalk effects depend not only on the alignment of the detector but also on the cantilever properties, position, and detection conditions. The measurements may provide information on the origin of the crosstalk effect. After determination of its magnitude, simple correction formulas can be applied to correct the crosstalk effects and then the single-load wedge method, using a commercially available grating, can be employed for accurate calibration of the lateral force.     

Energy dissipation and frequency shift of a damped dynamic force microscopy

The closed-form solution of the transient response of damped dynamic force microscopy subjected to the nonlinear interatomic force is derived. The frequency shift and the decay rate of a V-typed probe can be determined easily and precisely by the proposed method. If the taper ratio is zero, a uniform cantilever is obtained. Moreover, the transient response of a non-uniform cantilever can be determined also in the same way. The complex Young's modulus is used to describe the viscoelastic material property. In the modulus, the loss factor is introduced. The relation between the Q-factor and the loss factor is discussed. Moreover, the relation between the energy dissipation and the frequency shift is revealed. Finally, the effects of several parameters on the Q-factor, the frequency shift and the decay rate are investigated. The proposed method can be easily applied to investigate the tapping mode of AFM.     

Precise atomic force microscope cantilever spring constant calibration using a reference cantilever array

A method for calibrating the stiffness of atomic force microscope (AFM) cantilevers is demonstrated using an array of uniform microfabricated reference cantilevers. A series of force-displacement curves was obtained using a commercial AFM test cantilever on the reference cantilever array, and the data were analyzed using an implied Euler-Bernoulli model to extract the test cantilever spring constant from linear regression fitting. The method offers a factor of 5 improvement over the precision of the usual reference cantilever calibration method and, when combined with the Systeme International traceability potential of the cantilever array, can provide very accurate spring constant calibrations.     

A new model for investigating the flexural vibration of an atomic force microscope cantilever

A new model for the flexural vibration of an atomic force microscope cantilever is proposed, and a closed-form expression is derived. The effects of angle, damping and tip moment of inertia on the resonant frequency were analysed. Because the tip is not exactly located at one end of the cantilever, the cantilever is modelled as two beams. The results show that the frequency first increases with increase in angle and then decreases to a constant value for high values of the angle. Moreover, the damping is increased at lower contact positions. The tip moment of inertia is also sensitive to the resonant frequency at small values for the odd modes and large values for the even modes.     

原子力显微镜矩形测力臂弹性系数计算方法研究

原子力显微镜测力臂弹性系数的准确性直接影响其测量精度,是仪器标定的一个重要指标。分别运用理论计算方法、动态计算方法和静态计算方法计算原子力显微镜测力臂弹性系数。以矩形测力臂为例,对其进行灵敏度分析,找出影响测力臂弹性系数的参数。分别选取矩形测力臂原始参数值及参数上下极限值,构成3组实验数据。利用上述3种计算方法,分别计算出3组不同参数值的矩形测力臂的弹性系数,然后对这3种计算方法计算所得的弹性系数进行分析并和生产商给出的名义值进行比较,所得结果为原子力显微镜矩形测力臂弹性系数的精确计算提供参考。     

Topography imaging with a heated atomic force microscope cantilever in tapping mode

This article describes tapping mode atomic force microscopy (AFM) using a heated AFM cantilever. The electrical and thermal responses of the cantilever were investigated while the cantilever oscillated in free space or was in intermittent contact with a surface. The cantilever oscillates at its mechanical resonant frequency, 70.36 kHz, which is much faster than its thermal time constant of 300 micros, and so the cantilever operates in thermal steady state. The thermal impedance between the cantilever heater and the sample was measured through the cantilever temperature signal. Topographical imaging was performed on silicon calibration gratings of height 20 and 100 nm. The obtained topography sensitivity is as high as 200 microVnm and the resolution is as good as 0.5 nmHz(1/2), depending on the cantilever power. The cantilever heating power ranges 0-7 mW, which corresponds to a temperature range of 25-700 degrees C. The imaging was performed entirely using the cantilever thermal signal and no laser or other optics was required. As in conventional AFM, the tapping mode operation demonstrated here can suppress imaging artifacts and enable imaging of soft samples.     

Jumping mode AFM imaging of biomolecules in the repulsive electrical double layer

We present a method to image single biomolecules in aqueous media by atomic force microscope (AFM) without establishing any mechanical contact between the tip and the sample. It works by placing the feedback set point in the repulsive electrical double-layer curve just before the mechanical instability occurs. We use the jumping operation mode, where the set point is controlled at every image point and a stable imaging is achieved for several hours. This is a necessary condition for this method to be operative, otherwise the tip can fall in contact in a short time. The method is applied to image single-avidin protein molecules deposited on cleaved mica. In addition, the dependence of the height of avidin molecules as a function of ion concentration, due to differences in surface charge density of mica and avidin, is tentatively used to deduce relative values of these quantities.     

Ferrule-top atomic force microscope

Ferrule-top cantilevers are a new generation of all-optical miniaturized devices for utilization in liquids, harsh environments, and small volumes [G. Gruca et al., Meas. Sci. Technol. 21, 094033 (2010)]. They are obtained by carving the end of a ferruled fiber in the form of a mechanical beam. Light coupled from the opposite side of the fiber allows detection of cantilever deflections. In this paper, we demonstrate that ferrule-top cantilevers can be used to develop ultra compact AFMs for contact mode imaging in air and in liquids with sensitivity comparable to that of commercial AFMs. The probes do not require any alignment procedure and are easy to handle, favoring applications also outside research laboratories.     

Note: vibration reduction control of an atomic force microscope using an additional cantilever

Since an atomic force microscope is used to measure sub-nanometer level precision, it is sensitive to external vibration. If the vibration can be measured by using an additional sensor, we can obtain the vibration-free signal by subtracting the vibration signal from the signal containing the vibration. To achieve a highly effective vibration rejection ratio, it is important to decide where to locate the additional sensor. This is because the vibration measured at the sensing position should have the same phase as that of the vibration in the signal. Vibration reduction control using this electrical sensing method is verified through time domain analysis and topology images of a standard grid sample.     

Single-molecule avidin-biotin association reaction studied by force-clamp spectroscopy

Using single-molecule force-clamp spectroscopy, where the distance between the AFM tip and the sample surface is fixed and a few parallel avidin-biotin complexes are kept stretched by a certain force, we were able to observe the formation of single avidin-biotin bonds. Perspectives to use such an approach to study association reactions at single-molecule level in the conditions resembling those characteristic for some processes in vivo (e.g. virus-cell membrane attachment) are briefly discussed.