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.     

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.     

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.     

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.     

Energy dissipation and dynamic response of an amplitude-modulation atomic-force microscopy subjected to a tip-sample viscous force

In a common environment of atomic force microscopy (AFM), a damping force occurs between a tip and a sample. The influence of damping on the dynamic response of a cantilever must be significant. Moreover, accurate theory is very helpful for the interpretation of a sample's topography and properties. In this study, the effects of damping and nonlinear interatomic tip-sample forces on the dynamic response of an amplitude-formulation AFM are investigated. The damping force is simulated by using the conventional Kelvin-Voigt damping model. The interatomic tip-sample force is the attractive van der Waals force. For consistance with real measurement of a cantilever, the mathematical equations of the beam theory of an AM-AFM are built and its analytical solution is derived. Moreover, an AFM system is also simplified into a mass-spring-damper model. Its exact solution is simple and intuitive. Several relations among the damping ratio, the response ratio, the frequency shift, the energy dissipation and the Q-factor are revealed. It is found that the resonant frequencies and the phase angles determined by the two models are almost same. Significant differences in the resonant quality factors and the response ratios determined by using the two models are also found. Finally, the influences of the variations of several parameters on the error of measuring a sample's topography are investigated.     

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.     

Reduction of frequency noise and frequency shift by phase shifting elements in frequency modulation atomic force microscopy

We recently reported the analysis of the frequency noise in the frequency modulation atomic force microscopy (FM-AFM) both in high-Q and low-Q environments [Rev. Sci. Instrum. 80, 043708 (2009)]. We showed in the paper that the oscillator noise, the frequency fluctuation of the oscillator, becomes prominent in the modulation frequency lower than f(0)∕2Q, where f(0) and Q are the resonance frequency and Q-factor. The magnitude of the oscillator noise is determined by the slope of the phase versus frequency curve of the cantilever at f(0). However, in actual FM-AFM in liquids, the phase versus frequency curve may not be always ideal because of the existence of various phase shifting elements (PSEs). For example, the spurious resonance peaks caused by the acoustic excitation and a band-pass filter in the self-oscillation loop increase the slope of the phase versus frequency curve. Due to those PSEs, the effective Q-factor is often increased from the intrinsic Q-factor of the cantilever. In this article, the frequency noise in the FM-AFM system with the PSEs in the self-oscillation loop is analyzed to show that the oscillator noise is reduced by the increase of the effective Q-factor. It is also shown that the oscillation frequency deviates from the resonance frequency due to the increase of the effective Q-factor, thereby causing the reduction in the frequency shift signal with the same factor. Therefore the increase of the effective Q-factor does not affect the signal-to-noise ratio in the frequency shift measurement, but it does affect the quantitativeness of the measured force in the FM-AFM. Furthermore, the reduction of the frequency noise and frequency shift by the increase of the effective Q-factor were confirmed by the experiments.     

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.     

Electrostatic force microscopy measurements of charge trapping behavior of Au nanoparticles embedded in metal-insulator-semiconductor structure

Charge trapping properties of electrons and holes in Au nanoparticles embedded in metal-insulator-semiconductor (MIS) on p-type Si (100) substrates were investigated by electrostatic force microscopy (EFM). The Au nanoparticles were prepared with a unique laser irradiation method and charged by applying a bias voltage between EFM tip and sample. The EFM system was used to image charged areas and to determine quantitatively the amount of stored charge in the Au nanoparticle-inserted MIS structure. In addition, charge trapping characteristics of the samples were carried out with electrical measurements, such as capacitance-voltage and current-voltage measurement for memory characteristics. Finally, the comparison of EFM results with the electrically measured data was done to determine the amount of stored charge in the Au nanoparticle-inserted MIS structure, confirming the usefulness of EFM system for the characterization of nanoparticle-based non-volatile devices.     

Probe three-dimensional structure of soft organized surfactants at solid-liquid interface with an AFM in MAC Mode and contact mode

Atomic force microscopy provides a unique direct-visualization tool to study the three-dimensional structure of adsorbed surfactants on solid surfaces. Ionic surfactant molecules spontaneously adsorbed onto hydrophilic surfaces from aqueous solution above the critical micelle concentration (cmc) have been imaged using an atomic force microscope in magnetic ac mode (MAC Mode) and contact mode. It was found that the soft organized surfactants were highly compressible and therefore showed a wide range of corrugations depending on imaging forces. When using gentle MAC Mode, corrugations of the organized surfactants around half of the estimated height of the proposed surfactant aggregate cylinders on mica have been stably observed. Traditional contact mode operating in the pre-contact double-layer electrostatic interaction region, however, showed significantly reduced height of the organized molecules.     

Amplitude and frequency modulation torsional resonance mode atomic force microscopy of a mineral surface

Scanning probe imaging in a shear force mode allows for the characterization of in-plane surface properties. In a standard AFM, shear force imaging can be realized by the torsional resonance mode. In order to investigate the imaging conditions on mineral surfaces, a torsional resonance mode atomic force microscope was operated in amplitude (AM) and frequency modulation (FM) feedback. Freshly cleaved chlorite was investigated, which showed brucite-like and talc-like surface areas. In constant amplitude FM mode, a slight variation in energy dissipation was observed between both surfaces. Amplitude and frequency vs. distance curves revealed that the tip was in repulsive contact with the specimen during imaging.     

Study of the antibacterial effects of chitosans on Bacillus cereus (and its spores) by atomic force microscopy imaging and nanoindentation

Bacillus cereus is a Gram-positive, spore-forming bacterium that is widely distributed in nature. Its intrinsic thermal resistance coupled with the extraordinary resistance against common food preservation techniques makes it one of the most frequent food-poisoning microorganisms causing both intoxications and infections. In order to control B. cereus growth/sporulation, and hence minimize the aforementioned hazards, several antimicrobial compounds have been tested. The aim of this work was to assess by atomic force microscopy (AFM) the relationship between the molecular weight (MW) of chitosan and its antimicrobial activity upon both vegetative and resistance forms of B. cereus. The use of AFM imaging studies helped us to understand how chitosans with different MW act differently upon B. cereus. Higher MW chitosans (628 and 100 kDa) surrounded both forms of B. cereus cells by forming a polymer layer—which eventually led to the death of the vegetative form by preventing the uptake of nutrients yet did not affect the spores since these can survive for extended periods without nutrients. Chitooligosaccharides (COS) (<3 kDa), on the other hand, provoked more visible damages in the B. cereus vegetative form—most probably due to the penetration of the cells by the COS. The use of COS by itself on B. cereus spores was not enough for the destruction of a large number of cells, but it may well weaken the spore structure and its ability to contaminate, by inducing exosporium loss.     

Effect of SP-C on surface potential distribution in pulmonary surfactant: Atomic force microscopy and Kelvin probe force microscopy study

The air–lung interface is covered by a molecular film of pulmonary surfactant (PS). The major function of the film is to reduce the surface tension of the lung's air–liquid interface, providing stability to the alveolar structure and reducing the work of breathing. Earlier we have shown that function of bovine lipid extract surfactant (BLES) is related to the specific molecular architecture of surfactant films. Defined molecular arrangement of the lipids and proteins of the surfactant film also give rise to a local highly variable electrical surface potential of the interface. In this work we investigated a simple model of artificial lung surfactant consisting of DPPC, eggPG, and surfactant protein C (SP-C).     

Characteristics of a dynamic atomic force microscopy based on a higher-order resonant silicon cantilever and experiments

In order to improve the sensitivity and scanning speed of the dynamic AFM, a surface scanning method using higher-order resonant cantilever is adopted and investigated based on the higher-order resonance characteristics of the silicon cantilever, and the theoretical analysis and experimental verification on the higher-order resonance characteristics of the corresponding dynamic AFM cantilever are given. In this method, the cantilever is excited to oscillate near to its higher-order resonant frequency which is several times higher than that of the fundamental mode. Then the characteristic changes a lot compared with the first-order resonant cantilever. Because of the changes of the quality factor, amplitude and the mode shape of the cantilever, the higher-order resonant AFM gets higher sensitivity and scanning speed. Based on the home-built tapping-mode AFM experiment system, the resolution and the response time of the first and second order resonance measured by experiment are respectively: 0.83 nm, 0.42 nm; 1265 μs, 573 μs. The higher-order resonance cantilever has higher sensitivity and the dynamic measurement performance of the cantilever is significantly improved from the experimental results. This can be a useful method to develop AFM with high speed and high sensitivity. Besides above, the surface profile of a grating sample and its three-dimensional topography are obtained by the higher-order resonant mode AFM.     

Atomic force microscopy study of the antibacterial effects of chitosans on Escherichia coli and Staphylococcus aureus

Chitosan has been reported to be a non-toxic, biodegradable antibacterial agent. The aim of this work was to elucidate the relationship between the molecular weight of chitosan and its antimicrobial activity upon two model microorganisms, one Gram-positive (Staphylococcus aureus) and one Gram-negative (Escherichia coli). Atomic force microscopy (AFM) imaging was used to obtain high-resolution images of the effect of chitosans on the bacterial morphology. The AFM measurements were correlated with viable cell numbers, which show that the two species reacted differently to the high- and low-molecular-weight chitosan derivatives. The images obtained revealed not only the antibacterial effects, but also the response strategies used by the bacteria; cell wall collapse and morphological changes reflected cell death, whereas clustering of bacteria appeared to be associated with cell survival. In addition, nanoindentation experiments with the AFM revealed mechanical changes in the bacterial cell wall induced by the treatment. The nanoindentation results suggested that despite little modification observed in the Gram-positive bacteria in morphological studies, cell wall damage had indeed occurred, since cell wall stiffness was reduced after chitooligosaccharide treatment.     

Explanation and correction of false step heights in amplitude modulation atomic force microscopy measurements on alkane films

We use a prototypical alkane film (n-C(32)H(66) or C32) adsorbed on a SiO(2) surface to compare step heights measured by amplitude modulation atomic force microscopy (AM-AFM) with those measured in the contact mode. The C32 film exhibits layers in which the molecules are oriented with their long axis parallel to the SiO(2) surface followed by partial layers of perpendicular molecules. We show that step heights measured in the AM and contact modes agree in all cases except where the step is between a surface formed by a layer of parallel molecules and one of perpendicular molecules. In this case, the AM mode gives a false step height that is as much as 20% lower than that measured in the contact mode and inferred from synchrotron X-ray specular reflectivity measurements. We propose that the weaker van der Waals forces between the AFM tip and a perpendicular layer compared to a parallel layer causes this discrepancy. We show how to correct the false step height by using the approximately linear relationship observed between phase angle (cantilever oscillation relative to the drive signal) and cantilever height measured in an approach curve.     

Comparative study of a block copolymer morphology by transmission electron microscopy and scanning force microscopy

Using transmission electron microscopy (TEM) and scanning force microscopy (SFM) together, it was possible to verify important structural features of a nanostructured bulk material such as the kp‐morphology in an ABC triblock copolymer. By applying suitable imaging techniques during the SFM measurements it was possible to determine the morphology without additional manipulation steps in between. In comparison, TEM investigations on this type of material usually require selective staining procedures prior to the measurement. Also electron beam damage is often encountered during TEM measurements especially if components such as poly(methacrylates) are present. In contrast, SFM measurements can be assumed not to significantly change the phase dimensions of the components.     

The effect of fluid properties and geometrical parameters of cantilever on the frequency response of atomic force microscopy

Nowadays, the atomic force microscopy plays an indispensable role in imaging and manipulation of biological samples. To observe some specific behaviors and biological processes, fast and accurate imaging techniques are required, and one way to speed up the imaging process is to use short cantilevers. For short beams, the Timoshenko model seems to be more accurate compared to other models such as the Euler–Bernoulli. By using the Timoshenko beam model, the effects of rotational inertia and shear deformation are taken into consideration. In this paper, the frequency response of a rectangular atomic force microscope (AFM) in liquid environment has been analyzed by using the Timoshenko beam model. Afterward, since the dynamic response of AFM is influenced by the applied medium, the effects of physical and mechanical properties (e.g., fluid density and viscosity) on the frequency response of the system have been investigated. The frequency responses of the AFM cantilever immersed in various liquids have been compared with one another. And eventually, to study the influence of geometry on the dynamic behavior of AFM, the effect of the cantilever's geometrical parameters (e.g., cantilever length, width and thickness) on the frequency response of the system has been studied.