Effect of tip mass on frequency response and sensitivity of AFM cantilever in liquid

The effect of tip mass on the frequency response and sensitivity of atomic force microscope (AFM) cantilever in the liquid environment is investigated. For this purpose, using Euler–Bernoulli beam theory and considering tip mass and hydrodynamic functions in a liquid environment, an expression for the resonance frequencies of AFM cantilever in liquid is derived. Then, based on this expression, the effect of the surface contact stiffness on the flexural mode of a rectangular AFM cantilever in fluid is investigated and compared with the case where the AFM cantilever operates in the air. The results show that in contrast with an air environment, the tip mass has no significant impact on the resonance frequency and sensitivity of the AFM cantilever in the liquid. Hence, analysis of AFM behaviour in liquid environment by neglecting the tip mass is logical.     

Observations of fission-tracks in zircons by atomic force microscope

The fission-track (FT) method is a dating technique based on the observation of damage (tracks) by spontaneous fission of ²³⁸U left in a mineral. The date is calculated from the track density and the uranium concentration in the mineral. This is possible because the number of tracks is a function of uranium concentration and time since the start of track accumulation. Usually, the number of tracks is counted under an optical microscope after etching (chemical expansion of a track). However, as FT density per unit area rises, it becomes difficult to count the number of tracks. This is due to the fact that FTs overlap one another and are unable to be readily distinguished. This research examines the potential of atomic force microscope (AFM) for FT dating using zircons, which are likely to show higher FT density than other minerals due to their high U concentrations.To obtain an AFM image for a sample prepared for FT dating, removing the static electricity of the sample is essential to avoid an unexpected movement of the cantilever. A grain should be wider than about 30 μm to bring the cantilever on the mineral surface. Polishing with a fine grained compound is very important. There is not much difference in sharpness between images by AC mode (scanning with vibrating cantilever at a constant cycle) and Contact mode (scanning with the cantilever always in close contact with the surface). To confirm how tracks can be identified with the AFM, an AFM image was compared with an image obtained with the optical microscope. When change in the number of tracks and their shapes were observed through stepwise etching, the track expanded as the etching time increased. In addition, the etching rate was slower for large tracks than those for small tracks. This implied that the AFM can be used to observe etching of zircons with different degrees of nuclear fission damage. A track that could not be seen with the optical microscope due to insufficient etching could be observed by AFM methods, indicating the possibility of FT dating with high track densities using AFM after relatively short etching periods.     

Probing into adsorption behavior of human plasma fibrinogen on self-assembled monolayers with different chemical properties by scanning probe microscopy

The adsorption behaviors of fibrinogen on the self-assembled monolayers (SAMs) with different chemical properties were investigated using an atomic force microscopy (AFM). AFM images indicated that the adsorption amounts of fibrinogen molecules increased with an increase of the surface hydrophobicity. High-resolution AFM imaging revealed that the fibrinogen conformations adsorbed on the SAM surface changed with dependent on the surface chemistry. The adsorption models of fibrinogen molecules adsorbed on SAM surfaces with different chemical properties were proposed based on the high-resolution AFM images.     

Material anisotropy revealed by phase contrast in intermittent contact atomic force microscopy

Phase contrast in intermittent-contact atomic force microscopy (AFM) reveals in-plane structural and mechanical properties of polymer monolayers. This is surprising, because measurements of nanoscale in-plane properties typically require contact mode microscopies. Our measurements are possible because the tip oscillates not just perpendicular but also parallel to the sample surface along the long axis of the cantilever. This lateral tip displacement is virtually universal in AFM, implying that any oscillating-tip AFM technique is sensitive to in-plane material properties.     

Hydrodynamic interaction of AFM cantilevers with solid walls: an investigation based on AFM noise analysis

The noise power spectrum of the thermally activated motion of an AFM cantilever has been analyzed with respect to viscoelastic and hydrodynamic coupling between the cantilever and a substrate surface. Spheres with radii between 5 and 25 microm were glued to the cantilever to provide a well-defined geometry. The cantilever is modeled as a harmonic resonator with a frequency-dependent complex drag coefficient xi(omega). The variation of the drag coefficient xi(omega) with the tip-sample distance, D, and the sphere radius, R, can be expressed as a function of the single dimensionless parameter D/ R. However, this scaling breaks down close to the surface. There are two sources of a frequency dependence of xi(omega), which are viscoelastic memory and hydrodynamics. Viscoelastic relaxation is observed when the surface is covered with a soft polymer layer. In the absence of such a soft layer one still finds a frequency dependence of xi(omega) which is caused by hydrodynamics. At large substrate-cantilever distances, the drag coefficient increases with frequency because of inertial effects. At small distances, on the other hand, the drag coefficient decreases with increasing frequency, which is explained by the reflection of shear waves from the substrate surface. In liquids, inertial effects can be important when performing dynamic AFM experiments.     

Surface defects characterization with frequency and force modulation atomic force microscopy using molecular dynamics simulations

This paper is devoted to the characterization of the surface defects using a recently developed AFM technique called frequency and force modulation AFM (FFM–AFM). The simulated system includes a recently developed gold coated AFM probe which interacts with a sample including single-atom vacancy and impurities. In order to examine the behavior of the above system on different transition metals, the molecular dynamics (MD) simulation with Sutton–Chen (SC) inter-atomic potential is used. In this study, an online imaging simulation of the probe and sample is performed, and the effects of the horizontal scan speed, the effective frequency set-point, the cantilever stiffness, the tip-sample rest position and the cantilever quality factor on the resulting images are investigated. Using a proposed optimum controlling scheme for the excitation force amplitude, the cantilever horizontal speed can be increased.     

Giant enhancement of noncontact friction between closely spaced bodies by dielectric films and two-dimensional systems

The effect of an external bias voltage and spatial variations of the surface potential on the damping of cantilever vibrations in an atomic force microscope (AFM) is considered. The damping is due to an electrostatic friction that arises due to dissipation of the energy of an electromagnetic field generated in the sample by oscillating static charges induced on the surface of the AFM probe tip by the bias voltage or spatial variations of the surface potential. A similar effect appears when the tip is oscillating in an electrostatic field created by charged defects present in the dielectric sample. The electrostatic friction is compared to the van der Waals (vdW) friction between closely spaced bodies, which is caused by a fluctuating electromagnetic field related to the quantum and thermal fluctuations of current density inside the bodies. It is shown that the electrostatic friction and the vdW friction can be strongly enhanced in the presence of dielectric films or two-dimensional (2D) structures—such as a 2D electron system or an incommensurate layer of adsorbed ions exhibiting acoustic oscillations—on the probe tip and sample surfaces. It is also shown that the damping of cantilever oscillations caused by the electrostatic friction in the presence of such 2D structures can have the same order of magnitude and the same dependence on the distance as observed in experiment by Stipe et al. [Phys. Rev. Lett. 87, 096801 (2001)]. At small distances, the vdW friction can be large enough to be measured in experiment. In interpreting the experimental data that obey a quadratic dependence on the bias voltage, one can reject a phonon mechanism according to which the friction depends on the fourth power of the voltage.     

原子力显微镜探针耦合变形下的微观扫描力研究

原子力显微镜(AFM)的微探针系统是典型的微机械构件，它在接触扫描过程处于耦合变形状态.采用数值模拟方法探究恒力模式下探针耦合变形对微观扫描力信号、微观形貌信号的影响.研究表明，AFM的恒力模式扫描中，法向扫描力并不是恒定大小，与轴向扫描力存在耦合作用，在粗糙峰峰值增加阶段，二力均增加；在粗糙峰峰值减小阶段，二力均减小；该耦合作用随形貌坡度、针尖长度等增加而加强.微观形貌的测试信号和横向扫描侧向力信号受探针耦合变形影响较小，但侧向力与形貌斜率密切相关，且其极值点与形貌极值点存在位置偏差，这些结果均与原子力 关键词： 原子力显微镜 探针悬臂梁 耦合变形 扫描力     

Film morphology and orientation of amino silicone adsorbed onto cellulose substrate

A series of amino silicones with different amino values were synthesized and adsorbed onto surfaces of cotton fibers and cellulose substrates. The film morphology, hydrophobic properties and surface composition of the silicones are investigated and characterized by field emission scanning electron microscope (FESEM), atomic force microscope (AFM), contact angle measurement, X-ray photoelectron spectroscopy (XPS) and attenuated total reflectance infrared (ATR-IR). The results of the experiments indicate that the amino silicone can form a hydrophobic film on both cotton fibers and cellulose substrates and reduce the surface roughness significantly. Furthermore, the roughness becomes smaller with an increase in the amino value. All these results suggest that the orientation of amino silicone molecule is with the amino functional groups of amino silicone molecule adsorbed onto the cellulose interface while the main polymer chains and the hydrophobic Si-CH₃ groups extend toward the air.     

Adsorption of bovine serum albumin (BSA) on polystyrene (PS) and its acid copolymer

The effect of surface polarity on the adsorption of bovine serum albumin (BSA) on polystyrene (PS), 7% polystyrene-co-maleic anhydride (7%PSMAn) and 50% polystyrene-co-maleic acid (50%PSMA), at pH 7.4, was investigated. Polystyrene represented the non-polar surface while 7%PSMAn and 50%PSMA represented a low and high acid content copolymer. The amount of the adsorbed BSA depended on the amount of the acid content in the copolymer. BSA formed a monolayer with a side-on orientation on the low polarity PS surface, a mixed side-on and end-on orientation on 7%PSMAn and a predominantly side-on orientation on 50%PSMA. The thickness of adsorbed BSA, measured with an atomic force microscope (AFM), varied from 3 nm to 5 nm for the side-on orientation and from 10 nm to 15 nm for the end-on orientation. The average area occupied per BSA molecule was consistent with the proposed orientation, and was 34.8 nm², 27.8 nm² and 18.0 nm² for PS, 7%PSMAn and 50%PSMA, respectively. The adsorption showed a concentration dependency following the Freundlich isotherm, which indicated the interactions among adsorbed BSA molecules on the polymer surface. The adsorption took place as an island-like morphology and started to fuse into a patch-like morphology at higher concentrations before achieving a complete monolayer formation. A non-uniform surface coverage and defects were observed in all cases. It is recommended that for an effective blocking of PS, 7%PSMAn and 50%PSMA, the BSA concentration should be higher than 3 mg/mL.     

Immobilization of protein molecules on step-controlled sapphire surfaces

We have studied effects of surface morphology on immobilization of protein molecules using step-controlled sapphire surfaces. Preferential adsorption of avidin molecules on the step edges was observed on the single-stepped sapphire surface. A randomly-stepped sapphire surface was found to be suitable for high-density immobilization of protein molecules. These results indicate atomic scale structures of the substrate surface influence the adsorption efficiency of the proteins. By using an atomic force microscopy (AFM) equipped with a biotin-modified cantilever, we have confirmed that the immobilized avidin molecules on the substrates keep their biological activity. This means that the ligand-receptor interaction can be detected using the phase image mode of a standard AFM.     

Physical bounds of metallic nanofingers obtained by mechano-chemical atomic force microscope nanolithography

To obtain metallic nanofingers applicable in surface acoustic wave (SAW) sensors, a mechano-chemical atomic force microscope (AFM) nanolithography on a metallic thin film (50 nm in thickness)/piezoelectric substrate covered by a spin-coated polymeric mask layer (50-60 nm in thickness) was implemented. The effective shape of cross-section of the before and after etching grooves have been determined by using the AFM tip deconvolution surface analysis, structure factor, and power spectral density analyses. The wet-etching process improved the shape and aspect ratio (height/width) of the grooves and also smoothed the surface within them. We have shown that the relaxed surface tension of the polymeric mask layer resulted in a down limitation in width and length of the lithographed nanofingers. The surface tension of the mask layer can be changed by altering the initial concentration of the polymer in the deposition process. As the surface tension reduced, the down limitation decreased. In fact, an extrapolation of the analyzed statistical data has indicated that by decreasing the surface tension from 39 to 10 nN/nm, the minimum obtainable width and length of the metallic nanofingers was changed from about 55 nm and 2 μm to 15 nm and 0.44 μm, respectively. Using the extrapolation’s results, we have shown that the future SAW sensors buildable by this nanolithography method possess a practical bound in their synchronous frequency (∼58 GHz), mass sensitivity (∼6125 MHz-mm²/ng), and the limit of mass resolution (∼4.88 × 10⁻¹⁰ ng/mm²).     

Adsorption of polyampholytes on charged surfaces

We have studied the adsorption of neutral polyampholytes on model charged surfaces that have been characterized by contact angle and streaming current measurements. The loop size distributions of adsorbed polymer chains have been obtained using atomic-force microscopy (AFM) and compared to recent theoretical predictions. We find a qualitative agreement with theory; the higher the surface charge, the smaller the number of monomers in the adsorbed layer. We propose an original scenario for the adsorption of polyampholytes on surfaces covered with both neutral long-chain and charged short-chain thiols. Received 22 February 2002 and Received in final form 23 April 2002     

Time of flight grazing incidence small angle neutron scattering

Grazing incidence small angle neutron scattering (GISANS) overcomes the limitations of conventional small angle scattering with respect to extremely small sample volumes in the thin film geometry. In time of flight (TOF) mode neutrons with a broad range of wavelengths are used simultaneously and recorded as a function of their respective times of flight. The combination of both, TOF-GISANS, enables the simultaneous performance of several GISANS measurements, which differ in wavelength. As a consequence, within one measurement a full set of GISANS pattern related to different scattering vectors, different scattering depths and resolutions result. This allows the detection of nanostructures with a chemical sensitivity. The possibilities of TOF-GISANS are demonstrated by the simple example of polymer nano-dots located on top of a silicon surface. As probed with atomic force microscopy (AFM) the nano-dots exhibit a large characteristic nearest neighbour distance of 545 nm and a surface coverage of 28%. From the analysis of the wavelength dependent data in combination with AFM the mass density of the polymer nano-dots is determined to be equal to the bulk value. A comparison to common single wavelength GISANS experiments is shown.     

Optically driven actuators using poly(vinylidene difluoride)

Optically driven actuators have a feature of a non-contact method supplied by light energy. A new method is proposed with three poly(vinylidene difluoride) (PVDF) cantilevers as the legs and a polymer film as the body. The PVDF cantilevers are coated with silver on one surface. When one side of the cantilever is irradiated by a laser beam, an electric field is produced along a cross-section of the cantilever by the pyroelectric effect and a mechanical displacement occurs by the piezoelectric effect. Its response time and its generated force are measured experimentally. Two types of optically driven actuators using PVDF film are proposed to move using different characteristics.     

Analyses of vibration responses on nanoscale processing in a liquid using tapping-mode atomic force microscopy

An analytical solution of the vibration responses of biological specimens using atomic force microscopy (AFM), which often requires operation in a liquid, is developed. In this study, the modal superposition method is employed to analyze the vibration responses of AFM cantilevers in tapping mode (TM) operated in a liquid and in air. The hydrodynamic force exerted by the fluid on AFM cantilevers is approximated by additional mass and hydrodynamic damping. The tip–sample interaction forces were transformed into axial, distributed transversal, and bending loading, and then applied to the end region of the AFM through the tip holder. The effects of transverse stress and bending stress were adopted to solve the dynamic model. With this model, a number of simulations were carried out to investigate the relationship between the transient responses of the cantilever in a liquid and the parameters considered in nanoscale processing. The simulations show that the vibration of AFM cantilevers in a liquid has dramatically different dynamic characteristics from these of that in air. The liquid reduces the magnitude of the transversal response and reduces the cantilever resonances. Moreover, the magnitudes of response become larger with increasing intermolecular distances and smaller with decreasing tip length. The cantilever vibration amplitudes significantly depend on the damping constant and the mass proportionality constant.     

Adsorption and manipulation of carbon onions on highly oriented pyrolytic graphite studied with atomic force microscopy

Carbon onions produced by DC arc discharge method were deposited on highly oriented pyrolytic graphite (HOPG) surface and their adsorption and manipulation was studied using an atomic force microscopy (AFM). Well-dispersed adsorption of carbon onions on HOPG surface was obtained and aggregations of onions were not observed. The van der Waals interaction between the onion and HOPG surface and that between two onions, were calculated and discussed using Hamaker's theory. The manipulation of adsorbed onions on HOPG surface was realized using the AFM in both the raster mode and the vector mode. The controllability and precision of two manipulation modes were compared and the vector mode manipulation was found superior, and is a useful technique for the construction of nano-scale devices based on carbon onions.     

Surface modification study of low energy electron beam irradiated polycarbonate film

The effect of low energy electron beam irradiation on polycarbonate (PC) film has been studied here. The PC film of thickness 20 μm was exposed by 10 keV electron beam with 100 nA/cm² current density. The irradiated film was characterized by mean of X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM) and residual gas analyzer (RGA). Formation of unsaturated bonds and partial graphitization of the surface layer are measured by XPS. Results of the AFM imaging shows electron implantation induce changes in surface morphology of the polymer film. The residual gas analyzer (RGA) spectrum of PC is recorded in situ during irradiation. The results show the change in cross-linking density of the polymer at the top surface.     

Controlled assembly of DNA nanostructures on silanized silicon and mica surfaces for future molecular devices

In order to establish key technology for future molecular devices, we have explored the assembly behaviour of λ-deoxyribonucleic acid (DNA) molecules adsorbed on silanized mica and silanized oxide silicon surfaces by using atomic force microscopy (AFM). AFM experiments show that λ-DNA molecules can be hardly adsorbed on untreated mica and oxidized silicon surfaces, but can be strongly adsorbed onto aminosilanized mica and oxidized silicon surfaces. Importantly, DNA molecules can be assembled into linear DNA alignment, and can also self-assemble into various network structures on the silanized surfaces. Our experimental observations have demonstrated the feasibility of assembling DNA-based nanostructures by varying surface chemistry of substrates, and offer useful clues in constructing DNA-based nanodevices for nanoelectronics and biomolecular computation as well as quantum computation.     

How to measure energy dissipation in dynamic mode atomic force microscopy

When studying a mechanical system like an atomic force microscope (AFM) in dynamic mode it is intuitive and instructive to analyse the forces involved in tip–sample interaction. A different but complementary approach is based on analysing the energy that is dissipated when the tip periodically interacts with the sample surface. This method does not require solving the differential equation of motion for the oscillating cantilever, but is based entirely on the analysis of the energy flow in and out of the dynamic system. Therefore the problem of finding a realistic model to describe the tip–sample interaction in terms of non-linear force–distance dependencies and damping effects is omitted. Instead, it is possible to determine the energy dissipated by the tip–sample interaction directly by measuring such quantities as oscillation amplitude, frequency, phase shift and drive amplitude. The method proved to be important when interpreting phase data obtained in tapping mode, but is also applicable to a variety of scanning probe microscopes operating in different dynamic modes. Additional electronics were designed to allow a direct mapping of local energy dissipation while scanning a sample surface. By applying this technique to the cross-section of a polymer blend a material specific contrast was observed.