Features of sample preparation and atomic force microscopy study of dispersed nanomaterials

Techniques for preparing samples of highly dispersed materials of different chemical nature for studying their surface using atomic force microscopy were considered. Advantages and disadvantages of the techniques were determined. By the examples of nanodispersed carbon, iron oxide (III), and A-300 aerosil, the possibility of forming a nanoparticle sample whose surface morphology does not significantly change in comparison with initial particles is shown.     

A comparison of atomic force microscopy (AFM) and dynamic light scattering (DLS) methods to characterize nanoparticle size distributions

This paper compares the accuracy of conventional dynamic light scattering (DLS) and atomic force microscopy (AFM) for characterizing size distributions of polystyrene nanoparticles in the size range of 20–100 nm. Average DLS values for monosize dispersed particles are slightly higher than the nominal values whereas AFM values were slightly lower than nominal values. Bimodal distributions were easily identified with AFM, but DLS results were skewed toward larger particles. AFM characterization of nanoparticles using automated analysis software provides an accurate and rapid analysis for nanoparticle characterization and has advantages over DLS for non-monodispersed solutions.     

Influence of quantum dots shape approximation on size reconstructed from atomic force microscopy measurements

In this work we discuss the influence of the atomic force microscopy (AFM) probe tip geometry and the object — quantum dot form on the quantum dots dimension in the growth plane reconstructed from the AFM measurements. It is shown that ignoring the geometry of the probe tip and the quantum dot leads to significant differences between dimensions obtained from the AFM measurements and the real dimensions. Inaccuracies in QD size determination of the nano-objects from AFM measurements are defined.     

Nanoscopic measurements of the electrostriction responses in P(VDF/TrFE) ultra-thin-film copolymer using atomic force microscopy

Atomic force microscopy (AFM) has been used as a new method to perform nanoscale measurements of the electrostriction coefficients in the lamellae structure of the ferroelectric P(VDF/TrFE) 73/27 copolymers. The result found shows that the electrostriction coefficient inside (in the middle of) the lamella crystals is 6×10^-19 (m²V^-2), which is three times larger than that at the boundary, 2×10^-19 (m²V^-2). To explain the dependence of the electrostriction coefficients with those two regions, some suggestions are proposed. By heat treatment at 140 °C during 2 h, the sample changed its morphology as well as its crystallinity; the amorphous phase is much reduced and the degree of the crystallinity inside the lamellae is higher than that in the border. Also, it is suggested that in the lamellae’s boundary the macromolecular chains come to an end, or one monolayer folds over the other layer. In this case, the electrostriction was suppressed due to the loss of surface energy in the lamellae’s boundary. The achievements will supply a guideline to develop new and better devices for electromechanical and actuator applications. Received: 23 June 2000 / Accepted: 23 August 2000 / Published online: 5 October 2000     

试样激励下轻敲模式原子力声显微镜的非线性动力学特性

利用Euler-Bernoulli梁理论和DMT针尖-样品作用力模型建立了试样激励下轻敲模式原子力声显微镜(AFAM)系统的动力学方程,并应用非线性动力学分析方法对AFAM微悬臂梁的振动特性进行研究。通过合理改变超声激励幅值、超声激励频率和针尖-样品初始间距等模型参数模拟得到微悬臂梁的超谐波、次谐波、准周期和混沌振动现象,采用时间序列、频谱、相空间、Poincare截面和Lyapunov指数等方法对不同非线性振动特性进行表征。通过分析不同模型参数条件下微悬臂梁针尖-样品作用力特性,探索了微悬臂梁不同非线性振动现象的产生机制。此外,研究了AFAM微悬臂梁运动的分岔特性,发现当超声激励幅值和针尖-样品初始间隙连续变化时,周期、准周期和混沌运动交替出现。研究结果对AFAM系统非线性动力学行为分析和混沌振动控制提供了理论参考。     

Surface structure investigations using noncontact atomic force microscopy

Surfaces of several A_IIIB_V compound semiconductors (InSb, GaAs, InP, InAs) of the (0 0 1) orientation have been studied with noncontact atomic force microscopy (NC-AFM). Obtained atomically resolved patterns have been compared with structural models available in the literature. It is shown that NC-AFM is an efficient tool for imaging complex surface structures in real space. It is also demonstrated that the recent structural models of III-V compound surfaces provide a sound base for interpretation of majority of features present in recorded patterns. However, there are also many new findings revealed by the NC-AFM method that is still new experimental technique in the context of surface structure determination.     

Single-spin measurements for quantum computation using magnetic resonance force microscopy

The quantum theory of a single-spin measurement using magnetic resonance force microscopy is presented. We use an oscillating cantilever-driven adiabatic reversal technique. The frequency shift of the cantilever vibrations is estimated. We show that the frequency shift causes the formation of a Schrödinger cat state for the cantilever. The interaction between the cantilever and the environment quickly destroys the coherence between the two cantilever trajectories. It is shown that using partial adiabatic reversals one can obtain a significant increase in the frequency shift. We discuss the possibility of sub-magneton spin density detection in molecules using magnetic resonance force microscopy.     

Thermomechanical properties of polymer nanolithography using atomic force microscopy

The temperature-dependent mechanical properties of polyethylene terephthalate (PET) polymers are investigated using force-distance curves, adhesion force, and atomic force microscope (AFM) nanolithography combined the heating techniques. The results show that the width of grooves on the polymers at 20-60 °C were in the range of 14-363 nm. The wear depth of the polymers increased with increasing heating temperature. A volume of 251.85-2422.66 μm(3) at a load of 30-50 nN with heating to 30-60 °C was removed, as compared to that of 26.60-70.30 μm(3) obtained at room temperature. The contact forces of PET started increasing at 9 nN, whereas the size of the holes was average at a pressure. The results may be of importance in explaining the heating relationship among adhesion force, volume removal rate, and pressure.     

Quantitative nanoscopic impedance measurements on silver-ion conducting glasses using atomic force microscopy combined with impedance spectroscopy

Nanoscopic impedance measurements were carried out on silver ion conducting glasses by coupling an impedance spectrometer with an atomic force microscope. When ac voltages were applied to a conducting AFM tip being in contact with the glass surface, silver nanoparticles were formed during the cathodic half cycle, which were not completely reoxidized in the anodic half cycle. We describe two protocols allowing for a controlled particle growth. The electrochemical oxidation/reduction processes led to low tip/sample interfacial impedances, and the formed silver particles acted as nanoelectrodes sensing the spreading resistance of the glass below the particles. We made a quantitative check of the spreading resistance formula under the assumption that spreading of the electric field is governed by the lateral diameter of the particles and found good agreement between the mean value of the local conductivities obtained at different tip positions and the macroscopic conductivity.     

Dynamic modeling of submerged nanoparticle pushing based on atomic force microscopy in liquid medium

This article introduces a theoretical analysis of submerged nanoparticle manipulation in liquid medium using the atomic force microscopy, and gives a review of the major differences between dry and submerged manipulation processes. In this regard, the manipulation is modeled by adding the influences of the hydrodynamic forces surface forces to the manipulation model in dry air. Then, the pushing of a gold nanoparticle of 50-nm radius on a silicon substrate at a velocity of 100 nm/s is simulated, and the dynamic behaviors of the tip and nanoparticle are investigated. The results show that, in water (as compared to air), the required manipulation force and time for nanoparticle sliding and rolling increase by 3.5 and 6.5%, for sliding and 2 and 4.3% for rolling, respectively. Also, in liquids with different viscosities, the critical values related to sliding and rolling have a maximum variation of 17 and 32% for the manipulation time, and 6 and 22% for the manipulation force, respectively, as compared to the critical values related to particle manipulation in air. Moreover, for various submerged lengths of the cantilever in water, the critical values related to sliding and rolling show a maximum time variation of 9 and 10.5%, and 7 and 7.2% (for the manipulation force), respectively. Qualitative comparisons between the obtained results and those of the existing experimental investigations show the advantages of the liquid medium for the manipulation purposes.     

Numerical study of the hydrodynamic drag force in atomic force microscopy measurements undertaken in fluids

When atomic force microscopy (AFM) is employed for in vivo study of immersed biological samples, the fluid medium presents additional complexities, not least of which is the hydrodynamic drag force due to viscous friction of the cantilever with the liquid. This force should be considered when interpreting experimental results and any calculated material properties. In this paper, a numerical model is presented to study the influence of the drag force on experimental data obtained from AFM measurements using computational fluid dynamics (CFD) simulation. The model provides quantification of the drag force in AFM measurements of soft specimens in fluids.The numerical predictions were compared with experimental data obtained using AFM with a V-shaped cantilever fitted with a pyramidal tip. Tip velocities ranging from 1.05 to 105 μm/s were employed in water, polyethylene glycol and glycerol with the platform approaching from a distance of 6000 nm. The model was also compared with an existing analytical model. Good agreement was observed between numerical results, experiments and analytical predictions. Accurate predictions were obtained without the need for extrapolation of experimental data. In addition, the model can be employed over the range of tip geometries and velocities typically utilized in AFM measurements.     

Three-dimensional molecular imaging using mass spectrometry and atomic force microscopy

We combine imaging ToF-SIMS depth profiling and wide area atomic force microscopy to analyze a test structure consisting of a 300 nm trehalose film deposited on a Si substrate and pre-structured by means of a focused 15-keV Ga⁺ ion beam. Depth profiling is performed using a 40-keV C₆₀⁺ cluster ion beam for erosion and mass spectral data acquisition. A generic protocol for depth axis calibration is described which takes into account both lateral and in-depth variations of the erosion rate. By extrapolation towards zero analyzed lateral area, an “intrinsic” depth resolution of about 8 nm is found which appears to be characteristic of the cluster-surface interaction process.     

Characterization of electrodeposited nickel film surfaces using atomic force microscopy

Microstructures of nickel surfaces electrodeposited on indium tin oxides coated glasses are investigated using atomic force microscopy. The fractal dimension D and Hurst exponent H of the nickel surface images are determined from a frequency analysis method proposed by Aguilar et al. [J. Microsc. 172 (1993) 233] and from Hurst rescaled range analysis. The two methods are found to give the same value of the fractal dimension D∼2.0. The roughness exponent α and growth exponent β that characterize scaling behaviors of the surface growth in electrodeposition are calculated using the height-difference correlation function and interface width in Fourier space. The exponents of α∼1.0 and β∼0.8 show that the surface growth does not belong to the universality classes theoretically predicted by statistical growth models.     

Determination of silicone coating Young's modulus using atomic force microscopy

The polymerisation degree of thin polymer coatings was checked by following the variation of their local mechanical properties. Atomic force microscope (AFM) was used in an indentation mode to investigate the mechanical characteristics of silicone coatings on polycarbonate substrates. The evolution of Young's modulus of the silicone coatings was determined as a function of the polymer annealing time. We have used a relative method to measure Young's moduli, which involves a calibration step with a set of reference polymers. No variation was observed for the modulus of silicone coatings annealed during more than 40 min at 130 °C. This result indicates that over-heating does not modify the mechanical properties of the coating.     

Measurement of nanomechanical properties of biomolecules using atomic force microscopy

The capabilities of atomic force microscopy (AFM) have been rapidly expanding beyond topographical imaging to now allow for the analysis of a wide range of properties of diverse materials. The technique of nanoindentation, traditionally performed via dedicated indenters can now be reliably achieved using AFM instrumentation, enabling mechanical property determination at the nanoscale using the high spatial and force resolutions of the AFM. In the study of biological systems, from biomolecules to complexes, this technique provides insight into how mesoscale properties and functions may arise from a myriad of single biomolecules. In vivo and in situ analyses of native structures under physiological conditions as well as the rapid analysis of molecular species under a variety of experimental treatments are made possible with this technique. As a result, AFM nanoindentation has emerged as a critical tool for the study of biological systems in their natural state, further contributing to both biomaterial design and pharmacological research. In this review, we detail the theory and progression of AFM-based nanoindentation, and present several applications of this technique as it has been used to probe biomolecules and biological nanostructures from single proteins to complex assemblies. We further detail the many challenges associated with mechanical models and required assumptions for model validity. AFM nanoindentation capabilities have provided an excellent improvement over conventional nanomechanical tools and by integration of topographical data from imaging, enabled the rapid extraction and presentation of mechanical data for biological samples.     

Topographical observation of silane-treated inorganic surface using atomic force microscopy

The topography of the silane-treated layer on an inorganic surface was observed using an atomic force microscope. For this purpose, the cleaved mica plate was treated with some silane coupling agent at varying conditions. The silanes having aminopropyl or methacryloxypropyl group as organofunctional groups with di- or trialkoxyl structures were used. Three different solvents for silane solution — 2-propanol, 2-propanol/water mixture and water — were used. The pH of the aqueous solution was controlled. As a result, the most suitable solvent and pH in order to obtain smooth silane layer was clarified. The solubility of silane molecules in the solution, the wettability of silane molecule onto inorganic surface, and prevention of the mutual condensation of silane molecules in the solution were found to be important parameters for this purpose.     

Quantitative determination of contact stiffness using atomic force acoustic microscopy

Atomic force acoustic microscopy is a near-field technique which combines the ability of ultrasonics to image elastic properties with the high lateral resolution of scanning probe microscopes. We present a technique to measure the contact stiffness and the Young's modulus of sample surfaces quantitatively, with a resolution of approximately 20 nm, exploiting the contact resonance frequencies of standard cantilevers used in atomic force microscopy. The Young's modulus of nanocrystalline ferrite films has been measured as a function of oxidation temperature. Furthermore, images showing the domain structure of piezoelectric lead zirconate titanate ceramics have been taken.     

Adaptive semi-empirical model for non-contact atomic force microscopy

Non-contact atomic force microscope is a powerful tool to investigate the surface topography with atomic resolution. Here we propose a new approach to estimate the interaction between its tips and samples, which combines a semi-empirical model with density functional theory (DFT) calculations. The generated frequency shift images are consistent with the experiment for mapping organic molecules using CuCO, Cu, CuCl, and CuO_x tips. This approach achieves accuracy close to DFT calculation with much lower computational cost.