Electrical nanoprobing of semiconducting carbon nanotubes using an atomic force microscope

We use an atomic force microscope (AFM) tip to locally probe the electronic properties of semiconducting carbon nanotube transistors. A gold-coated AFM tip serves as a voltage or current probe in three-probe measurement setup. Using the tip as a movable current probe, we investigate the scaling of the device properties with channel length. Using the tip as a voltage probe, we study the properties of the contacts. We find that Au makes an excellent contact in the p region, with no Schottky barrier. In the n region, large contact resistances were found which dominate the transport properties.     

Surface modification of a biomedical polyethylene terephthalate (PET) by air plasma

In this work, low-pressure air plasma has been used to improve polyethylene terephthalate (PET) surface properties for technical applications. Surface free energy values have been estimated using contact angle value for different exposure times and different test liquids. Surface composition and morphology of the films were analyzed by X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). Surface topography changes related with the etching mechanism have been followed by weight loss study. The results show a considerable improvement in surface wettability and the surface free energy values even for short exposure times in the different discharge areas (discharge area, afterglow area and remote area), as observed by a remarkable decrease in contact angle values. Change of chemical composition made the polymer surfaces to be highly hydrophilic, which mainly depends on the increase in oxygen-containing groups. In addition to, the surface activation and AFM analyses show obvious changes in surface topography as a consequence of the plasma-etching mechanism.     

Evaluation of the contact resonance frequencies in atomic force microscopy as a method for surface characterisation (invited)

The combination of ultrasound with atomic force microscopy (AFM) opens the high lateral resolution of scanning probe techniques in the nanometer range to ultrasonics. One possible method is to observe the resonance frequencies of the AFM sensors under different tip-sample interaction conditions. AFM sensors can be regarded as small flexible beams. Their lowest flexural and torsional resonance frequencies are usually found to be in a range between several kHz and several MHz depending on their exact geometrical shape. When the sensor tip is in a repulsive elastic contact with a sample surface, the local indentation modulus can be determined by the contact resonance technique. Contact resonances in the ultrasonic frequency range can also be used to improve the image contrast in other dynamic techniques as, for example, in the so-called piezo-mode. Here, an alternating electric field is applied between a conducting cantilever and a piezoelectric sample. Via the inverse piezoelectric effect, the sample surface is set into vibration. This excitation is localised around the contact area formed by the sensor tip and the sample surface. We show applications of the contact resonance technique to piezoelectric ceramics.     

Influence of thermal fluctuations on the interactions between nanoscale particles

We present a method to investigate the influences of the thermal fluctuations on the nanometer-sized particle in pickup manipulation by an atomic force microscope (AFM). We show that thermal fluctuations can play an important and even major role in the interaction between particles at room temperature. Moreover, thermal fluctuations always have an opposing effect on the particle interactions. The deterministic directional motion of a particle governed by the interfacial properties of the nanoparticles becomes non-deterministic, with a reduction of the adhesion probability up to 44% under different strength of the thermal fluctuations.     

Does thermophoretic mobility depend on particle size?

Thermophoresis is particle drift induced by a temperature gradient. By measuring the full temperature dependence of this effect for polystyrene latex suspensions, we show that the thermophoretic mobility (or "thermal diffusion coefficient") D(T) is basically independent on particle size, in particular, when the interfacial properties of the colloidal particles are carefully standardized by adsorbing a surfactant layer on the particle surface. Even more, all investigated systems show values of D(T) which are very close to those measured for simple micellar solutions of the adsorbed surfactant. Our findings could be of relevance for downsizing microfluidics to the nanometric range.     

Surface investigation of adhesive formulation consisting of UV sensitive triblock poly(styrene–b-butadiene–b-styrene) copolymer

Atomic force microscopy (AFM) analysis in conjunction with macroscopic studies such as peel testing and contact angle measurement have been undertaken to explain the nanomechanical properties of adhesive formulation consisting of triblock poly(styrene–b-butadiene–b-styrene) (SBS) copolymers. The cross-linking of this photosensitive copolymer was investigated by analyzing the mechanical and morphological changes of each phase induced by the UV exposure. Main result is that the adhesive properties are strongly influenced by the cross-linking of the polybutadiene (PB) phase leading to an increase in the surface stiffness without affecting the surface energy. AFM analysis shows that the adhesion force is mostly governed by the contact area between the adhesive and the probe. The surface mobility may explain the increase in adhesion for this pressure sensitive copolymer.     

Local surface cleaning and cluster assembly using contact mode atomic force microscopy

Conventional contact mode atomic force microscopy (AFM) has been used for local surface cleaning and cluster alignment. By using the AFM tip to sweep and push in contact mode, we have demonstrated that Cu clusters, prepared by vacuum evaporation onto Dow Cyclotene 3022 polymer and subsequent exposure to atmosphere, can easily be moved by the AFM tip, and assembled at the outer edge of the scanned region to form a line of clusters. We have found that the force applied by the tip plays an important role in the ease of cluster motion. Cyclotene surface treatment that enhances cluster adhesion hinders this ability, and may be used as a method of nanofabrication.     

Growth, structure and electrical properties of tungsten oxide nanorods

Tungsten trioxide has shown good sensing properties towards various gases. Recently thin nanostructured WO₃ films have been tested. Due to their large surface area to volume ratio they exhibit good sensitivity depending on the grain size. However in conventional WO₃ thin films the average grain size exceeds the thickness of the surface space charge layer, so the electrical conduction is mainly controlled by the carriers transport across the grain boundaries. An alternative way seems to be in a monocrystalline material with nanometric dimensions. Our objective is to fabricate nanosized tungsten oxide rods and to test their sensing properties under gas adsorption. In this work, we focus on the growth, the structure and the electrical properties of tungsten nanorods. The tungsten oxide nanorods were grown by vapour transport from a WO₃ layer onto a substrate (Mica). The nanorods growth was controlled by the temperature gradient between the WO₃ layer and the substrate. Their morphology was investigated by AFM and their structure by TED and TEM. We have investigated the conductivity of the WO₃ nanorods with a technique derived from Atomic Force Microscopy operating in contact mode with a conductive tip (Resiscope).     

Enhanced surface atomic step motion observed in real time after nanoindentation of NaCl(100)

The nanometer-scale indentation of a crystalline surface produces nanostructures that evolve on a timescale that is inaccessible to existing imaging methods for the vast majority of surfaces. We have been able to observe the dynamic evolution of the freshly cleaved surface of a NaCl(100) crystal after indentation with an atomic force microscope (AFM) in air. Here we present sequential AFM images featuring vertical atomic resolution which show that atomic terrace motion is greatly enhanced by the AFM indentation. Moreover, some of the nanometric features generated by the indentation become reassimilated into the crystalline surface structure of the surroundings of the indentation over a period of time of the order of several minutes.     

Surface characterization of plasma deposited nano-structured fluorocarbon coatings for promoting in vitro cell growth

Nano-structured “teflon-like” coatings characterized by highly-fluorinated, random, ribbon-shaped, micrometers-long structures were deposited on polyethylenetherephtalate (PET) substrates by plasma enhanced-chemical vapour deposition (PE-CVD) using modulated radiofrequency (RF, 13.56 MHz) glow discharges fed with C₂F₄ in modulated discharge (MD) and continuous wave (CW) regimes. Surfaces obtained in this way featured identical chemical composition and different roughness in the nanometric scale. Water contact angle (WCA) measurements, scanning electron microscopy (SEM) and atomic force microscopy (AFM) were utilized to characterize the surfaces. A positive relationship was shown to exist between the WCA value and the mean nano-structure height and the area root-mean-square (RMS) roughness of coatings. The possibility of obtaining coatings of varying nano-structure height, i.e., roughness, in a nanometric scale represents a promising result for further use of these surfaces as substrates for experiments on cell adhesion, proliferation and growth.     

Tribological properties of silicate materials on nano and microscale

We studied the friction properties of four model silicate materials at the nanoscale and microscale. From nanotribology, we characterized the tribological properties at single asperity contact scale and from microtribology, we characterized the tribological properties at multi asperity contact scale. First, for each material we measured chemical composition by XPS, Young's modulus by acoustical microscopy and roughness σ by atomic force microscopy (AFM). Second, we measured the nanofriction coefficients with an AFM and the microfriction coefficients with a ball probe tribometer, for three hardnesses of the ball probe. We identified one friction mechanism at the nanoscale (sliding friction) and two friction mechanisms at the microscale (sliding friction and yielding friction). Comparison of the nano and microfriction coefficients at the same sliding friction regime shown, that the tribological properties of these materials didn’t depend on roughness.     

Computing Particle Surface Areas and Contact Areas from Three‐Dimensional Tomography Data of Particulate Materials

Microtomography is an emerging technique for particle and particulate‐materials characterization. To use this technology effectively, robust and accurate computational algorithms are needed to compute relevant particle properties, including particle surface area and particle‐particle contact area. However, the most accurate algorithms that have been developed for computing the exposed (void/solid) surface area in a microtomography image cannot be used directly for computing surface areas or particle‐particle contact areas for individual particles in a dense packing. This paper presents an algorithm for extracting particle contact areas from a digitized, segmented image of a packed granular material, which in turn can be used to find individual particle surface areas (even if the complete surfaces are not exposed because of contacts in the packing). Results show that small errors in the binary surface‐area computations are magnified in the course of determining particle contact areas; the total error in the computation depends mainly on the size of the contact area in voxel units.     

Metrology of electromagnetic static actuation of MEMS microbridge using atomic force microscopy

The objective of this paper is to describe application of atomic force microscopy (AFM) for characterization and calibration of static deflection of electromagnetically and/or thermally actuated micro-electromechanical (MEMS) bridge. The investigated MEMS structure is formed by a silicon nitride bridge and a thin film metal path enabling electromagnetic and/or thermal deflection actuation. We present how static microbridge deflection can be measured using contact mode AFM technology with resolution of 0.05 nm in the range of up to tens of nm. We also analyze, for very small structure deflections and under defined and controlled load force varied in the range up to ca. 32 nN, properties of thermal and electromagnetical microbridge deflection actuation schemes.     

基于扫描电子显微镜的碳纳米管拾取操作方法研究

碳纳米管场效应管是未来纳米器件的发展方向,而制造纳米器件的前提是拾取碳纳米管,基于扫描电子显微镜(SEM)的微纳机器人操作系统能够实现碳纳米管拾取操作.本文建立拾取操作中碳纳米管与原子力显微镜(AFM)探针间范德瓦耳斯力力学模型,不同接触状态下范德瓦耳斯力越大越有利于拾取碳纳米管.在SEM视觉反馈图像中建立相对坐标系,首先提出倾角变值方法检测碳纳米管与AFM探针的接触状态,然后运用动态差值方法识别碳纳米管与AFM探针空间位姿并校正碳纳米管位姿,最后自下而上拾取碳纳米管.实验结果表明:拟合直线倾角变值较大时碳纳米管与AFM探针发生接触,动态差值变化为零时碳纳米管与AFM探针为空间线接触,在完全线接触模型下选择合适的接触角度、接触长度和拾取速度能够成功拾取碳纳米管.     

Theory of higher harmonics imaging in tapping-mode atomic force microscopy

The periodic impact force induced by tip-sample contact in tapping mode atomic force microscope (AFM) gives rise to non-harmonic response of a micro-cantilever. These non-harmonic signals contain the full characteristics of tip-sample interaction. A complete theoretical model describing the dynamical behaviour of tip--sample system was developed in this paper. An analytic formula was introduced to describe the relationship between time-varying tip--sample impact force and tip motion. The theoretical analysis and numerical results both show that the time-varying tip--sample impact force can be reconstructed by recording tip motion. This allows for the reconstruction of the characteristics of the tip--sample force, like contact time and maximum contact force. It can also explain the ability of AFM higher harmonics imaging in mapping stiffness and surface energy variations.     

Investigation into layers formed by selective transfer CMP mechanisms with atomic force microscope

To understand mechanisms of chemical mechanical planarization (CMP), an atomic force microscope (AFM) was used to characterize polished layer surfaces formed by selective transfer after a set of polishing experiments. It is know that in the process of friction of two materials and in the presence of own lubricants, wear phenomenon itself manifests as a transfer of material from an element of a friction couple on the other, this phenomenon being characteristic to the selective transfer process. A selective transfer can be safely achieved in a friction couple, if there is a favorable energy, and in the presence of relative movement, if in the friction area is a material made by copper and the lubricant is adequate (glycerin or special lubricant). The forming selective layer on the contact surfaces makes that the friction force to be very low because of the structure formed by selective transfer. To optimize the CMP process, one needs to obtain information on the interaction between the slurry abrasive particles (with the size range of about 30–70 nm) and the polished surface. To study such interactions, we used AFM. Surface analysis of selective layer using the AFM revealed detailed surface characteristics obtained by CMP. Studying the selective layer CMP, of which the predominated one is copper (in proportion of over 85%), we found that the AFM scanning removes the surface oxide layer in different rates depending on the depth of removal and the pH of the solution. Oxide removal happens considerably faster than the copper CMP removal from the selective layer. This is in agreement with generally accepted models of copper CMP. It was found that removal mechanisms depend on the slurry chemistry, potential per cent of oxidizer, and the applied load. This presentation discusses these findings. Both load force and the friction forces acting between the AFM tip and surface during the polishing process were measured. One big advantage of using the AFM tip (of radius about 50 nm) as abrasive silica particle is that we can measure forces acting between the particle-tip and the surface being polished. Here, we report measurement of the friction force while scratching and polishing. The correlation between those forces and removal rate is discussed.     

Strong water repellency effect on SiO<Subscript>2</Subscript> films processed at a nanometric scale

The present study deals with the creation of nano-rough surfaces with stable and controlled high hydrophobicity. These surfaces were obtained by combining the ion track etching technique with a simple functionalization by grafting perfluoroctyltrichlorosilane (PFOTS) molecules. Surface morphology was investigated by AFM observations which evidenced a self-affine fractal structure with a fractal dimension D_f ~ 2.6. The study of the wetting properties of these surfaces allowed to elucidate the conditions for observing a high hydrophobicity phenomenon and to predict the contact angle values for surfaces designed at a nanometric scale.     

Multi-modal analysis on the intermittent contact dynamics of atomic force microscope

A multi-modal analysis on the intermittent contact between an atomic force microscope (AFM) with a soft sample is presented. The intermittent contact induces the participation of the higher modes into the motion and various subharmonic motions are shown. The AFM tip mass enhances the coupling of different modes. The AFM tip mass is modeled by the Dirac delta function and the coupling effects are analyzed via the Galerkin method. The necessity of applying multi-modal analysis to the intermittent contact problem is demonstrated. Unlike the impact oscillator model which assumes the impact/contact time is infinitesimal, the contact time can be a significant fractional portion in each cycle, especially for the soft sample case and thus results in different dynamic behavior from that of an impact oscillator.     

Adhesion studies of latex film surfaces on the meso- and nanoscale

In this paper the effects of surface roughness and annealing temperature (T) of latex coating films on adhesion are discussed for the different stages of the film formation process. The surface free energy of latex films was assessed in terms of practical work of adhesion (W) (or adherence) using a custom-built adhesion-testing device (ATD), atomic force microscopy (AFM), and contact angle measurements. For preannealed latex films surface roughness averages (R_a) were determined from AFM height images and were related to the values of W obtained from ATD measurements at room temperature. The results obtained using these tests exhibiting surface behavior on different length scales indicate a dependence of the measured adhesion on surface roughness and temperature, as well as on the length scale of the measurements.First preannealed samples were studied, which were obtained by heat treatment above the respective glass transition temperatures (T_g). Increasing the temperature of preannealing resulted in a decrease of the adherence observed in ATD experiments at room temperature. However, on the nanoscale, using AFM, no significant variation of the adherence was observed. This observation can be explained by roughness arguments. Preannealing decreases roughness which results in lower adherence values measured by ATD while for essentially single asperity AFM experiments roughness has an insignificant effect. Specimens were also annealed over a constant period of time (90 min) at different temperatures. At the end of the heat treatment, adhesion was measured at the treatment temperature by ATD. The amplified effect of temperature observed in this case on adherence is attributed to the combination of roughness decrease and increasing test temperature. In a third set of experiments completely annealed samples were studied by ATD as well as by AFM as a function of temperature. With increasing T values ATD showed a decrease in adherence, which is attributed to a decreasing surface free energy of the annealed films at elevated T values. AFM, on the other hand, showed an opposite trend which is assigned to increasing penetration of the tip into the tip/wetting polymer samples versus increasing temperature. Finally, annealing isotherms as a function of time were investigated by ATD in situ at different temperatures. This last set of experiments allowed us to optimize annealing time and temperature to achieve complete curing.     

Thermally activated depinning of a narrow domain wall from a single defect

We describe the field induced depinning process of a magnetic domain wall (DW) from a single bidimensional nanometric defect. The DW propagates in a wire lithographed on a film with strong perpendicular anisotropy. We observe a statistical distribution of the relaxation time consistent with a Néel-Brown picture of magnetization reversal. This indicates that the nanometric DW can be considered as an ideal monodomain particle switching over a single energy barrier. Such a stochastic character of DW depinning has to be taken into account for spintronic applications.