An AFM study of the processing of hydrogen passivated silicon(1 1 1) of a low miscut angle

We present atomic force microscopy (AFM) measurements from a passivated silicon crystal miscut by 0.1° and show the etching regime to be significantly different from surfaces with a larger miscut angle. A simple kinetic model is developed to explain the results and is used to derive the optimal etching conditions for nominally flat Si(1 1 1)–(1×1)H. We show that small changes in miscut angle can alter the kinetic steady state and promote the formation of deep etch pits, even on the least stable, miscut surface. Collisions of steps with these pits result in arrays of stable, self-aligned ‘etch hillocks' over micron dimensions. Following preparation, we use AFM to observe the initial growth of native oxide on the Si(1 1 1)–(1×1)H surface, and demonstrate that AFM is a sensitive probe to surface oxidation in the sub-monolayer regime.     

How narrow can a meniscus be?

A water meniscus naturally forms in air between an atomic force microscope (AFM) tip and a substrate. This nanoscale meniscus produces a capillary force on the AFM, and also serves as a molecular transport channel in dip-pen nanolithography (DPN). A stable meniscus is a necessary condition for DPN and for the validity of the Kelvin equation commonly applied to AFM experiments. Lattice gas Monte Carlo simulations show that, due to thermal fluctuation, a stable meniscus has a lower limit in width. We find a minimum width of 5 molecular diameters (1.9 nm) when the tip becomes atomically sharp (terminated by a single atom).     

Observation of antiphase domains in Cd<Subscript>x</Subscript>Hg<Subscript>1−<Emphasis Type="Italic">x</Emphasis></Subscript>Te films on silicon by the phase contrast method in atomic force microscopy

It has been shown that phase contrast in atomic force microscopy (AFM) can be used to obtain adequate information on the density and distribution of antiphase domains on the surface of CdHgTe films grown by molecular beam epitaxy on a Si(301) substrate. By comparing the AFM phase images of the film surface with TEM images of structural defects in the near-surface region, the relation between microstructure and micromorphology of the films is revealed.     

A dislocation mechanism of friction between a nanoprobe and solid surface

A dislocation mechanism of friction between an atomic-force microscope (AFM) probe and an atomically smooth solid surface is put forward. In this mechanism, the contact region is represented by an edge dislocation. The triboacoustic emission measured with an AFM shows the dislocation nature of friction. The friction force is calculated for a parabolic tip.     

Modeling of surfaces of constant force above a lattice of close-packed atoms in the repulsive mode

Surfaces of constant force (force contours) are calculated for the scanning of an AFM tip over a lattice of close-packed atoms in the repulsive mode. It is shown that discontinuities are observed on the force contours in the regions between the atoms of the surface lattice for sufficiently small initial scanning heights of a tip with a single atom at its end. A cluster model of the tip end, which ensures continuity of the scanning at arbitrary initial heights, is constructed. The dependence of the AFM images on the orientation of the cluster on the tip end relative to the crystallographic axes of the surface is investigated for both an unperturbed lattice of close-packed atoms and a lattice containing point defects. The diagnostic possibilities of the findings are discussed. Zh. Tekh. Fiz. 67, 77–85 (June 1997)     

Shear modulation force microscopy study of near surface glass transition temperatures

We report results of glass transition (T(g)) measurements for polymer thin films using atomic force microscopy (AFM). The AFM mode, shear modulation force microscopy (SMFM), involves measuring the temperature-dependent shear force on a tip modulated parallel to the sample surface. Using this method we have measured the surface T(g) of thin (17-500 nm) polymer films and found that T(g) is independent of film thickness (t>17 nm), strength of substrate interactions, or even presence of substrate.     

A Thin Liquid Film and Its Effects in an Atomic Force Microscopy Measurement

Recently, it has been observed that a liquid film spreading on a sample surface will significantly distort atomic force microscopy （AFM） measurements. In order to elaborate on the effect, we establish an equation governing the deformation of liquid film under its interaction with the AFM tip and substrate. A key issue is the critical liquid bump height yoc, at which the liquid film jumps to contact the AFM tip. It is found that there are three distinct regimes in the variation of yoc with film thickness H, depending on Hamaker constants of tip, sample and liquid. Noticeably, there is a characteristic thickness H^＊ physically defining what a thin film is; namely, once the film thickness H is the same order as H^＊, the effect of film thickness should be taken into account. The value of H^＊ is dependent on Hamaker constants and liquid surface tension as well as tip radius.     

Sensor studies of the initial stages of the cadmium telluride film formation through vapor deposition

The results of sensor and electron-microscopic studies of the initial stages of cadmium telluride film formation through vapor deposition on a substrate at room temperature and on a substrate cooled by liquid nitrogen (highly nonequilibrium conditions) are reported. A piezoelectric quartz resonator is used as a sensor. The kinetic curves of the sensor analytical signal and photomicrographs are presented. A jumplike character of the nucleation process and a quasi-periodical growth mechanism for island films are disclosed. A sequence of new-phase island ensembles is formed in an analogous way. These islands increase the substrate surface coverage in a quasi-discrete manner. The experimental results are shown to agree with current theory of the first-order phase transitions and models of layer formation in highly nonequilibrium conditions.     

The phase behaviour of single polyethylene chains with and without fixing one end

The phase behaviour of a single polyethylene chain is studied by using molecular dynamics simulations. A free chain and a chain with fixing one end are considered here, since the atomic force microscope （AFM） tip can play a significant role in polymer crystallization in experiment. For a free chain, it is confirmed in our calculation that the polymer chain exhibits an extended coil state at high temperatures, collapses into a condensed state at low temperatures, i.e. the coil-to-globule transition that is determined by a high temperature shoulder of the heat capacity curve, and an additional liquid-to-solid transition that is described by a low temperature peak of the same heat curve. These results accord with previous studies of square-well chains and Lennard-Jones homopolymers. However, when one of the end monomers of the same chain is fixed the results become very different, and the chain cannot reach an extended coil-like state as a free chain does at high temperatures, i.e. there exists no coil-to-globule-like transition. These results may provide some insights into the influence of AFM tip when it is used to study the phase behaviour of polymer chains. If the interaction force between AFM tip and polymer monomers is strong, some monomers or one of them can be seen as being fixed by the tip, which is similar to our simulation model, and it is also found that AFM tip could induce polymer crystallization.     

Distance dependence of noncontact-AFM image contrast on Si(111) × –Ag structure

Atomic resolution imaging of the Si(111) × R30°–Ag surface was investigated using a noncontact atomic force microscopy (NC-AFM) in ultrahigh vacuum. NC-AFM images showed three types of contrasts depending on the distance between an AFM tip and a sample surface. When the tip–sample distance was about 1–3 Å, the images showed the honeycomb arrangement with weak contrast. When the tip–sample distance was about 0–0.5 Å, the images showed the periodic structure composed of three bright spots with relatively strong contrast. On the other hand, the contrasts of images measured at the distance of 0.5–1 Å seemed to be composed of the above-mentioned two types of contrasts. By comparing the site of bright spots in the AFM images with honeycomb-chained trimer (HCT) model, we suggested the following models: when the tip is far from the sample surface, tip–sample interaction force contributing to imaging is dominated by physical bonding interaction such as Coulomb force and/or van der Waals (vdW) force between the tip apex Si atoms and Ag trimer on the sample surface. On the other hand, just before the contact, tip–sample interaction force contributing to imaging is dominated by chemical bonding such as the force due to hybridization between the dangling bond out of the tip apex Si atom and the orbit of Si–Ag covalent bond on the sample surface.     

Modification of AFM Tips for Facilitating Picking-up of Nanoparticles

The radius of atomic force microscope (AFM) tip is a key factor that influences nonspecific interactions between AFM tip and nanoparticles. Generally, a tip with larger radius contributes to a higher efficiency of picking up nanoparticles. We provide two methods for modifying the AFM tip: one is to wear a tip apex on a solid substrate and the other is to coat a tip with poly (dimethylsiloxane) (PDMS). Both the approaches can enhance the adhesion force between the tip and nanoparticles by increasing tip radius. The experimental results show that a modified tip, compared to an unmodified one, achieves six-fold efficiency improvement in the capture of targeted colloidal gold nanoparticles.     

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.     

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.     

Assessing the structure and function of single biomolecules with scanning transmission electron and atomic force microscopes

The scanning transmission electron microscope (STEM) and the atomic force microscope (AFM) have provided a wealth of useful information on a wide variety of biological structures. These instruments have in common that they raster-scan a probe over a sample and are able to address single molecules. In the STEM the probe is a focused electron beam that is deflected by the scan-coils. Detectors collecting the scattered electrons provide quantitative information for each sub-nanometer sized sample volume irradiated. These electron scattering data can be reconstituted to images of single macromolecules or can be integrated to provide the mass of the macromolecules. Samples need to be dehydrated for such quantitative STEM imaging. In contrast, the AFM raster-scans a sharp tip over a sample surface submerged in a buffer solution to acquire information on the sample's surface topography at sub-nanometer resolution. Direct observation of function-related structural changes induced by variation of temperature, pH, ionic strength, and applied force provides insight into the structure-function relationship of macromolecules. Further, the AFM allows single molecules to be addressed and quantitatively unfolded using the tip as nano-tweezers. The performance of these two scanning probe approaches is illustrated by several examples including the chaperonin GroEL, bacterial surface layers, protein crystals, and bacterial appendices.     

Thin film semiconductor islands and numerical experiment

The distribution functions of island nuclei of germanium melt drops on Si(100) substrate over lateral sizes and heights in the presence of a surface linear defect are obtained in a numerical experiment simulating the initial stage of the first-order phase transition. A similar model of heterogeneous condensation of silicon carbide vapor is discussed. Quasi-linear kinetic partial differential equations are solved by the efficient numerical method of stochastic analogue of nonequilibrium processes. The Volmer-Weber mechanism of cluster formation from melt islands, their crystallization, and island structure formation on the substrate are considered.     

原子力显微镜在轻敲模式下的动力学模型

基于Hamaker假设、Lennard-Jones势能定律及经典弹性理论建立了一种新型的球体与平面黏着接触的弹性模型，该模型显示黏着力在原子力显微镜(AFM)针尖趋近和撤离样品表面，即加载和卸载的两个过程中存在黏着滞后现象，表明了AFM在轻敲工作模式中存在能量耗散.同时，根据所建的黏着接触弹性模型，建立了AFM在轻敲工作模式下的动力学模型，研究了AFM在轻敲工作模式下的振动幅度、相位差及耗散功率随针尖与样品表面间距的变化规律，仿真结果与现有的实验结果相一致.     

Effect of substrate temperature on the morphological,structural,and optical properties of RF sputtered Ge_(1-x)Sn_x films on Si substrate

In this study, Ge_(1-x)Sn_x alloy films are co-sputtered on Si(100) substrates using RF magnetron sputtering at different substrate temperatures. Scanning electron micrographs, atomic force microscopy(AFM), Raman spectroscopy, and x-ray photoemission spectroscopy(XPS) are conducted to investigate the effect of substrate temperature on the structural and optical properties of grown Ge Sn alloy films. AFM results show that RMS surface roughness of the films increases from 1.02 to 2.30 nm when raising the substrate temperature. This increase could be due to Sn surface segregation that occurs when raising the substrate temperature. Raman spectra exhibits the lowest FWHM value and highest phonon intensity for a film sputtered at 140?C. The spectra show that decreasing the deposition temperature to 140?C improves the crystalline quality of the alloy films and increases nanocrystalline phase formation. The results of Raman spectra and XPS confirm Ge–Sn bond formation. The optoelectronic characteristics of fabricated metal-semiconductor-metal photodetectors on sputtered samples at room temperature(RT) and 140?C are studied in the dark and under illumination. The sample sputtered at 140?C performs better than the RT sputtered sample.     

Scratch direction and threshold force in nanoscale scratching using atomic force microscopes

The nanoscaled tip in an AFM (atomic force microscope) has become an effective scratching tool for material removing in nanofabrication. In this article, the characteristics of using a diamond-coated pyramidal tip to scratch Ni-Fe thin film surfaces was experimentally investigated with the focus on the evaluation of the influence of the scratch or scan direction on the final shape of the scratched geometry as well as the applied scratch force. Results indicated that both the scratched profile and the scratch force were greatly affected by the scratch direction. It has been found that, to minimize the formation of protuberances along the groove sides and to have a better control of the scratched geometry, the tip face should be perpendicular to the scratching direction, which is also known as orthogonal cutting condition. To demonstrate the present findings, three groove patterns have been scratched with the tip face perpendicular to the scratching direction and very little amount of protuberances was observed. The threshold scratch force was also predicted based on the Hertz contact theory. Without considering the surface friction and adhesive forces between the tip and substrate, the threshold force predicted was twice smaller than the measurement value. Finally, recommendations for technical improvement and research focuses are provided.     

Synthesis of poly-<Emphasis Type="Italic">p</Emphasis>-xylylene + CdS nanocomposites and studing of their surface structure

Thin-film polymeric nanocomposites based on a poly-p-xylylene matrix (PPX) and nanoparticles of cadmium sulfide (CdS) have been obtained using solid-phase cryochemical synthesis on optical quartz substrates. The optimal conditions for the formation of PPX + CdS nanostructured polymeric films have been determined. The topography and surface characteristics of PPX + CdS nanocomposites have been studied by scanning atomic force microscopy (AFM). The characteristics of the morphological and structural changes of the film surfaces have been found at different CdS nanoparticle concentrations. These changes point to a reorganization of the PPX + CdS polymeric matrix. It is shown that at 2–10 vol % CdS concentration, the elements of the surface’s structural organization are polymeric nanofibers, parallel to the substrate plane, and a small number of nanoglobules, locally positioned directly on the nanofiber surfaces. Ordering of the surface structure accompanied by the formation of a periodic surface relief in the shape of nanoglobules was observed at a CdS concentration of 13.5 vol %. A mechanism of the formation of nanostructured PPX + CdS films is proposed. Based on the AFM experimental data, one can assume that during co-condensation of a p-xylylene monomer, CdS nanoparticles initiate radical polymerization of the PPX matrix, when the substrate is heated from 77 K to 300 K. The type of surface structure (fibrillar, fibrillar + globular and globular) depends on the nanoparticle concentration in the polymeric matrix.     

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.