Identifying individual single-walled and double-walled carbon nanotubes by atomic force microscopy

We show that the number of concentric graphene cylinders forming a carbon nanotube can be found by squeezing the tube between an atomic force microscope tip and a silicon substrate. The compressed height of a single-walled nanotube (double-walled nanotube) is approximately two (four) times the interlayer spacing of graphite. Measured compression forces are consistent with the predicted bending modulus of graphene and provide a mechanical signature for identifying individual single-walled and double-walled nanotubes.     

Effects of tip-nanotube interactions on atomic force microscopy imaging of carbon nanotubes

We examine the effect of van der Waals (vdW) interactions between atomic force microscope tips and individual carbon nanotubes (CNTs) supported on SiO₂. Molecular dynamics (MD) simulations reveal how CNTs deform during atomic force microscopy (AFM) measurement, irrespective of the AFM tip material. The apparent height of a single- (double-) walled CNT can be used to estimate its diameter up to ～2 nm (～3 nm), but for larger diameters the CNT cross-section is no longer circular. Our simulations were compared against CNT dimensions obtained from AFM measurements and resonant Raman spectroscopy, with good agreement for the smaller CNT diameters. In general, AFM measurements of large-diameter CNTs must be interpreted with care, but the reliability of the approach is improved if knowledge of the number of CNT walls is available, or if additional verification (e.g., by optical techniques) can be obtained.

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Studying the high-field electron conduction of tetrahedral amorphous carbon thin films by conducting atomic force microscopy

The high-field electron conduction of tetrahedral amorphous carbon (ta-C) thin films substrate has been studied using a conducting atomic force microscope (C-AFM). The ta-C thin films with a high concentration of sp³ bonding (80–90%) were deposited on Si by field arc deposition (FAD). The high-field “conductance” and surface morphology were mapped simultaneously. At low bias, the “conductance” exhibits inhomogeneities on a large scale, presumably due to thickness variations or interface defects. However, at high bias, the small difference in “conductance” due to thickness variations or interface defects was buried by the high intrinsic “conductivity.” It has also been shown that high field causes electric breakdown in these films by converting sp³ bonding to sp² at high electric field.     

Determination of nano-roughness of carbon fibers by atomic force microscopy

We present a novel approach to determine the surface roughness on varying scales using atomic force microscopy data. The key factor is to find a suitable background correction for the desired scale. Using the example of the surface of sized and unsized high-tenacity carbon fibers, we present an easy method to find backgrounds for widely varying scales and to evaluate respective topography and surface roughness with the same lateral resolution as the microscope itself. The analysis is done by subtracting a tunable background from the respective height data. By choosing an appropriate background to investigate the surface topography of a carbon fiber on a nm-scale, only small nano-structures with a width of around 20 nm remain after the background subtraction. Evaluating the mean roughness R _a of these nano-structures, sized carbon fibers show an overall value of around 0.1 nm while unsized carbon fibers a value of around 0.4 nm. Total background corrected height analysis shows an even distribution of these nano-structures along the fibrils of the unsized fibers, whereas for the sized fibers the nano-structures are not present. The presented method allows analysis and visualization of the distribution of nano-structures on a carbon fiber surface for the first time. This feature is used to visualize the distribution of the sizing and can further be used to investigate the influence of different production parameters on the fiber topography or to evaluate the contribution of mechanical interlocking to the interfacial strength.     

In situ atomic force microscopy tip-induced deformations and Raman spectroscopy characterization of single-wall carbon nanotubes

In this work, an atomic force microscope (AFM) is combined with a confocal Raman spectroscopy setup to follow in situ the evolution of the G-band feature of isolated single-wall carbon nanotubes (SWNTs) under transverse deformation. The SWNTs are pressed by a gold AFM tip against the substrate where they are sitting. From eight deformed SWNTs, five exhibit an overall decrease in the Raman signal intensity, while three exhibit vibrational changes related to the circumferential symmetry breaking. Our results reveal chirality dependent effects, which are averaged out in SWNT bundle measurements, including a previously elusive mode symmetry breaking that is here explored using molecular dynamics calculations.     

Probing electrical transport in individual carbon nanotubes and junctions

The electrical transport properties of individual carbon nanotubes (CNTs) and multi-terminal junctions of CNTs are investigated with a quadraprobe scanning tunneling microscope. The CNTs used in this study are made of stacked herringbone-type conical graphite sheets with a cone angle of ～20° to the tube axis, and the CNT junctions have no catalytic particles in the junction areas. The CNTs have a significantly higher resistivity than conventional CNTs with concentric walls. The straight CNTs display linear current-voltage (I-V) characteristics, indicating diffusive transport rather than ballistic transport. The structural deformation in CNTs with bends substantially increases the resistivity in comparison with that for the straight segments on the same CNTs, and the I-V curve departs slightly from linearity in curved segments. The junction area of the CNT junctions behaves like an ohmic-type scattering center with linear I-V characteristics. In addition, a gating effect has not been observed, in contrast to the case for conventional multi-walled CNT junctions. These unusual transport properties can be attributed to the enhanced inter-layer interaction in the herringbone-type CNTs.     

Studying the effect of alginate overproduction on Pseudomonas aeruginosa biofilm by atomic force microscopy

Pseudomonas aeruginosa is the most important pathogen in cystic fibrosis patients and forms biofilms in the lung. P. aeruginosa strains isolated from the lungs of the patients have a mucoid phenotype overproducing alginate. The phenotype forms highly structured biofilms which are more resistant to antibiotics than biofilms formed by its nonmucoid phenotype. Conversion to the alginate-overproducing phenotype occurs through a mutation in rpoN gene in the strains. The biofilms formed by the alginate-overproducing phenotype are highly sticky, but their stickiness has not been measured. Herein, the stickiness of biofilms formed by the rpoN mutant was measured by atomic force microscopy (AFM). Confocal laser scanning microscopy showed that the biofilms formed by the slowly-growing rpoN mutant were more structured than those formed by the wild-type strain. AFM analysis indicated that the biofilms formed by the rpoN mutant were stickier than those formed by the wild type strain during the attachment and establishment stages, but the difference in stickiness was greatly reduced during the maturation stage possibly due to the cytosolic contents released from dead cells in the biofilms formed by the wild type. These results suggest that the alginate overproduction greatly affects the physical properties (topography and stickiness) of P. aeruginosa biofilms as well as the physiological properties (cell death and growth) of the bacterial cells inside the biofilms.     

Studying multilayer langmuir film structure by confocal laser scanning and atomic force microscopy techniques

Features of extracting information on the surface structure of a multilayer organic film from data on its optical properties and surface relief are considered. The object of investigation was a multilayer Langmuir-Blodgett film based on a prepolymer (polyamic acid salt). It is suggested that the formation of the film volume is influenced by inhomogeneities in the structure of layers.     

Electron transport through supported biomembranes at the nanoscale by conductive atomic force microscopy

We present a reliable methodology to perform electron transport measurements at the nanoscale on supported biomembranes by conductive atomic force microscopy (C-AFM). It allows measurement of both (a) non-destructive conductive maps and (b) force controlled current-voltage characteristics in wide voltage bias range in a reproducible way. Tests experiments were performed on purple membrane monolayers, a two-dimensional (2D) crystal lattice of the transmembrane protein bacteriorhodopsin. Non-destructive conductive images show uniform conductivity of the membrane with isolated nanometric conduction defects. Current-voltage characteristics under different compression conditions show non-resonant tunneling electron transport properties, with two different conduction regimes as a function of the applied bias, in excellent agreement with theoretical predictions. This methodology opens the possibility for a detailed study of electron transport properties of supported biological membranes, and of soft materials in general.     

Electrical transport properties of oligothiophene-based molecular films studied by current sensing atomic force microscopy

Using conducting probe atomic force microscopy (CAFM) we have investigated the electrical conduction properties of monolayer films of a pentathiophene derivative on a SiO(2)/Si-p+ substrate. By a combination of current-voltage spectroscopy and current imaging we show that lateral charge transport takes place in the plane of the monolayer via hole injection into the highest occupied molecular orbitals of the pentathiophene unit. Our CAFM data suggest that the conductivity is anisotropic relative to the crystalline directions of the molecular lattice.     

General theories for the electrical transport properties of carbon nanotubes

We have shown that the general theories of metals and semiconductors can be employed to understand the diameter and voltage dependency of current through metallic and semiconducting carbon nanotubes, respectively. The current through a semiconducting multiwalled carbon nanotube (MWCNT) is associated with the energy gap that is different for different shells. The contribution of the outermost shell is larger as compared to the inner shells. The general theories can also explain the diameter dependency of maximum current through nanotubes. We have also compared the current carrying ability of a MWCNT and an array of the same diameter of single wall carbon nanotubes (SWCNTs) and found that MWCNTs are better suited and deserve further investigation for possible applications as interconnects.     

Local electronic structure of single-walled carbon nanotubes from electrostatic force microscopy

An atomic force microscope was used to locally perturb and detect the charge density in carbon nanotubes. Changing the tip voltage varied the Fermi level in the nanotube. The local charge density increased abruptly whenever the Fermi level was swept through a van Hove singularity in the density of states, thereby coupling the cantilever's mechanical oscillations to the nanotube's local electronic properties. By using our technique to measure the local band gap of an intratube quantum-well structure, created by a nonuniform uniaxial strain, we have estimated the nanotube chiral angle. Our technique does not require attached electrodes or a specialized substrate, yielding a unique high-resolution spectroscopic tool that facilitates the comparison between local electronic structure of nanomaterials and further transport, optical, or sensing experiments.     

Detecting mechanical resonance in carbon nanotubes via inter-tube electrical transport measurements

Detecting the mechanical resonance frequency of carbon nanotubes has strong potential applications that range from nano-scale balances to detect very small mass changes to ultra-sensitive bio-sensors. Detection of nanotube resonance requires elaborate and time-consuming techniques such as in-situ TEM, which limits the practical utility of this concept. In this paper we report a simple and accurate technique for detection of nanotube resonance by monitoring inter-tube electrical transport in a vibrating array of aligned multiwalled carbon nanotubes. The conductivity measurements are performed using a four-point probe in a direction perpendicular to the nanotube axis. We observe a dramatic decrease in the dc electrical resistance of the nanotube array at the mechanical resonance condition. We believe this is due to inter-tube impacts at resonance, which leads to an increase in the nanotube local temperature and hence increases the electron hopping rate. The impacting of the tubes could also enable localized tunneling of electrons through the nanotube array along with the hopping.     

Simultaneous electrical transport and scanning tunneling spectroscopy of carbon nanotubes

We performed scanning tunneling spectroscopy measurements on suspended single-walled carbon nanotubes with independently addressable source and drain electrodes in the Coulomb blockade regime. This three-terminal configuration allows the resistance to the source and drain electrodes to be individually measured, which we exploit to demonstrate that electrons were added to spin-degenerate states of the carbon nanotube. Unexpectedly, the Coulomb peaks also showed a strong spatial dependence. By performing simultaneous scanning tunneling spectroscopy and electrical transport measurements we show that the probed states are extended between the source and drain electrodes. This indicates that the observed spatial dependence reflects a modulation of the contact resistance.     

Chaos in dynamic atomic force microscopy

In tapping mode atomic force microscopy (AFM) the highly nonlinear tip-sample interaction gives rise to a complicated dynamics of the microcantilever. Apart from the well-known bistability under typical imaging conditions the system exhibits a complex dynamics at small average tip-sample distances, which are typical operation conditions for mechanical dynamic nanomanipulation. In order to investigate the dynamics at small average tip sample gaps experimental time series data are analysed employing nonlinear analysis tools and spectral analysis. The correlation dimension is computed together with a bifurcation diagram. By using statistical correlation measures such as the Kullback-Leibler distance, cross-correlation and mutual information the dataset can be segmented into different regimes. The analysis reveals period-3, period-2 and period-4 behaviour, as well as a weakly chaotic regime.     

Nanofabrication with atomic force microscopy

Atomic force microscopy (AFM) was developed in 1986. It is an important and versatile surface technique, and is used in many research fields. In this review, we have summarized the methods and applications of AFM, with emphasis on nanofabrication. AFM is capable of visualizing surface properties at high spatial resolution and determining biomolecular interaction as well as fabricating nanostructures. Recently, AFM-based nanotechnologies such as nanomanipulation, force lithography, nanografting, nanooxidation and dip-pen nanolithography were developed rapidly. AFM tip (typical radius ranged from several nanometers to tens of nanometers) is used to modify the sample surface, either physically or chemically, at nanometer scale. Nanopatterns composed of semiconductors, metal, biomolecules, polymers, etc., were constructed with various AFM-based nanotechnologies, thus making AFM a promising technique for nanofabrication. AFM-based nanotechnologies have potential applications in nanoelectronics, bioanalysis, biosensors, actuators and high-density data storage devices.     

Specific aptamer-protein interaction studied by atomic force microscopy

Aptamers are a new class of synthetic DNA/RNA oligonucleotides generated from in vitro selection to selectively bind with various molecules. Due to their molecular recognition capability for proteins, aptamers are becoming promising reagents in protein detection and new drug development. In this study, the specific interaction between the protein immunoglobulin E (IgE) and its 37-nt aptamer has been measured directly by atomic force microscopy. The single-molecule unbinding force between IgE and the aptamer is determined using the Poisson statistical method. The individual unbinding force between IgE and its monoclonal antibody has also been obtained and compared to that between IgE and the aptamer. The results reveal the high affinity of the aptamer to protein, which could match or even surpass that of the antibody to its antigen.     

Dielectric constants by multifrequency non-contact atomic force microscopy

We present a method to obtain capacitive forces and dielectric constants of ultra-thin films on metallic substrates using multifrequency non-contact atomic force microscopy with amplitude feedback in air. Capacitive forces are measured via cantilever oscillations induced at the second bending mode and dielectric constants are calculated by fitting an analytic expression for the capacitance (Casuso et al 2007 Appl. Phys. Lett. 91 063111) to the experimental data. Dielectric constants for self-assembled monolayers of thiol molecules on gold (2.0±0.1) and sputtered SiO2 (3.6±0.07) were obtained under dry conditions, in good agreement with previous measurements. The high Q-factor of the second bending mode of the cantilever increases the accuracy of the capacitive measurements while the low applied potentials minimize the likelihood of variation of the dielectric constants at high field strength and of damage from dielectric breakdown of air.     

Precise control of nanofabrication by atomic force microscopy

With an aim of the precise control of the anodic oxidation process by atomic force microscopy, the technical improvement has been carried out based on the mechanism studies. The accuracy and reliability of the nanofabrication have been improved by the combination of ambient humidity control, improvement of instrumental performance and meniscus lifetime control. In parallel, the mechanism study has been proceeded through the detection of Faradaic current. The in situ Faradaic current detection of the nano-oxidation process can actually work as a sensitive monitor for the nano-oxidation process with a high reliability. From an engineering viewpoint with an eye to practical applications, controllable physical parameters which affect on the product size are enumerated to consider what we should do to raise the precision of nano-oxidation. Then the fast fabrication in a large area by a patchwork method, Faradaic current detection during oxidation-reduction reaction, and nanofabrication by current-control are shown as examples.