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.     

Studying electrical transport in carbon nanotubes by conductance atomic force microscopy

An introduction to conductance atomic force microscopy in the context of carbon nanotubes is provided where the main problems and performances of this technique are discussed. The conductance measured in SWNT as a function of the loading force applied by an AFM metallized tip is reported. These experiments allow us to study the process of the electrical contact formation between the tip and the nanotube. This will also lead to a study of the electromechanical properties of nanotubes for radial deformations.     

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.

Open image in new window

     

Measurement of elastic properties of calcium silicate hydrate with atomic force microscopy

Atomic force microscopy (AFM) based indentation is compared to conventional nanoindentation for measuring mechanical properties of cement pastes. In evaluating AFM as a mechanical characterization tool, various analytical and numerical modeling approaches are compared. The disparities between the numerical self-consistent approach and analytical solutions are determined and reported. The measured elastic Young’s modulus determined from AFM indentation tests are compared to elastic Young’s modulus determined from nanoindentation tests of cement paste. These results indicate that the calcium silicate hydrate (C-S-H) phase of hydrated Portland cement has different properties on the different length scales probed by AFM versus nanoindenters. Packing density of C-S-H particles is proposed as an explanation for the disparity in the measured results.     

Relating elastic modulus to indentation response using atomic force microscopy

Abstracts are not published in this journal     

Electrical characterization of silicon tips using conducting atomic force microscopy

The electrical properties of n-doped Si tips have been characterized in conducting atomic force microscopy under various conditions. Si tips with SiO2 layer on them present complex electric properties: which include a larger positive threshold bias, which is different from that of its doped semiconductor material. Silicon tips after removing their SiO2 layer had smaller positive threshold bias; such bias varied with the loading force: smaller loading forces corresponding to larger positive threshold biases, and it remained constant at lower levels for larger loading forces. Humidity of experiments influenced the threshold bias: lower relative humidities (<25%) and larger loading forces were in favor of getting stable threshold bias. The conductance increased remarkably in high relative humidity although it was kept in a narrow range when relative humidity was lower than 40%. Loading force didn't affect the conductance in the examined relative humidity conditions. One advantage of bare silicon tips over commercial conducting ones is that they smaller radius than gold-coated tips; this is in more favor of reaching single molecular electronics.     

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.     

Mapping the elastic properties of granular Au films by contact resonance atomic force microscopy

Endowed with nanoscale spatial resolution, contact resonance atomic force microscopy (CR-AFM) provides extremely localized elastic property measurements. We advance here the applicability of CR-AFM on surfaces with nanosize features by considering the topography contribution to the CR-AFM signal. On nanosize granular Au films, the elastic modulus at the grain scale has been mapped out by considering a self-consistent deconvolution of the contact geometry effect in the CR-AFM image. Significant variation in the contact area over granular topography arises as the probe is either in single-?or multiple-asperity contact with the surface. Consequently, in extracting the elastic modulus from CR-AFM measurements on granular surfaces we considered both the normal and lateral couplings established through multiple-asperity contacts between the tip and the surface. Thus, by appropriately considering the change in the contact mechanics during CR-AFM imaging, variations in the elastic modulus have been revealed in the intergrain regions as well as across individual grains.     

Controllable nanoreactor confined to atomic force microscopy tips and its application in low copy DNA ligation

Less molecules reaction, especially at the single molecule level, plays an important role in biochemical or chemical research. It is also significant to achieve low copy or single molecule DNA ligation during the whole genome project. In this paper, a new type of nanoreactor was constructed around atomic force microscopy (AFM) tips under certain humidity, where DNA molecules can be limited to a special space through water meniscus, so the probability of molecules collision was increased and the efficiency of DNA ligation was greatly enhanced. Combined with the nanomanipulation based on AFM, controllable nanoreactor may provide a new tool to single molecule reaction. Low copy DNA ligation was successfully achieved by this method. Results showed the number of DNA molecules involved in the nanoreactor can not be more than sixty. This method will found a base for the ultimate realization of single-molecule DNA ligation.     

Investigation of sisal fibers by atomic force microscopy: morphological and adhesive characteristics

Atomic force microscopy (AFM) was used to study the nanoscale surface chemistry and morphological changes caused by chemical treatment of sisal fibers. Scanning Electron Microscopy (SEM) micrographs indicated that sisal in natura (bundle of fibers) is formed by fibers with diameters of approximately 10 microm. AFM images showed that these fibers consist of microfibrils with diameters varying from 250 to 600 nm, which are made up of nanofibrils of ca. 20 nm in diameter. The adhesion force (pull-off force) between the AFM tip and the fibers surface increased after benzylation, pointing to a decrease in the polar groups on the sisal fiber. The adhesion map measured over a scan range of 3 microm was heterogeneous in samples treated with 40% NaOH and the low adhesion sites disappeared after benzylation. Using an established mathematical model, it was possible to evaluate the increase in adhesion work and consequently in the interaction between the AFM tip and sisal fibers. These results indicated that AFM can detect heterogeneity in the wettability of sisal fibers with nanometer resolution and can be applied in the study of fiber-matrix adhesion in polymer composites.     

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.     

Variability of the elastic properties of multiwalled carbon nanotubes

The results of numerous experimental investigations of carbon nanotubes show evidence of a considerable variability in their mechanical properties. Based on the common features of the structures of graphite and multiwalled carbon nanotubes (MWNTs), it is demonstrated that structural polytype transitions are among the probable factors responsible for this variability. Analysis of the MWNT behavior under torsion shows that the torsional stiffness of MWNTs depends on the elastic moduli, the number and magnitudes of which vary with the local symmetry of the MWNT structure (on the transition from rhombohedral to hexagonal and turbostratic modifications). The effect of structural transformations on the Young modulus in stretched MWNTs is evaluated.     

Characterising the surface adhesive behavior of tablet tooling components by atomic force microscopy

Purpose: The aim of this study is to develop an atomic force microscopy (AFM) based approach to study the adhesive forces between tabletting punches and model formulation ingredients, that can ultimately be used to understand and predict issues such as sticking during tabletting compression.

Methods: Adhesive interactions were studied between single lactose particles and coated tablet punches. The adhesion was measured at varying relative humidities (RHs) and the influence of surface roughness was investigated. Roughness parameters were measured with AFM imaging and a modeling approach used to predict the influence of roughness on adhesion.

Results: Surface roughness was found to play a significant role in the observed lactose-punch adhesion and the variation of this adhesion across the punch surface. Such differences between punches can be correlated to observations from industrial use. Adhesion forces were spatially mapped to indentify “hot spots” of high adhesion. A modeling approach can predict the relative adhesion of different surfaces from roughness data. The adhesion was also significantly affected by RH, for one type of punch causing a greater than 3× increase in adhesion between 30 and 60% RH. Interestingly, different punches showed different RH-adhesion behavior, relating to their hydrophilicity.

Conclusions: The work introduces a new method for screening tablet punch materials and tabletting conditions. Important factors to be considered when evaluating adhesive interactions in tablet compression have been highlighted. Correlations are observed between AFM adhesion results and tabletting behavior during manufacture. This provides a promising basis for a predictive approach toward combating tabletting issues.     

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.     

The determination of the elastic modulus of microcantilever beams using atomic force microscopy

An investigation into the determination of the micromechanical properties of thin film materials has been performed. Thin metal and ceramic films are used extensively in the computer microprocessor industry and in the field of micro-electromechanical systems (MEMS). The demand for miniaturization and increased performance has resulted in the use of materials without a clear understanding of their mechanical properties on this scale. Micromechanical properties are difficult to obtain due to the lack of adequate testing equipment. The atomic force microscope (AFM), most commonly used as an imaging tool, lends itself to mechanical interaction with the sample surface utilizing a cantilever probe. An array of aluminum microcantilever beams were fabricated using standard IC processing techniques. The microbeams were deflected by the AFM cantilever probe and from this, the micromechanical properties of stiffness and elastic modulus were determined. Initial results indicate that this technique reliably determines the micromechanical properties of thin films.     

Electrostatic force microscopy evaluation of the conductivity of individual multiwalled carbon nanotubes

The electric conductivity of individual multiwalled carbon nanotubes (CNTs) doped with nitrogen has been studied in as-synthesized, heat-treated, and argon-ion-irradiated states by the method of electrostatic force microscopy (EFM). Modelling of transverse cross-section profiles of EFM images were used to determine the potential difference across the probe tip–CNT gap (U _tip-CNT), which is a parameter related to the conductivity of CNTs. A strong correlation between the specific volume conductivity of a CNT layer and average U _tip-CNT value has been found for all types of samples. It is established that a change in the conductivity of N-doped CNTs upon thermal annealing and argon-ion irradiation is caused by modification of the composition and/or concentration of defects in CNT walls.     

Mapping nanomechanical properties of live cells using multi-harmonic atomic force microscopy

The nanomechanical properties of living cells, such as their surface elastic response and adhesion, have important roles in cellular processes such as morphogenesis, mechano-transduction, focal adhesion, motility, metastasis and drug delivery. Techniques based on quasi-static atomic force microscopy techniques can map these properties, but they lack the spatial and temporal resolution that is needed to observe many of the relevant details. Here, we present a dynamic atomic force microscopy method to map quantitatively the nanomechanical properties of live cells with a throughput (measured in pixels/minute) that is ～10-1,000 times higher than that achieved with quasi-static atomic force microscopy techniques. The local properties of a cell are derived from the 0th, 1st and 2nd harmonic components of the Fourier spectrum of the AFM cantilevers interacting with the cell surface. Local stiffness, stiffness gradient and the viscoelastic dissipation of live Escherichia coli bacteria, rat fibroblasts and human red blood cells were all mapped in buffer solutions. Our method is compatible with commercial atomic force microscopes and could be used to analyse mechanical changes in tumours, cells and biofilm formation with sub-10?nm detail.     

原子力显微镜探针悬臂弹性常数校正技术进展

利用原子力显微镜对材料表面的力学性能进行定量表征时,需要准确知道原子力显微镜探针悬臂的弹性常数,所以对弹性常数进行校正十分重要。该文综述近年来对探针悬臂弹性常数的校正方法,主要包括维度法、静态挠度法、动态挠度法。维度法对不同悬臂形状(主要针对矩形、V型)进行阐述,分析不同方法使用的数学模型与优缺点;静态挠度法不仅对方法的数学模型进行阐述,还着重介绍近年来对该方法精确度的改进研究;动态挠度法以附加质量法、Sader法与热调谐法分别阐述,比较3种方法的模型特点与先进性;最后分析常用探针适合使用的校正方法,对今后校正方法的发展提供参考。