Charge trapping in carbon nanotube loops demonstrated by electrostatic force microscopy

Electronic devices made from carbon nanotubes (CNTs) can be greatly affected by substrate charges, which, for instance, induce strong hysteresis in CNT field effect transistors. In this work, electrostatic force microscopy (EFM) is employed to investigate single-walled nanotubes grown by chemical vapor deposition on SiO2 substrates. We demonstrate the use of this technique to gain quantitative information on the substrate charges. It is found that charge pools with densities around 10(-8) C/cm2 can be trapped inside nanotube loops for extended periods of time, showing that nanotubes can act as confining barriers for substrate charges. The trapped charges can be removed by scanning probe manipulation.     

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.     

Atomic-resolution imaging in liquid by frequency modulation atomic force microscopy using small cantilevers with megahertz-order resonance frequencies

In this study, we have investigated the performance of liquid-environment FM-AFM with various cantilevers having different dimensions from theoretical and experimental aspects. The results show that reduction of the cantilever dimensions provides improvement in the minimum detectable force as long as the tip height is sufficiently long compared with the width of the cantilever. However, we also found two important issues to be overcome to achieve this theoretically expected performance. The stable photothermal excitation of a small cantilever requires much higher pointing stability of the exciting laser beam than that for a long cantilever. We present a way to satisfy this stringent requirement using a temperature controlled laser diode module and a polarization-maintaining optical fiber. Another issue is associated with the tip. While a small carbon tip formed by electron beam deposition (EBD) is desirable for small cantilevers, we found that an EBD tip is not suitable for atomic-scale applications due to the weak tip-sample interaction. Here we show that the tip-sample interaction can be greatly enhanced by coating the tip with Si. With these improvements, we demonstrate atomic-resolution imaging of mica in liquid using a small cantilever with a megahertz-order resonance frequency. In addition, we experimentally demonstrate the improvement in the minimum detectable force obtained by the small cantilever in measurements of oscillatory hydration forces.     

Carbon nanotube air-bubble interactions studied by atomic force microscopy

Interaction forces between a multi-walled carbon nanotube (MWCNT) and an air-bubble in pure deionized water and methyl isobutyl carbinol (MIBC) solutions were measured by atomic force microscopy (AFM). The MWCNT terminated probe was brought into contact with the bubble at controlled applied forces. The repulsive steps followed by attractive jumps recorded in the approach force curves correspond to changes in the MWCNT diameter along its length, an observation confirmed by transmission electron microscopy (TEM) data. By processing the retraction part of the force curves obtained in pure water it is possible to estimate the end diameter of the carbon nanotube with nanometer resolution using a capillary force model.     

Three-dimensional electrostatic effects of carbon nanotube transistors

We explore the three-dimensional (3-D) electrostatics of planar-gate carbon nanotube field-effect transistors (CNTFETs) using a self-consistent solution to the Poisson equation with equilibrium carrier statistics. We examine the effects of the gate insulator thickness and dielectric constant and the source/drain contact geometry on the electrostatics of bottom-gated (BG) and top-gated (TG) devices. We find that the electrostatic scaling length is mostly determined by the gate oxide thickness, not by the oxide dielectric constant. We also find that a high-k gate insulator does not necessarily improve short-channel immunity because it increases the coupling of both the gate and the source/drain contact to the channel. It also increases the parasitic coupling of the source/drain to the gate. Although both the width and the height of the source and drain contacts are important, we find that for the BG device, reducing the width of the 3-D contacts is more effective for improving short channel immunity than reducing the height. The TG device, however, is sensitive to both the width and height of the contact. We find that one-dimensional source and drain contacts promise the best short channel immunity. We also show that an optimized TG device with a thin gate oxide can provide near ideal subthreshold behavior. The results of this paper should provide useful guidance for designing high-performance CNTFETs.     

Characterization of materials' nanomechanical properties by force modulation and phase imaging atomic force microscopy with soft cantilevers

Soft cantilevers, although having good force sensitivity, have found limited use for investigating materials' nanomechanical properties by conventional force modulation (FM) and intermittent contact (IC) atomic force microscopy. This is due to the low forces and small indentations that these cantilevers are able to exert on the surface, and to the high amplitudes required to overcome adhesion to the surface. In this paper, it is shown that imaging of local elastic properties of surface and subsurface layers can be carried out by employing electrostatic forcing of the cantilever. In addition, by mechanically exciting the higher vibration modes in contact with the surface and monitoring the phase of vibrations, the contrast due to local surface elasticity is obtained.     

Mapping of local electrical properties in epitaxial graphene using electrostatic force microscopy

Local electrical characterization of epitaxial graphene grown on 4H-SiC(0001) using electrostatic force microscopy (EFM) in ambient conditions and at elevated temperatures is presented. EFM provides a straightforward identification of graphene with different numbers of layers on the substrate where topographical determination is hindered by adsorbates. Novel EFM spectroscopy has been developed measuring the EFM phase as a function of the electrical DC bias, establishing a rigorous way to distinguish graphene domains and facilitating optimization of EFM imaging.     

Accuracy of the spring constant of atomic force microscopy cantilevers by finite element method

Atomic force microscopy (AFM) probe with different functions can be used to measure the bonding force between atoms or molecules. In order to have accurate results, AFM cantilevers must be calibrated precisely before use. The AFM cantilever's spring constant is usually provided by the manufacturer, and it is calculated from simple equations or some other calibration methods. The spring constant may have some uncertainty, which may cause large errors in force measurement. In this paper, finite element analysis was used to obtain the deformation behavior of the AFM cantilever and to calculate its spring constant. The influence of prestress, ignored by other methods, is discussed in this paper. The variations of Young's modulus, Poisson's ratio, cantilever geometries, tilt angle, and the influence of image tip mass were evaluated to find their effects on the cantilever's characteristics. The results were compared with those obtained from other methods.     

Controlled electrostatic gating of carbon nanotube FET devices

Carbon nanotube transistors are a promising platform for the next generation of nonoptical biosensors. However, the exact nature of the biomolecule interactions with nanotubes in these devices remains unknown, creating one of the major obstacles to their practical use. We assembled alternating layers of oppositely charged polyelectrolytes on the carbon nanotube transistors to mimic gating of these devices by charged molecules. The devices showed reproducible oscillations of the transistor threshold voltage depending on the polarity of the outer polymer layer in the multilayer film. This behavior shows excellent agreement with the predictions of a simple electrostatic model. Finally, we demonstrate that complex interactions of adsorbed species with the device substrate and the surrounding electrolyte can produce significant and sometimes unexpected effects on the device characteristics.     

Polarizability of G4-DNA observed by electrostatic force microscopy measurements

G4-DNA, a quadruple helical motif of stacked guanine tetrads, is stiffer and more resistant to surface forces than double-stranded DNA (dsDNA), yet it enables self-assembly. Therefore, it is more likely to enable charge transport upon deposition on hard supports. We report clear evidence of polarizability of long G4-DNA molecules measured by electrostatic force microscopy, while coadsorbed dsDNA molecules on mica are electrically silent. This is another sign that G4-DNA is potentially better than dsDNA as a conducting molecular wire.     

3D finite element analysis of electrostatic deflection of commercial and FIB-modified cantilevers for electric and Kelvin force microscopy: I. Triangular shaped cantilevers with symmetric pyramidal tips

The investigation of the nanoscale distribution of electrostatic forces on material surfaces is of paramount importance for the development of nanotechnology, since these confined forces govern many physical processes on which a large number of technological applications are based. For instance, electric force microscopy (EFM) and micro-electro-mechanical-systems (MEMS) are technologies based on an electrostatic interaction between a cantilever and a specimen. In the present work we report on a 3D finite element analysis of the electrostatic deflection of cantilevers for electric and Kelvin force microscopy. A commercial triangular shaped cantilever with a symmetric pyramidal tip was modelled. In addition, the cantilever was modified by a focused ion beam (FIB) in order to reduce its parasitic electrostatic force, and its behaviour was studied by computation analysis. 3D modelling of the electrostatic deflection was realized by using a multiphysics finite element analysis software and it was applied to the real geometry of the cantilevers and probes obtained by using basic CAD tools. The results of the modelling are in good agreement with experimental data.     

Control of curvature in highly compliant probe cantilevers during carbon nanotube growth

Direct growth of a sharp carbon nanotube (CNT) probe on a very thin and highly flexible cantilever by plasma-enhanced chemical vapor deposition (PECVD) is desirable for atomic force microscopy (AFM) of nanoscale features on soft or fragile materials. Plasma-induced surface stresses in such fabrication processes, however, tend to cause serious bending of these cantilevers, which makes the CNT probe unsuitable for AFM measurements. Here, we report a new tunable CNT growth technique that controls cantilever bending during deposition, thereby enabling the creation of either flat or deliberately curved AFM cantilevers containing a CNT probe. By introducing hydrogen gas to the (acetylene + ammonia) feed gas during CNT growth and adjusting the ammonia to hydrogen flow ratio, the cantilever surface stress can be altered from compressive to tensile stress, and in doing so controlling the degree of cantilever bending. The CNT probes grown under these conditions have high aspect ratios and are robust. Contact-mode imaging has been demonstrated using these probe tips. Such CNT probes can be useful for bio-imaging involving DNA and other delicate biological features in a liquid environment.     

Time-resolved electrostatic force microscopy of polymer solar cells

Blends of conjugated polymers with fullerenes, polymers, or nanocrystals make promising materials for low-cost photovoltaic applications. Different processing conditions affect the efficiencies of these solar cells by creating a variety of nanostructured morphologies, however, the relationship between film structure and device efficiency is not fully understood. We introduce time-resolved electrostatic force microscopy (EFM) as a means to measure photoexcited charge in polymer films with a resolution of 100 nm and 100 micros. These EFM measurements correlate well with the external quantum efficiencies measured for a series of polymer photodiodes, providing a direct link between local morphology, local optoelectronic properties and device performance. The data show that the domain centres account for the majority of the photoinduced charge collected in polyfluorene blend devices. These results underscore the importance of controlling not only the length scale of phase separation, but also the composition of the domains when optimizing nanostructured solar cells.     

原子力显微镜微悬臂梁杨氏模量动态测试方法

原子力显微镜微悬臂梁是微纳米领域重要的微力传感器,而微悬臂梁的杨氏模量又是决定其力学性能的重要参数.由于微悬臂梁的尺寸处于微米级,有些特征尺寸甚至达到纳米级,常规的测试结构材料特性的检测方法已经难以满足需求,急需研究新的测试方法和装置对微悬臂梁的机械特性进行研究和分析.本文提出了一种基于微悬臂梁振动固有频率测试的杨氏模量测试方法.使用本方法时,首先建立待测微悬臂梁在空气中的振动模型,并使用数值仿真的方法计算结构尺寸相同但杨氏模量不同的各种微悬臂梁在空气中的振动固有频率,然后实际测量微悬臂梁的振动固有频率,和实验结果最接近的仿真结果所对应的杨氏模量参数就是待测微悬臂梁的杨氏模量.本文最后对Mikromaseh公司生产的NSC型探针的杨氏模量进行了测试,实验结果证实了本文提出的方法的正确性.     

Probing electrostatic potentials in solution with carbon nanotube transistors

We have used single-walled carbon nanotube transistors to measure changes in the chemical potential of a solution due to redox-active transition-metal complexes. The interaction of the molecules with a gold electrolyte-gate wire changes the electrostatic potential sensed by the nanotube, which in turn shifts the gate-voltage dependence of the nanotube conductance. As predicted by the Nernst equation, this shift depends logarithmically on the ratio of oxidized to reduced molecules.     

3D finite element analysis of electrostatic deflection and shielding of commercial and FIB-modified cantilevers for electric and Kelvin force microscopy: II. Rectangular shaped cantilevers with asymmetric pyramidal tips

This paper deals with an application of 3D finite element analysis to the electrostatic interaction between (i) a commercial rectangular shaped cantilever (with an integrated anisotropic pyramidal tip) and a conductive sample, when a voltage difference is applied between them, and (ii) a focused ion beam (FIB) modified cantilever in order to realize a probe with reduced parasitic electrostatic force. The 3D modelling of their electrostatic deflection was realized by using multiphysics finite element analysis software and applied to the real geometry of the cantilevers and probes as used in conventional electric and Kelvin force microscopy to evaluate the contribution of the various part of a cantilever to the total force, and derive practical criteria to optimize the probe performances. We report also on the simulation of electrostatic shielding of nanometric features, in order to quantitatively evaluate an alternative way of reducing the systematic error caused by the cantilever-to-sample capacitive coupling. Finally, a quantitative comparison between the performances of rectangular and triangular cantilevers (part I of this work) is reported.     

Thermomagnetic fluctuations and hysteresis loops of magnetic cantilevers for magnetic resonance force microscopy

We have used frequency-shift cantilever magnetometry to study individual nickel magnets patterned at the end of ultra-sensitive silicon cantilevers for use in magnetic resonance force microscopy (MRFM). We present a procedure for inferring a magnet's full hysteresis curve from the response of cantilever resonance frequency versus magnetic field. Hysteresis loops and small-angle fluctuations were determined at 4.2 K with an applied magnetic field up to 6 T for magnets covering a range of dimensions and aspect ratios. Compared to magnetic materials with higher anisotropy, we find that nickel is preferable for MRFM experiments on nuclear spins at high magnetic fields.     

Electronic properties of a single-walled carbon nanotube/150mer-porphyrin system measured by point-contact current imaging atomic force microscopy

The electronic properties of a single-walled carbon nanotube/150mer of porphyrin polymer wire system were investigated. Current-voltage (I-V) curves were measured simultaneously along with topographic observations using point-contact current imaging atomic force microscopy. Symmetric I-V curves were obtained at bare single-walled carbon nanotubes but characteristic asymmetrical rectifying behavior was found at the single-walled carbon nanotube/150mer-porphyrin junctions. This finding is of key importance for the development of new nanoscale molecular electronic devices.     

Two-dimensional stick-slip on a soft elastic polymer: pattern generation using atomic force microscopy

It has been demonstrated that it is possible to create laterally differentiated frictional patterning and three-dimensional structures using an atomic force microscope (AFM) probe on the surface of a soft elastic polymer, poly(dimethylsiloxane) (PDMS). The resulting effect of contact mode imaging at low loading forces (<100?nN), observed in the lateral force mode, revealed a homogeneous pattern on the PDMS surface exhibiting higher friction. With higher loading forces ([Formula: see text]?nN) the effect is non-uniform, resulting in structures with depths on the nanometre scale. The topographic and frictional data revealed stick-slip responses in both the fast (orthogonal to the long axis of the lever) and slow (parallel to the long axis of the lever) directions of probe travel from scanning in a raster pattern. The stick-slip events are manifested in the form of a series of shallow channels spaced evenly apart on the polymer surface. Detailed friction loop analysis acquired during the manipulation process showed that the lateral force changed according to the strength of trapping of the tip with the polymer surface exhibiting significant in-plane deformation due to lateral forces being imposed. An incremental increase in the initial loading force resulted in an increase in in-plane displacement and a greater spacing between the stick lines/channels in the slow-scan direction. A decrease in channel length in the fast-scan direction is also observed as a result of an increase in static friction with normal force, resulting in greater surface deformation and shorter track length for sliding friction.     

Ultrasharp and high aspect ratio carbon nanotube atomic force microscopy probes for enhanced surface potential imaging

The resolution of scanning surface potential microscopy (SSPM) is mainly limited by non-local electrostatic interactions due to the finite probe size. Here we present high resolution surface potential imaging with ultrasharp and high aspect ratio carbon nanotube (CNT) atomic force microscopy (AFM) probes fabricated via dielectrophoresis. Enhancement of surface potential contrast by several factors is reported for integrated circuit structures and purple membrane fragments for these CNT AFM probes as compared to conventional probes. In particular, ultrahigh lateral resolution (～2?nm) surface potential images of self-assembled bacteriorhodopsin proteins are reported at ambient conditions, with the implication of label-free protein detection by SSPM techniques.