Complex dynamics of carbon nanotube probe tips

Carbon nanotube (CNT) tips in tapping mode atomic force microscopy (AFM) enable very high-resolution imaging, measurements, and manipulation at the nanoscale. We present recent results based on experimental analysis that yield new insights into the dynamics of CNT probe tips in tapping mode AFM. Experimental measurements are presented of the frequency response and dynamic amplitude-distance data of a high-aspect-ratio multi-walled (MW) CNT tip. Higher harmonics of the microcantilever are measured in frequency ranges corresponding to attractive regime and the repulsive regime where the CNT buckles dynamically. Surface scanning is performed using a MWCNT tip on a SiO(2) grating to verify the imaging instabilities associated with MWCNT buckling when used with normal control schemes in the tapping mode. Lastly, the choice of optimal setpoints for tapping mode control using CNT tip are discussed using the experimental results.     

Carbon nanotubes: a promising standard for quantitative evaluation of AFM tip apex geometry

The direct contact between tip and sample in atomic force microscopy (AFM) leads to demand for a quantitative knowledge of the AFM tip apex geometry in high-resolution AFM imaging and many other types of AFM applications like force measurements and surface roughness measurements. Given, the AFM tip apex may change continuously during measurements due to wear or during storage due to oxidation, it is very desirable to develop an easy and quick way for quantitative evaluation of AFM tip radius when necessary. In this study, we present an efficient method based on Zenhausern model (Scanning 14 (1992) 212) by measuring single-wall carbon nanotubes deposited on a flat substrate to reach this goal. Experimental results show the method can be used for routine quantitative evaluation of AFM tip apex geometry for tips with effective radii down to the nanometer scale.     

Direct deformation study of AFM probe tips modified by hydrophobic alkylsilane self-assembled monolayers

The in-use wear of atomic force microscopy (AFM) probe tips is crucial for the reliability of AFM measurements. Increase of tip size for several nanometers is difficult to monitor but it can already taint subsequent AFM data. We have developed a method to study the shape evolution of AFM probe tips in nanometer scale. This approach provides direct comparison of probe shape profiles, and thus can help in evaluation of the level of tip damage and quality of acquired AFM data. Consequently, the shape degradation of probes modified by hydrophobic alkylsilane self-assembled monolayers (SAMs) was studied. The tip wear length and wear volume were adopted to quantitatively verify the effectiveness of hydrophobic coatings. When compared with their silicon counterparts, probes modified by SAM materials exhibit superior wear-resistant behavior in tapping mode scans.     

Using defined structures on very thin foils for characterizing AFM tips

Knowledge of tip geometry is necessary for reproducible atomic force microscope (AFM) measurements. This is particularly important for measurements in contact mode, in which a certain wear of the tip will always occur. For small or flat structures or for structures of larger dimensions, knowledge of the tip radius and the entire tip geometry is important. Additionally, the tilt of the tip in relation to the sample is of importance. Normally, very complicated lithographically manufactured structures for tip characterization are used. In contrast, the structures shown in this work are very simple. For measuring the tip geometry very thin foils patterned by focused ion beam (FIB) were used. In this work we demonstrate the possibility of determining the AFM tip geometry and the tilt based on several different large structures. A proven algorithm was developed for the reconstruction of the tips. The shape of FIB-structured foils was determined by electron microscopy prior to AFM measurements. This new method for determining tip shape is also presented as it compares to other current methods. In this case a discussion on the stability and advantages of the new method is presented.     

Feasibility of multi-walled carbon nanotube probes in AFM anodization lithography

Multi-walled carbon nanotube (CNT) tips were used in atomic force microscope (AFM) anodization lithography to investigate their advantages over conventional tips. The CNT tip required a larger threshold voltage than the mother silicon tip due to the Schottky barrier at the CNT-Si interface. Current-to-voltage curves distinguished the junction property between CNTs and mother tips. The CNT-platinum tip, which is more conductive than the CNT-silicon tip, showed promising results for AFM anodization lithography. Finally, the nanostructures with high aspect ratio were fabricated using a pulsed bias voltage technique as well as the CNT tip.     

Evidence of commensurate contact and rolling motion: AFM manipulation studies of carbon nanotubes on HOPG

We report on experiments in which multiwall carbon nanotubes (CNTs) are manipulated with AFM on a graphite (HOPG) substrate. We find certain discrete orientations in which the lateral force of manipulation dramatically increases as we rotate the CNT in the plane of the HOPG surface with the AFM tip. The three-fold symmetry of these discrete orientations indicates commensurate contact of the hexagonal graphene surfaces of the HOPG and CNT. As the CNT moves into commensurate contact, we observe the motion change from sliding/rotating in-plane to stick–roll motion.     

Contact mechanics and tip shape in AFM-based nanomechanical measurements

Stiffness-load curves obtained in quantitative atomic force acoustic microscopy (AFAM) measurements depend on both the elastic properties of the sample and the geometry of the atomic force microscope (AFM) tip. The geometry of silicon AFM tips changes when used in contact mode, affecting measurement accuracy. To study the influence of tip geometry, we subjected ten AFM tips to the same series of AFAM measurements. Changes in tip shape were observed in the scanning electron microscope (SEM) between individual AFAM tests. Because all of the AFAM measurements were performed on the same sample, variations in AFAM stiffness-load curves were attributed to differences in tip geometry. Contact-mechanics models that assumed simple tip geometries were used to analyze the AFAM data, but the calculated values for tip dimensions did not agree with those provided by SEM images. Therefore, we used a power-law approach that allows for a nonspherical tip geometry. We found that after several AFAM measurements, the geometry of the tips at the very end is intermediate between those of a flat punch and a hemisphere. These results indicate that the nanoscale tip-sample contact cannot easily be described in terms of simple, ideal geometries.     

A torsional resonance mode AFM for in-plane tip surface interactions

Changing the method of tip/sample interaction leads to contact, tapping and other dynamic imaging modes in atomic force microscopy (AFM) feedback controls. A common characteristic of these feedback controls is that the primary control signals are based on flexural deflection of the cantilever probes, statically or dynamically. We introduce a new AFM mode using the torsional resonance amplitude (or phase) to control the feedback loop and maintain the tip/surface relative position through lateral interaction. The torsional resonance mode (TRmode™) provides complementary information to tapping mode for surface imaging and studies. The nature of tip/surface interaction of the TRmode facilitates phase measurements to resolve the in-plane anisotropy of materials as well as measurements of dynamic friction at nanometer scale. TRmode can image surfaces interleaved with TappingMode™ with the same probe and in the same area. In this way we are able to probe samples dynamically in both vertical and lateral dimensions with high sensitivity to local mechanical and tribological properties. The benefit of TRmode has been proven in studies of water adsorption on HOPG surface steps. TR phase data yields approximately 20 times stronger contrast than tapping phase at step edges, revealing detailed structures that cannot be resolved in tapping mode imaging. The effect of sample rotation relative to the torsional oscillation axis of the cantilever on TR phase contrast has been observed. Tip wear studies of TRmode demonstrated that the interaction forces between tip and sample could be controlled for minimum tip damage by the feedback loop.     

A relocated technique of atomic force microscopy (AFM) samples and its application in molecular biology

A kind of simple atomic force microscopy (AFM) relocated technique, which takes advantage of homemade sample locator system, is used for investigating repeatedly imaging of some specific species on the whole substrate (over 1 x 1 cm2) with resolution about 400 nm. As applications of this sample locator system, single extended DNA molecules and plasmid DNA network are shown in different AFM operational modes: tapping mode and contact mode with different tips after the substrates have been moved.     

Controlling tip–sample interaction forces during a single tap for improved topography and mechanical property imaging of soft materials by AFM

We introduce a method that exploits the “active” nature of the force-sensing integrated readout and active tip (FIRAT), a recently introduced atomic force microscopy (AFM) probe, to control the interaction forces during individual tapping events in tapping mode (TM) AFM. In this method the probe tip is actively retracted if the tip–sample interaction force exceeds a user-specified force threshold during a single tap while the tip is still in contact with the surface. The active tip control (ATC) circuitry designed for this method makes it possible to control the repulsive forces and indentation into soft samples, limiting the repulsive forces during the scan while avoiding instability due to attractive forces. We demonstrate the accurate topographical imaging capability of this method on suitable samples that possess both soft and stiff features.     

Comparison of different aminofunctionalization strategies for attachment of single antibodies to AFM cantilevers

Atomic force microscopy (AFM) has developed into a key technique for elucidation of biological systems on the single molecular level. In particular, molecular recognition force microscopy has proven to be a powerful tool for the investigation of biological interactions under near physiological conditions. For this purpose, ligands are tethered to AFM tips and the interaction forces with cognate receptors on the sample surface are measured with pico-Newton accuracy. In the first step of tip functionalization, amino groups are typically introduced on the initially inert AFM tip. Several methods have been developed to reproducibly adjust the desired low density of amino groups on the tip surface, i.e. esterification with ethanolamine, gas-phase silanization with aminopropyl-triethoxysilane (APTES), or treatment with aminophenyl-trimethoxysilane (APhS) in toluene solution. In the present study, the usefulness of these methods for attachments of antibodies to AFM tips was characterized by a standardized test system, in which biotinylated IgG was bound to the tip and a dense monolayer of avidin on mica served as test sample. All three methods of aminofunctionalization were found fully satisfactory for attachment of single antibodies to AFM tips, only in a parallel macroscopic assay on silicon nitride chips a minor difference was found in that APTES appeared to yield a slightly lower surface density of amino groups.     

Analysis of dynamic cantilever behavior in tapping mode atomic force microscopy

Tapping mode atomic force microscopy (AFM) provides phase images in addition to height and amplitude images. Although the behavior of tapping mode AFM has been investigated using mathematical modeling, comprehensive understanding of the behavior of tapping mode AFM still poses a significant challenge to the AFM community, involving issues such as the correct interpretation of the phase images. In this paper, the cantilever's dynamic behavior in tapping mode AFM is studied through a three dimensional finite element method. The cantilever's dynamic displacement responses are firstly obtained via simulation under different tip‐sample separations, and for different tip‐sample interaction forces, such as elastic force, adhesion force, viscosity force, and the van der Waals force, which correspond to the cantilever's action upon various different representative computer‐generated test samples. Simulated results show that the dynamic cantilever displacement response can be divided into three zones: a free vibration zone, a transition zone, and a contact vibration zone. Phase trajectory, phase shift, transition time, pseudo stable amplitude, and frequency changes are then analyzed from the dynamic displacement responses that are obtained. Finally, experiments are carried out on a real AFM system to support the findings of the simulations. Microsc. Res. Tech. 78:935–946, 2015. © 2015 Wiley Periodicals, Inc.     

Manipulation, dissection, and lithography using modified tapping mode atomic force microscope

A modified tapping mode of the atomic force microscope (AFM) was introduced for manipulation, dissection, and lithography. By sufficiently decreasing the amplitude of AFM tip in the normal tapping mode and adjusting the setpoint, the tip-sample interaction can be efficiently controlled. This modified tapping mode has some characteristics of the AFM contact mode and can be used to manipulate nanoparticles, dissect biomolecules, and make lithographs on various surfaces. This method did not need any additional equipment and it can be applied to any AFM system.     

Performance of the carbon nano-tube assembled tip for surface shape characterization

The carbon nano-tube (CNT) has ideal properties for atomic force microscope (AFM) tips. We assembled a CNT using 2 three-axial manipulators in a scanning electron microscope (SEM) chamber. In this process, the length and angle of the CNT were adjusted by observing the SEM image, after which the CNT was glued by amorphouscarbon. The results of performance are as follows. The lifetime of the CNT tip proved to be 5 times better than that of the silicon tip when continuously measuring the micro-roughness of a Czochralski (Cz) P-type (100) silicon wafer. The CNT tip is able to trace a narrow space (width less than 1 microm) better than the conventional silicon tip because of its high aspect ratio. The relationship between the observed image and CNT geometry is discussed herein.     

碳纳米管原子力显微镜针尖的制作研究

研究在光学显微镜下，运用两个独立的三维工作台分别控制针尖和碳纳米管的位置，将碳纳米管吸附在传统的原子力显微镜针尖上。首先将碳纳米管粘附在导电的胶带上，然后用涂胶的针尖与其接触将碳纳米管粘附到针尖上，最后运用电蚀的方法优化碳纳米管针尖的长度，以达到高分辨率的要求。运用制作的碳纳米管针尖对硅表面的深槽进行成像，获得了传统针尖无法得到的信息。     

Dual resonance excitation system for the contact mode of atomic force microscopy

We propose an improved system that enables simultaneous excitation and measurements of at least two resonance frequency spectra of a vibrating atomic force microscopy (AFM) cantilever. With the dual resonance excitation system it is not only possible to excite the cantilever vibrations in different frequency ranges but also to control the excitation amplitude for the individual modes. This system can be used to excite the resonance frequencies of a cantilever that is either free of the tip-sample interactions or engaged in contact with the sample surface. The atomic force acoustic microscopy and principally similar methods utilize resonance frequencies of the AFM cantilever vibrating while in contact with the sample surface to determine its local elastic modulus. As such calculation demands values of at least two resonance frequencies, two or three subsequent measurements of the contact resonance spectra are necessary. Our approach shortens the measurement time by a factor of two and limits the influence of the AFM tip wear on the values of the tip-sample contact stiffness. In addition, it allows for in situ observation of processes transpiring within the AFM tip or the sample during non-elastic interaction, such as tip fracture.     

Dynamic analysis of tapping mode atomic force microscope (AFM) for critical dimension measurement

Transient dynamics of tapping mode atomic force microscope (AFM) for critical dimension measurement are analyzed. A simplified nonlinear model of AFM is presented to describe the forced vibration of the micro cantilever-tip system with consideration of both contact and non-contact transient behavior for critical dimension measurement. The governing motion equations of the AFM cantilever system are derived from the developed model. Based on the established dynamic model, motion state of the AFM cantilever system is calculated utilizing the method of averaging with the form of slow flow equations. Further analytical solutions are obtained to reveal the effects of critical parameters on the system dynamic performance. In addition, features of dynamic response of tapping mode AFM in critical dimension measurement are studied, where the effects of equivalent contact stiffness, quality factor and resonance frequency of cantilever on the system dynamic behavior are investigated. Contact behavior between the tip and sample is also analyzed and the frequency drift in contact phase is further explored. Influence of the interaction between the tip and sample on the subsequent non-contact phase is studied with regard to different parameters. The dependence of the minimum amplitude of tip displacement and maximum phase difference on the equivalent contact stiffness, quality factor and resonance frequency are investigated. This study brings further insights into the dynamic characteristics of tapping mode AFM for critical dimension measurement, and thus provides guidelines for the high fidelity tapping mode AFM scanning.     

Simulation-aided design and fabrication of nanoprobes for scanning probe microscopy

We proposed and demonstrated a flexible and effective method to design and fabricate scanning probes for atomic force microscopy applications. Computer simulations were adopted to evaluate design specifications and desired performance of atomic force microscope (AFM) probes; the fabrication processes were guided by feedback from simulation results. Through design-simulation-fabrication iterations, tipless cantilevers and tapping mode probes were successfully made with errors as low as 2% in designed resonant frequencies. For tapping mode probes, the probe tip apex achieved a 10 nm radius of curvature without additional sharpening steps; tilt-compensated probes were also fabricated for better scanning performance. This method provides AFM users improved probe quality and practical guidelines for customized probes, which can support the development of novel scanning probe microscopy (SPM) applications.     

Origin of phase shift in atomic force microscopic investigation of the surface morphology of NR/NBR blend film

Atomic force microscopy (AFM) was used to study the morphology and surface properties of NR/NBR blend. Blends at 1/3, 1/1 and 3/1 weight ratios were prepared in benzene and formed film by casting. AFM phase images of these blends in tapping mode displayed islands in the sea morphology or matrix-dispersed structures. For blend 1/3, NR formed dispersed phase while in blends 1/1 and 3/1 phase inversion was observed. NR showed higher phase shift angle in AFM phase imaging for all blends. This circumstance was governed by adhesion energy hysteresis between the device tip and the rubber surface rather than surface stiffness of the materials, as proved by force distance measurements in the AFM contact mode.     

Scanning tunnelling and atomic force microscopy performed with the same probe in one unit

The technique demonstrated here provides features of both scanning tunnelling microscopy (STM) and atomic force microscopy (AFM). The metallic probe acts to record current variations and sense forces from the same sample area simultaneously. Thus, separate images may be recorded, in registry. The collected data allows real space correlations between some electrical properties and the geometric structure of a sample surface. The same tip is used since the geometry and condition of the tip can effect the data recordings. Platinum alloys, tungsten and graphite tips have been employed successfully. An AFM lever can respond to surface contact forces, within the elastic limits of the sample, while electric current is sensed by the tip of the lever. The usefulness of this experimental procedure is tested here by an application to semiconducting samples of Ag-doped CdTe in air and in paraffin oil media.