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.     

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.     

Attachment of carbon nanotubes to atomic force microscope probes

In atomic force microscopy (AFM) the accuracy of data is often limited by the tip geometry and the effect on this geometry of wear. One way to improve the tip geometry is to attach carbon nanotubes (CNT) to AFM tips. CNTs are ideal because they have a small diameter (typically between 1 and 20nm), high aspect ratio, high strength, good conductivity, and almost no wear. A number of methods for CNT attachment have been proposed and explored including chemical vapour deposition (CVD), dielectrophoresis, arc discharge and mechanical attachment. In this work we will use CVD to deposit nanotubes onto a silicon surface and then investigate improved methods to pick-up and attach CNTs to tapping mode probes. Conventional pick-up methods involve using standard tapping mode or non-contact mode so as to attach only those CNTs that are aligned vertically on the surface. We have developed improved methods to attach CNTs using contact mode and reduced set-point tapping mode imaging. Using these techniques the AFM tip is in contact with a greater number of CNTs and the rate and stability of CNT pick-up is improved. The presence of CNTs on the modified AFM tips was confirmed by high-resolution AFM imaging, analysis of the tips dynamic force curves and scanning electron microscopy (SEM).     

High-yield synthesis of conductive carbon nanotube tips for multiprobe scanning tunneling microscope

We have established a fabrication process for conductive carbon nanotube (CNT) tips for multiprobe scanning tunneling microscope (STM) with high yield. This was achieved, first, by attaching a CNT at the apex of a supporting W tip by a dielectrophoresis method, second, by reinforcing the adhesion between the CNT and the W tip by electron beam deposition of hydrocarbon and subsequent heating, and finally by wholly coating it with a thin metal layer by pulsed laser deposition. More than 90% of the CNT tips survived after long-distance transportation in air, indicating the practical durability of the CNT tips. The shape of the CNT tip did not change even after making contact with another metal tip more than 100 times repeatedly, which evidenced its mechanical robustness. We exploited the CNT tips for the electronic transport measurement by a four-terminal method in a multiprobe STM, in which the PtIr-coated CNT portion of the tip exhibited diffusive transport with a low resistivity of 1.8 kOmega/microm. The contact resistance at the junction between the CNT and the supporting W tip was estimated to be less than 0.7 kOmega. We confirmed that the PtIr thin layer remained at the CNT-W junction portion after excess current passed through, although the PtIr layer was peeled off on the CNT to aggregate into particles, which was likely due to electromigration or a thermally activated diffusion process. These results indicate that the CNT tips fabricated by our recipe possess high reliability and reproducibility sufficient for multiprobe STM measurements.     

A novel cleaning method of gold-coated atomic force microscope tips for their chemical modification

For chemical modification of gold-coated AFM tips with thiol or sulfide compounds, a new two-step precleaning procedure was studied. The two-step cleaning procedure involves (i) oxidation of organic contaminants on the AFM tips with ozone treatment and (ii) reduction of the oxidized gold surface by immersing the oxidized tip into pure hot ethanol at ca. 65 degrees C. The chemically modified tips prepared from gold-coated AFM tips precleaned by the two-step procedure gave almost the same tip characteristics as those chemically modified immediately after gold vapor deposition in a factory. The present two-step cleaning procedure can be used widely for chemical modification of commercially available gold-coated AFM tips with thiol or disulfide compounds for chemical force microscopy.     

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.     

The study on the atomic force microscopy base nanoscale electrical discharge machining

This study proposes an innovative atomic force microscopy (AFM) based nanoscale electrical discharge machining (AFM-based nanoEDM) system which combines an AFM with a self-produced metallic probe and a high-voltage generator to create an atmospheric environment AFM-based nanoEDM system and a deionized water (DI water) environment AFM-based nanoEDM system. This study combines wire-cut processing and electrochemical tip sharpening techniques on a 40-μm thick stainless steel sheet to produce a high conductive AFM probes, the production can withstand high voltage and large current. The tip radius of these probes is approximately 40 nm. A probe test was executed on the AFM using probes to obtain nanoscales morphology of Si wafer surface. The silicon wafer was as a specimen to carry out AFM-base nanoEDM process in atmospheric and DI water environments by AFM-based nanoEDM system. After experiments, the results show that the atmospheric and DI water environment AFM-based nanoEDM systems operate smoothly. From experimental results, it can be found that the electric discharge depth of the silicon wafer at atmospheric environments is a mere 14.54 nm. In a DI water environment, the depth of electric discharge of the silicon wafer can reach 25.4 nm. This indicates that the EDM ability of DI water environment AFM-based nanoEDM system is higher than that of atmospheric environment AFM-based nanoEDM system. After multiple nanoEDM process, the tips become blunt. After applying electrochemical tip sharpening techniques, the tip radius can return to approximately 40 nm. Therefore, AFM probes produced in this study can be reused.     

Effect of tip geometry of atomic force microscope on mechanical responses of bovine articular cartilage and agarose gel

The objective of this study is to investigate the effect of different Atomic Force Microscope (AFM) tip geometries (sharp-conical and spherical tips) on the microscale Young’s modulus of bovine articular cartilage and agarose gel that is calculated by the method of the average point-wise modulus. The measurements of the microscale Young’s moduli of 3% agarose gel under a conical AFM tip (20.9±4.9 kPa) and under a spherical AFM tip (17.5±3.0 kPa), averaged over an indentation depth of 600 nm, were comparable. However, the microscale Young’s moduli of articular cartilage, as measured with a conical AFM tip (116.9±62.9 kPa), were significantly higher than the corresponding values under a spherical AFM tip (30.9±14.3 kPa). The results of the current study suggest that the AFM tip geometry affects the microscale measurements of the mechanical properties on the surfaces of biological materials. The findings of the study can help to elucidate more accurately the microscale mechanical properties on the surface layers of diverse biological materials including tissue-engineered cartilages with different material characteristics.     

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.     

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.     

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.     

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。     

运用碳纳米管原子力显微镜针尖减小长程力作用的研究

减小探针和样品表面之间的长程宏观力是原子力显微镜获得高分辨率成像的关键。首先通过理论分析得出影响长程力的主要因素是探针的几何形状和尺寸。然后分别运用几何形状和尺寸不同的原子力显微镜的传统Si针尖和碳纳米管针尖对样品进行扫描试验研究,结果显示碳纳米管针尖较传统针尖获得了高分辨率的图像。这一结果表明,碳纳米管针尖减小了成像中宏观长程作用力的影响,是理想的原子力显微镜针尖。     

Using carbon nanotube probes for high-resolution three-dimensional imaging of cells

While atomic force microscopy (AFM) has become a promising tool for visualizing membrane morphology of cells, many studies have reported the presence of artifacts such as cliffs on the edges of cells. These artifacts shield important structural features such as lamellopodia, filopodia, microvilli and membrane ridges, which represent characteristic status in signaling processes such as spreading and activation. These cliff-like edges arise from a premature contact of the probe side contact with the cell prior to the probe top apex-cell contact. Carbon nanotube (CNT) modified AFM probes were utilized to address this drawback. Using rat basophilic leukemia (RBL) cells, this work revealed that CNT probes diminish cliff-like artifacts and enabled visualization of entire membrane morphology and structural features in three dimensions. The high aspect ratio of CNT probes provides a very effective remedy to the cliff-like artifacts as well as tip convolution of conventional probes, which shall enhance the validity and application of AFM in cellular biology research.     

Atomic force microscope tip cleaning by using gratings as micro‐washboards

The sharpness of atomic force microscope (AFM) tips is essential for acquiring high quality AFM images. However, AFM tips would easily get contaminated during scanning and storage at ambient condition, which influences image resolution and causes image distortion. Replacing the probe frequently is a solution, but uneconomical. To solve this problem, several tip cleaning methods have been proposed but there is space for further improvement. Therefore, this article developed a method of tip cleaning by using a one‐dimensional grating (600 lines/mm) as a micro‐washboard to “wash” contaminated tips. We demonstrate that the contaminants can be scrubbed away by rapidly scanning such micro‐washboard against the tip in the aids of Z‐dithering (10–20 Hz) exerted on the washboard. This method is highly efficient and proved to be superior to traditional ones. Experiments show that AFM images acquired with “washed” tips have higher resolution and less distortion compared with images acquired using contaminated tips, even comparable to those scanned by new ones. Microsc. Res. Tech. 76:1131–1134, 2013. © 2013 Wiley Periodicals, Inc.     

Characterization of nanoscale recording mark on Ge2Sb2Te5 film

We have fabricated nanoscale recording marks on Ge(2)Sb(2)Te(5) (GST) films with conductive atomic force microscope (AFM). GST films were deposited on glass or polyimide film with thickness of 150-200nm by the rf-sputtering method. Through current-voltage (I-V) spectroscopy, good cantilevers for fabrication and characterization of nanoscale marks on GST were selected. A fresh and highly conductive tip showed voltage-switching characteristic in the I-V curve, where the threshold voltage was approximately 1.6V. Nanoscale dot and wire arrays of crystalline phases were successfully obtained by varying sample bias voltage from -10 to 10V. With highly conductive tips, nanowires having full-width at half-maximum of approximately 20nm could be fabricated, whereas nanowires could not be fabricated with bias voltage below -2V. The width of the nanoscale mark was increased by repetition of AFM lithography even with same applied voltage and lithography speed. For a thicker nanowire, the width measured in current-image (C-image) was observed to be approximately 2 times of that measured in topography-image (T-image). This result supports that current sensing provides an image of phase-changed GST area with higher resolution than topography sensing.     

Membrane deformation of living glial cells using atomic force microscopy

Using atomic force microscopy (AFM) it has been possible to detect actin filaments that are beneath the cell membrane of living cells despite the fact that the AFM tip is applied to the surface of the cell. To determine whether the AFM tip actually penetrates or deforms the cell membrane we determined whether an intracellularly trapped fluorescent indicator was lost from cells during AFM. Using epi-fluorescence illumination to monitor the presence of fluo-3 in the cell, we found that AFM did not cause dye leakage from the cell. Further, force–distance curves indicated that standard tips did not penetrate the membrane while sharper Supertips^TM did. In addition, the physiology of cells was found to be unaffected by AFM with standard tips since volume regulatory signal transduction mechanisms were intact in such studies. Thus, traditional AFM tips deform the cell membrane in order to reveal the presence of subcellular structures.     

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.     

Fabrication of various tip-size AFM probes for evaluating single-molecular retraction force between actin and anti-actin

The authors fabricated a probe tip with various sizes and examined the size dependency of the probe tip on the distribution of retraction forces between actin and anti-actin. Probe tips of various sizes were fabricated by two-photon polymerization methods on a micro cantilever of an atomic force microscope (AFM). The authors succeeded in fabricating a spherical tip having a smooth surface and the tip size varied between φ 0.8 and 5.5 μm. Anti-actin was immobilized on the fabricated probe tips and force curves were measured against an actin-immobilized mica substrate by AFM to analyze the retraction forces. The histograms of retraction forces showed that the single-molecular retraction force between actin and anti-actin was ca. 350–400 pN. It was observed that the average retraction forces for each tip size correlated with the square of the tip radius.     

Correlation Between Mechanical Properties and Nanofriction of [Ti–Cr/Ti–Cr–N] n and [Ti–Al/Ti–Al–N] n Multilayers

In this work, thin films deposited by pulsed DC magnetron sputtering of [Ti–Al/Ti–Al–N] _n and [Ti–Cr/Ti–Cr–N] _n multilayers of nanometric periods were analyzed by AFM in contact mode to measure values of lateral and normal forces. From these measurements, the coefficient of friction (COF) of these materials in contact with the AFM tip was calculated. Measurements were made with three types of silicon tips, diamond-coated, Pt–Cr-coated, and bare silicon. Significant differences between the tip materials in contact with the samples, which affected the COF, were observed. The effect of the environmental layer of water covering the surface sample and the tip appears as the most important factor affecting the tribology behavior of the tip-sample contact. For diamond-coated and bare silicon tips there is an additional adherence force increasing the normal load. But for tips platinum–chromium-coated there is a repulsive force due to this water layer, which behaves as a lubricant layer before a threshold load.