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.     

Imaging streptavidin 2D crystals on biotinylated lipid monolayers at high resolution with the atomic force microscope

Streptavidin crystals were grown on biotinylated lipid monolayers at an air/water interface and transferred onto highly oriented pyrolytic graphite (HOPG). These arrays could be imaged to a resolution below 1 nm using the atomic force microscope. The surface topographs obtained were compared with negative-stain electron microscopy images and the atomic model as determined by X-ray crystallography. The streptavidin tetramer (60 kDa) exposes two free biotin-binding sites to the buffer solution, while two are occupied by linkage to the lipid monolayer. Therefore, the streptavidin 2D crystals can be used as nanoscale matrices for binding biotinylated compounds. Furthermore, this HOPG-based preparation method provides a general novel approach to study the structure of protein arrays assembled on lipid monolayers with the AFM.     

Differences between nanoscale structural and electrical properties of AZO:N and AZO used in polymer light‐emitting diodes

Conducting atomic force microscopy and scanning surface potential microscopy were adopted to investigate the nanoscale surface electrical properties of N‐doped aluminum zinc oxide (AZO:N) films that were prepared by pulsed laser deposition (PLD) at various substrate temperatures. Experimental results demonstrated that when the substrate temperature is 150°C and the N₂O background pressure is 150 mTorr, the N‐dopant concentration on the surface is optimal. In addition, the root‐mean‐square roughness value of the film surface, the low contact current (<400 nA) conducting region as a percentage of the total area, and the mean work function value are 1.43 nm, 96.9%, and 4.88 eV, respectively, all of which are better than those of the optimal AZO film made by PLD. This result indicates that N‐doped AZO films are better for use as window materials in polymer light‐emitting diodes. Microsc. Res. Tech., 2010. © 2009 Wiley‐Liss, Inc.     

超薄类金刚石膜纳米摩擦性能研究

使用原子力显微镜对由微波等离子体电子回旋共振化学气相沉积技术制备的超薄类金刚石薄膜的纳米摩擦性能进行了研究。结果表明：氢化非晶碳膜(a-C：H)的摩擦力和外加载荷基本成线性关系，可以使用修正的Amonton公式进行表征；厚度在64．9nm以下薄膜的微观承载性能和膜厚存在明显的正比例关系。通过分析磨损深度和循环次数之间的关系以及对磨损区域的导电性研究，表明a-C：H膜表层的微观承载性能较其内层相差很大，表面存在着一层软膜。     

High-voltage nano-oxidation in deionized water and atmospheric environments by atomic force microscopy

This study used atomic force microscopy (AFM), metallic probes with a nanoscale tip, and high-voltage generators to investigate the feasibility of high-voltage nano-oxidation processing in deionized water (DI water) and atmospheric environments. Researchers used a combination of wire-cutting and electrochemical etching to transform a 20-μm-thick stainless steel sheet into a conductive metallic AFM probe with a tip radius of 60 nm, capable of withstanding high voltages. The combination of AFM, high-voltage generators, and nanoscale metallic probes enabled nano-oxidation processing at 200 V in DI water environments, producing oxides up to 66.6 nm in height and 467.03 nm in width. Oxides produced through high-voltage nano-oxidation in atmospheric environments were 117.29 nm in height and 551.28 nm in width, considerably exceeding the dimensions of those produced in DI water. An increase in the applied bias voltage led to an apparent logarithmic increase in the height of the oxide dots in the range of 200-400 V. The performance of the proposed high-voltage nano-oxidation technique was relatively high with seamless integration between the AFM machine and the metallic probe fabricated in this study.     

Rapid and accurate measurement for phase-change optical recording bits

Conducting atomic force microscopy (CAFM) and scanning surface potential microscopy (SSPM) have been used to image the phase-change optical recording bits. Commercially available digital versatile discs (DVD) + rewritable (RW) with initialization process were measured in experiments. Comparing the measurement results of both, the measurement resolution of CAFM is far superior to that of SSPM. With the DVD + RW disc rotating at a linear speed of 3.5 m/s, appropriate writing laser power range, may be precisely identified by CAFM as 10-15 mW. This is sufficient to verify the high-resolution recording bits research method. This new method may also be applied to the development of new types of phase-change recording materials.     

Evaluation of surface roughness and nanostructure of indium tin oxide (ITO) films by atomic force microscopy

Indium tin oxide was deposited on a glass (soda lime glass) by radiofrequency sputtering system at different sputtering gas (argon/oxygen 90/10%) pressures (20-34 mTorr) at room temperature. The sputtering rate was affected by the sputtering gas pressure. The optimum sputtering gas pressure was found to be 27 mTorr. The samples at different thicknesses (168, 300, 400, 425, 475, 500 and 630 nm) were deposited on the substrate. Transparency, electrical conductivity and surface roughness of the films were characterized. The samples were annealed at 350, 400 and 450 degrees C to evaluate annealing process effects on the concerned parameters and, therefore, the above-mentioned measurements were repeated again. The films exhibited reasonable optical transmittance and electrical conductivity and greatly improved after annealing. The characterization was focused on the scanning of the film surfaces before and after annealing, which has a prominent effect on the optical properties of the films. Film surfaces were scanned by scanning probe microscopy in contact atomic force mode. The most consideration was devoted to image analysis.     

SEM investigation of interfacial dislocations in nickel-base superalloys

Chromatography is a widely used separation unit operation for separating nanomaterials such as proteins and enzymes, quantum dots and carbon nanotubes. An understanding of the chromatographic stationary phase on a nanoscale would be extremely helpful in improving the process and developing efficient and new materials. This study is an attempt to characterize the stationary phase in its swollen wet state using environmental scanning electron microscope (ESEM) and atomic force microscopy (AFM). Observation of the wet beads using ESEM is limited to a micron-range resolution. However, AFM can be used in wet mode to characterize the stationary phase in both wet and dry states with nanometric resolution. In the swollen state, microscale cracks were observed on the surface and this may explain the high mass transfer rate and lower back pressures of the stationary phase. The structures on the surface of the stationary phase depict that the micron-sized beads may be composed of nanometric beads.     

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.     

Assembling and imaging of his-tag green fluorescent protein on mica surfaces studied by atomic force microscopy and fluorescence microscopy

The adsorption of his-tag green fluorescent protein (GFPH(6)) onto the mica surfaces has been studied by atomic force microscopy (AFM) and laser confocal fluorescence microscopy. By controlling the adsorption conditions, separated single GFPH(6) and GFPH(6) monolayer can be adsorbed and formed on mica surfaces. In present experiments, based on the AFM measurement, we found that the adsorbed GFPH(6) was bound on the mica surface with its beta-sheets. The formed GFPH(6) monolayer on mica surfaces was flat, uniform, and stable. Some applications of the formed monolayer have been demonstrated. The formed monolayer can be used as a substrate for DNA imaging and AFM mechanical lithography.     

Nanoscale electrical characterization of semiconducting polymer blends by conductive atomic force microscopy (C-AFM)

For the first time local electrical characteristics of a blend of two semiconducting polymers were studied with conductive atomic force microscopy (C-AFM). The investigated mixture is potentially interesting as the active layer in plastic photovoltaic devices. Besides conventional topography analysis of morphology and phase separation, the internal structure of the active layer was investigated by observing the current distribution with nanoscale spatial resolution. Similar to force spectroscopy, current imaging spectroscopy was performed during scanning the sample surface. Different types of current-voltage (I-V) characteristics were extracted from the array of spectroscopic data obtained from each point of the scans, and local heterogeneities of the electric characteristic were determined and discussed.     

Implementation of a piezoresistive MEMS cantilever for nanoscale force measurement in micro/nano robotic applications

The nanoscale sensing and manipulation have become a challenging issue in micro/nanorobotic applications. In particular, a feedback sensor-based manipulation is necessary for realizing an efficient and reliable handling of particles under uncertain environment in a micro/ nano scale. This paper presents a piezoresistive MEMS cantilever for nanoscale force measurement in microrobotics. A piezoresistive MEMS cantilever enables sensing of gripping and contact forces in nanonewton resolution by measuring changes in the stress-induced electrical resistances. The calibration of a piezoresistive MEMS cantilever is experimentally carried out. In addition, as part of the work on nanomanipulation with a piezoresistive MEMS cantilever, the analysis on the interaction forces between a tip and a material, and the associated manipulation strategies are investigated. Experiments and simulations show that a piezoresistive MEMS cantilever integrated into a microrobotic system can be effectively used in nanoscale force measurements and a sensor-based manipulation.     

Optimized hand fabricated AFM probes for simultaneous topographical and electrochemical tapping mode imaging

In this work hybrid AFM-electrochemical (SECM) probes to be used in dynamic atomic force microscopy are presented. These nanosensors are hand fabricated from gold microwires using a simple benchtop method. They display proportions close to commercially available silicon and silicon nitride cantilevers giving comparable performance in terms of resolution and imaging stability. The remarkable characteristic of these hybrid nanosensors is that they allow the coupling of 3D imaging ability and versatility of atomic force microscopy with the power of electrochemical methods. Local measurement of electrochemical-activity of a test sample consisting of gold bands functionalized by redox-labeled nanometer-sized polyethylene glycol chains has been achieved with simultaneous imaging of the 3D surface topography at high resolution. These hybrid AFM-SECM tips are capable of sensing local electrochemical currents down to ∼10 fA emphasizing the sensitivity and resolution of this technique.     

An AFM study of single-contact abrasive wear: The Rabinowicz wear equation revisited

A nanoscale study of the abrasive wear behaviour of a ductile monophasic metallic alloy (the stainless steel AISI 316L) is presented. By using atomic force microscopy (AFM) based techniques, particularly a diamond tip mounted on a stiff steel cantilever, the contact of a single abrasive asperity was simulated, and it was possible to determine accurately the load threshold below which no measurable wear occurs. It was observed that, once this nanoscale threshold for wear is overcome, the worn volume increases linearly with the load, as predicted by the Rabinowicz model. However, it was found that, although this critical threshold for measurable wear is most certainly related with the yield-onset of plastic deformation, it cannot be predicted by using directly a criterion based on the bulk microhardness. Hence, the results presented in this paper strongly indicate that indentation size effects play a crucial role on the response to abrasive wear at the asperity contact level.     

High accuracy FIONA-AFM hybrid imaging

Multi-protein complexes are ubiquitous and play essential roles in many biological mechanisms. Single molecule imaging techniques such as electron microscopy (EM) and atomic force microscopy (AFM) are powerful methods for characterizing the structural properties of multi-protein and multi-protein-DNA complexes. However, a significant limitation to these techniques is the ability to distinguish different proteins from one another. Here, we combine high resolution fluorescence microscopy and AFM (FIONA-AFM) to allow the identification of different proteins in such complexes. Using quantum dots as fiducial markers in addition to fluorescently labeled proteins, we are able to align fluorescence and AFM information to ≥8 nm accuracy. This accuracy is sufficient to identify individual fluorescently labeled proteins in most multi-protein complexes. We investigate the limitations of localization precision and accuracy in fluorescence and AFM images separately and their effects on the overall registration accuracy of FIONA-AFM hybrid images. This combination of the two orthogonal techniques (FIONA and AFM) opens a wide spectrum of possible applications to the study of protein interactions, because AFM can yield high resolution (5-10 nm) information about the conformational properties of multi-protein complexes and the fluorescence can indicate spatial relationships of the proteins in the complexes.     

Optimization of the film coating process for polymer blends by the grey-based Taguchi method

The purpose of this paper is to find the optimum conditions of the film coating process for polymer blends and the influence of major processing parameters on the morphological properties of the material surface has been discussed. The surface roughness is regarded as the target characteristic of the smaller-the-better system. In order to achieve the aim of the multiple-response process of robustness, the grey-based Taguchi method is proposed. Nine experimental trials based on the L₉(3⁴) orthogonal array are conducted to determine the optimum processing conditions, the significant factor levels, and the percent contributions together with the analysis of variance (ANOVA). Also, confirmation experiments are performed to verify that the experimental results are reproducible. Moreover, atomic force microscopy (AFM) can be carried out with 3D atomic resolution in air for the measurement and analysis of the precision surface .     

Optimized sample preparation for high-resolution AFM characterization of fixed human cells

Atomic force microscopy enables the simultaneous acquisition of high-resolution topographical and biophysical data allowing integrated analysis of cell surfaces during development and pathogenesis, and, critically, can link molecular and biophysical events. Here we used atomic force microscopy to analyse endometrial epithelial cells and neuronally differentiated P19 cells. Optimized reproducible sample preparation techniques enabled micro- and nanoscale multi-parameter analysis. Comparative analysis using atomic force microscopy and scanning electron microscopy demonstrated the utility of atomic force microscopy for examining tissue morphology, and its ability to generate data allowing differentiation of cells from different origins to be monitored. At low resolution atomic force microscopy produced topographic data complementary to scanning electron microscopy images, whilst at high resolution atomic force microscopy captured novel cell surface structural detail for both epithelial and neuronal cell types. Analysis of surface roughness provided biophysical data which enabled qualitative and quantitative differences between samples to be measured. This study provides an important optimization of sample preparation enabling more generalized atomic force microscopy utilization for cellular analysis required for advanced cell surface morphological studies.     

The effect of deformation on the lateral resolution of atomic force microscopy

A computer model based on the elastic properties of rubber is introduced for the evaluation of the lateral resolution in atomic force microscopy of deformable specimens. The computational results show that, if the full width at half-height can be defined as the lateral resolution, it is continuously improved at greater probe forces, at the expense of a reduced molecular height. In fact, even for a probe that is bigger than the molecule, the real size of the molecule can be 'recovered' at about 25% compression. This result demonstrates that for a better lateral resolution, a greater probe force can be beneficial, provided that the molecule is not moved or damaged and the response remains elastic. Measurements on isolated low-density lipoproteins (LDL) show that with 26% vertical compression, the lateral size measured in atomic force microscopy is only about 72% of the value predicted by a simple convolution, and is only slightly larger (≈ 13%) than the known size of LDL. Therefore, the results on LDL provide a direct support for the conclusions of the computational model.     

Nanoscale surface electrical properties of zinc oxide films investigated by conducting atomic force microscopy

In this study, conducting atomic force microscopy was employed to investigate the nanoscale surface electrical properties of zinc oxide (ZnO) films prepared by pulsed laser deposition (PLD) at different substrate temperatures for use as anode materials in polymer light-emitting diodes. The results show that the surface conductivity distribution of ZnO is related to its surface structure. At substrate temperatures of 150-200 degrees C, the conducting regions may cover over 90% of the ZnO thin-film surface, thus providing the best local conductivity. Moreover, heating at substrate temperatures of above 250 degrees C can effectively make the conductivity on the ZnO surface uniform. In particular, at substrate temperatures of around 300 degrees C, the conducting regions where currents are between 1 and 2 muA may cover as much as 83% of the surface, and furthermore, the transmission ratio in the visible range is higher than 80%. This is a rather ideal production temperature for the PLD for ZnO films.     

Measuring material softening with nanoscale spatial resolution using heated silicon probes

This article describes the use of heated silicon atomic force microscopy probes to perform local thermal analysis (LTA) of a thin film of polystyrene. The experiments measure film softening behavior with 100 nm spatial resolution, whereas previous research on LTA used probes that had a resolution near 10 microm, which was too large to investigate some types of features. This article demonstrates four methods by which heated silicon probes can perform thermal analysis with nanoscale spatial resolution. The polystyrene softening temperature measured from nanoscale LTA techniques is 120 degrees C, compared to 100 degrees C, measured with bulk ellipsometry. The discrepancy is attributed to the thermal contact resistance at the end of the silicon probe tip, on the order of 10(7)K/W, which modulates heat flow between the tip and sample and governs the fundamental limits of this technique. The use of a silicon probe for LTA enables bulk fabrication, parallelization for high-throughput analysis, and fabrication of a sharp tip capable of nanoscale spatial resolution.