Nonlinear control techniques for an atomic force microscope system

Two nonlinear control techniques are proposed for an atomic force microscopesystem. Initially, a learning-based control algorithm is developed for the microcantilever-samplesystem that achieves asymptotic cantilever tip tracking for periodic trajectories. Specifically, thecontrol approach utilizes a learning-based feedforward term to compensate for periodic dynamics andhigh-gain terms to account for non-periodic dynamics. An adaptive control algorithm is thendeveloped to achieve asymptotic cantilever tip tracking for bounded tip trajectories despiteuncertainty throughout the system parameters. Simulation results are provided to illustrate theefficacy and performance of the control strategies.

MICRO/NANO-MACHINING ON SILICON SURFACE WITH A MODIFIED ATOMIC FORCE MICROSCOPE

To understand the deformation and removal mechanism of material on nano-scale at ultralow loads,a systemic study on AFM micro/nano-machining on single crystal ailicon is conducted. The results indicate that AFM nano- machining has a precisely dimensional controllability and a good surface quality on nanometer scale.A SEM is adopted to observe nano-machined region and chips,the results indicate that the material removal mechanisms change with the applied normal load. An XPS is used to analyze the changes of chemical composition inside and outside the nano-machined region respectively.The nano-indentation which is conducted with the same AFM diamond tip on the machined region shows a big discrepancy compared with that on the macro-scale. The calculated results show higher nano-hardness and elastic modulus than normal values .This phenomenon on be regarded as the indentation size effect(ISE).

Surface Electromechanical Coupling on DLC Film with Conductive Atomic Force Microscope

Diamond-like carbon (DLC) film composed of microscopically insulation but microscopically a mixture of conducting (sp2) and insulating (sp3) phases was discussed on the local modification with a conductive atomic force microscope (C-APM). Especially, a topographic change was observed when a direct current (DC) bias-voltage was applied to the DLC film. Experimental results show that a nanoscale pit on DLC surface was formed when applying a positive 25 V on DLC film. According to the interacting force between CoCr-coated microelectronic scanning probe (MESP) tip and DLC surface, as well as the Sondheimer oscillation theory, the 'scalewing effect' of the pit was explained. Electromechanical coupling on DLC film suggested that the depth of pits increased with an increase of load applied to surface when the cantilever-deflected signal was less than a certain threshold voltage.

Edge Effects and Coupling Effects in Atomic Force Microscope Images

The AFM images were obtained by an atomic force microscope (AFM) and transformed from the deformation of AFM micro cantilever probe. However, due to the surface topography and surface forces applied on the AFM tip of sample, the deformation of AFM probe results in obvious edge effects and coupling effects in the AFM images.The deformation of AFM probe was analyzed,the mechanism of the edge effects and the coupling effects was investigated, and their results in the AFM images were studied. It is demonstrated by the theoretical analysis and AFM experiments that the edge effects make lateral force images more clear than the topography images,also make extraction of frictional force from lateral force images more complex and difficult. While the coupling effects make the comparison between topography images and lateral force images more advantage to acquire precise topography information by AFM.

Sorting Gold and Sand(Silica) Using Atomic Force Microscope-Based Dielectrophoresis

Additive manufacturing-also known as 3D printing-has attracted much attention in recent years as a powerful method for the simple and versatile fabrication of complicated three-dimensional structures.However,the current technology still exhibits a limitation in realizing the selective deposition and sorting of various materials contained in the same reservoir,which can contribute significantly to additive printing or manufacturing by enabling simultaneous sorting and deposition of different substances through a single nozzle.Here,we propose a dielectrophoresis(DEP)-based material-selective deposition and sorting technique using a pipette-based quartz tuning fork(QTF)-atomic force microscope(AFM) platform DEPQA and demonstrate multi-material sorting through a single nozzle in ambient conditions.We used Au and silica nanoparticles for sorting and obtained 95% accuracy for spatial separation,which confirmed the surfaceenhanced Raman spectroscopy(SERS).To validate the scheme,we also performed a simulation for the system and found qualitative agreement with the experimental results.The method that combines DEP,pipette-based AFM,and SERS may widely expand the unique capabilities of 3D printing and nano-micro patterning for multi-material patterning,materials sorting,and diverse advanced applications.

Competitive Adsorption between Bovine Serum Albumin and Collagen Observed by Atomic Force Microscope

Atomic force microscopy (AFM) was used to study the competitive adsorption betweenbovine serum albumin (BSA) and type Ⅰ collagen on hydrophilic and hydrophobic silicon wafers.BSA showed a grain shape and the type Ⅰ collagen displayed fibril-like molecules with relativelyhomogeneous height and width, characterized with clear twisting (helical formation). These AFMimages illustrated that quite a lot of type Ⅰ collagen appeared in the adsorption layer on hydrophilicsurface in a competitive adsorption state, but the adsorption of BSA was more preponderant than thatof type Ⅰ collagen on hydrophobic silicon wafer surface. The experiments showed that theinfluence of BSA on type Ⅰ collagen adsorption on hydrophilic surface was less than that onhydrophobic surface.

Preparation of La-Ti Composite Oxide Nanocrystal and Examination of Their Surface Topography with Atomic Force Microscope

With sol-gel method, nanometer La-Ti composite oxide was successfully prepared at a low temperature (750～800C) using polyethylene glycol as dispersant. By means of atomic force microscope, the surface pattern, particle size distribution, and specific surface area were studied. The compound particle surface appears as a smooth sheet, the mean size of the compound is 25.38 nm. On the specific surface, the particle erects at a height of 4.69 nm. The surface area is 58.90 nm2. The La-Ti composite oxide nanocrystal prefers to narrow and even particle size distribution and the homogeneity of surface topography.

A Study on HA Titanium Surface with Atomic Force Microscope (AFM)

Three kinds of titanium surface especially the HA surface are analyzed. Titanium was treated by 3 kinds of methods that were acid ＆ alkali, calcic solution and apathe solution. Samples were observed by optic microscope and atomic force microscope （ AFM ） . The typical surface morphology of the acid and alkali group is little holes, and on the two HA surface the tiny protuberances is typical. The surface treated by apatite solution was smoother than the two formers. The rough surface treated with acid and alkali was propitious to Ca^＋ , P^- and proteins＇ adhesion, and the relatively smooth HA surface was of benefit to the cell adhesion.

Dissipation Energy in Tapping-Mode Atomic Force Microscopes Caused by Liquid Bridge

The dissipation of energy during the process of contact and separation between a tip and a sample is very important for understanding the phase images in the tapping mode of atomic force microscopes（AFMs）. In this study, a method is presented to measure the dissipated energy between a tip and a sample. The experimental results are found to be in good agreement with the theoretical model, which indicates that the method is reliable.Also, this study confirms that liquid bridges are mainly produced by extrusion modes in the tapping mode of AFMs.

Fabrication of Nanoscale Active Plasmonic Elements Using Atomic Force Microscope Tip-Based Nanomachining

Atomic force microscopy(AFM)is a widely adopted imaging and surface analysis technique that provides resolutions on the nanometer scale.AFM tip-based nanomachining has recently been adopted for the fabrication of arbitrarily shaped nanoscale structures.A major challenge of using AFM tip-based machining for the sculpting of nanoscale plasmonic structures is the build-up of displaced material along the sides of the channels.Here we apply this nanomechanical machining method to create active plasmonic elements and present the strategy we have been using to avoid the formation of such debris.Furthermore,a number of post-manufacturing treatments that can potentially be used to reduce the amount of debris surrounding the fabricated structures are discussed.

Visualization of Cellulose Microfibrils of Phyllostachys pubescens Fibers with Atomic Force Microscope

Atomic force microscope(AFM) was used to investigate the arrangement of cellulose microfibrils (CMF) in Moso bamboo (Phyllostachys pubescens) fibers. Two methods of sample preparation were used here for different purposes. The first method was chemical maceration with a mixture of hydrogen peroxide and glacial acetic acid, through which the obtained fibers were suitable for observing the orientation of CMF in the primary wal1. The other method was to prepare tangential microtomed sections with a thickness of approximately 30 μm, which was used to investigate the arrangement of CMF in the inner wall of cell cavity of bamboo fibers. The results indicated that the CMF are randomly oriented in the primary wall while in the inner wall of cell cavity they are nearly vertical to the long axis of fibers , which is similar to the arrangement of CMF in the corresponding layer of wood fibers. Meanwhile, the highly oriented arrangement of CMF is also observed in a certain layer of bamboo fibers, though it is incapable of determining which layer it is in this study. The pilot investigation demonstrates that AFM is a powerful tool for the high-resolution observation of CMF in bamboo fibers, meanwhile it has the advantages of simple procedure of sample preparation and easy operation compared to the traditional transmission electron microscopy.

Application of Atomic Force Microscopy in the Study of Polysaccharide

This paper gives a brief introduction to basic principle and working mode of atomic force microscope （AFM）. Sample preparation methods and factors that affect the AFM imaging of polysaccharide are described in detail. Advance in using AFM for morphological observation and quantitative study on polysaccharide molecules are reviewed. Research on single molecule force spectroscopy of polysaccharide and determination and adjustment of conformational change of sugar residue are introduced. Perspective on further application of AFM in polysaccharide investigation is presented.

IMPROVED FABRICATION METHOD FOR CARBON NANOTUBE PROBE OF ATOMIC FORCE MICROSCOPY(AFM)

An improved arc discharge method is developed to fabricate carbon nanotube probe of atomic force microscopy （AFM） here. First, silicon probe and carbon nanotube are manipulated under an optical microscope by two high precision microtranslators. When silicon probe and carbon nanotube are very close, several tens voltage is applied between them. And carbon nanotube is divided and attached to the end of silicon probe, which mainly due to the arc welding function. Comparing with the arc discharge method before, the new method here needs no coat silicon probe with metal film in advance, which can greatly reduce the fabrication＇s difficulty. The fabricated carbon nanotube probe shows good property of higher aspect ratio and can more accurately reflect the true topography of silicon grating than silicon probe. Under the same image drive force, carbon nanotube probe had less indentation depth on soft triblock copolymer sample than silicon probe. This showed that carbon nanotube probe has lower spring constant and less damage to the scan sample than silicon probe.

THEORETICAL ANALYSIS AND EXPERIMENTAL STUDY OF CARBON NANOTUBE PROBE AND CONVENTIONAL ATOMIC FORCE MICROSCOPY PROBE ON SURFACE ROUGHNESS

In this paper, three different tips are employed, i.e., the carbon nanotube tip, monocrystalline silicon tip and silicon nitride tip. Resorting to atomic force microscope （AFM）, they are used for measuring the surface roughness of indium tin oxide （ITO） film and the immunoglobulin G （IgG） proteins within the scanning area of 10 μm×10 μm and 0.5 μm×0.5 μm, respectively. Subsequently, the scanned surface of the ITO film and IgG proteins are analyzed by using fractal dimension. The results show that the ffactal dimension measured by carbon nanotube tip is biggest with the highest frequency components and the most microscopic information. Therefore, the carbon nanotube tip is the ideal measuring tool for measuring super-smooth surface, which will play a more and more important role in the high-resolution imaging field.

Evaluating Local Elasticity of the Metal Nano-films Quantitatively Based on Referencing Approach of Atomic Force Acoustic Microscopy

Traditional technique such nanoindenter（NI） can＇t measure the local elastic modulus at nano-scale（lateral）. Atomic force acoustic microscopy （AFAM） is a dynamic method, which can quantitatively determine indentation modulus by measuring the contact resonance spectra for high order modes of the cantilever. But there are few reports on the effect of experimental factors, such length of cantilever, contact stiffness on measured value. For three different samples, including copper（Cu） film with 110 nm thickness, zinc（Zn） film of 90 nm thickness and glass slides, are prepared and tested, using referencing approach in which measurements are performed on the test and reference samples （it＇s elastic modulus is known）, and their contact resonance spectra are measured used the AFAM system experimentally. According to the vibration theory, from the lowest two contact resonance frequencies, the tip-sample contact stiffness is calculated, and then the values for the elastic properties of test sample, such as the indentation modulus, are determined. Using AFAM system, the measured indentation modulus of copper nano-film, zinc nano-film and glass slides are 113.53 GPa, 87.92 GPa and 57.04 GPa, which are agreement with literature values Mcu--105-130 GPa, Mzn = 88.44 GPa and Molass = 50-90 GPa. Furthermore, the sensitivity of contact resonance frequency to contact stiffness is analyzed theoretically. The results show that for the cantilevers with the length 160 pm, 225 μm and 520 μm respectively, when contact stiffness increases from 400 N/m to 600 N/m, the increments of first contact resonance frequency are 126 kHz, 93 kHz and 0.6 kHz, which show that the sensitivity of the contact resonance frequency to the contact stiffness reduces with the length of cantilever increasing. The novel method presented can characterize elastic modulus of near surface for nano-film and bulk material, and local elasticity of near surface can be evaluated by optimizing the experimental parameters using the AFAM system.

Compensation of Parasitic Capacitance of Quartz Tuning Fork in AFM

We have built an atomic force microscope using a quartz tuning fork as sensor. The excitation method we adopted, the electrical excitation, introduces stray capacitance into the signal-processing circuit. In this report, we demonstrated a simple but effective method to compensate for this parasitic capacitance by adding a compensator circuit consisting of an inverting amplifier and a capacitor. The capacitor is connected in series with the inverting amplifier and the compensator is connected in parallel with the quartz tuning fork. The resonance curve of the system measured after adding the homemade compensator resembles that of a pure RLC circuit, meaning that the stray capacitance is successfully eliminated. Furthermore, we tried to use our equipment to measure PDMS sample and got clean data. This system can be further combined with confocal microscope and diamond with NV defect to build scanning NV magnetometry.

Effects of Astragalus Polysaccharide on Mechanical Characterization of Liver Sinusoidal Endothelial Cells by Atomic Force Microscopy at Nanoscale

Objective： To study the effects of Astragalus polysaccharide （APS）, the primary effective component of the Chinese herb medicine Astragalus membranaceus （frequently used for its anti-hepatic fibrosis effects）, on nanoscale mechanical properties of liver sinusoidal endothelial cells （SECs）. Methods： Using endothelial cell medium as the control, 5 experimental groups were established utilizing different concentrations of APS, i.e. 12.5, 25, 50, 100, and 200μg/mL. By using atomic force microscopy along with a microcantilever modified with a silicon dioxide microsphere as powerful tools, the value of Young＇s modulus in each group was calculated. SAS 9.1 software was applied to analyze the values of Young＇s modulus at the pressed depth of 300 nm. Environmental scanning electron microscopy was performed to observe the surface microtopography of the SECs. Results： The value of Young＇s modulus in each APS experimental group was significantly greater than that of the control group： as APS concentration increased, the value of Young＇s modulus presented as an increasing trend. The difference between the low-concentration （12.5 and 25 μg/mL） and high-concentration （200μg/mL） groups was statistically significant （P〈0.05）, but no significant differences were observed between moderate-concentration （50 and 100μg/mL） groups versus low- or high-concentration groups （P〉0.05）. Surface topography demonstrated that APS was capable of increasing the total area of fenestrae. Conclusions： The values of Young＇s modulus increased along with increasing concentrations of APS, suggesting that the stiffness of SECs increases gradually as a function of APS concentration. The observed changes in SEC mechanical properties may provide a new avenue for mechanistic rasearch of anti-hepatic fibrosis treatments in Chinese medicine.

The Effects of Low-Energy Nitrogen Ion Implantation on Pollen Exine Substructure and Pollen Germination of Cedrus deodara

The aim of this study is to investigate the biological effects of ion beams on pollen. Pollen grains of Cedrus deodara were implanted with 30 keV nitrogen ion beams at doses ranging from 1 × 10^15 ions/cm^2 to 15 × 10^15 ions/cm^2. The effects of N^＋ implantation on the pollen exine substructure were examined using an atomic force microscope （AFM）, and the structure and morphology of pollen and pollen tubes were observed using a laser scanning confocal microscope （LSCM）. AFM observations distinctly revealed the erosion of the pollen exine caused by N^＋ implantation in the micrometer to nanometer range. Typical results showed that the erosion degree was linearly proportional to the ion dose. Pollen germination experiments in vitro indicated that N^＋ implantation within a certain dose range increased the rate of pollen germination. The main abnormal phenomena in pollen tubes were also analyzed. Our results suggest that low energy ion implantation with suitable energy and dosage can be used to break the pollen wall to induce a transfer of exogenous DNA into the pollen without any damage to the cytoplasm and nuclei of the pollen. The present study suggests that a combination of the method of ion-beam-induced gene transfer and the pollen-tube pathway method （PTPW） would be a new plant transformation method.

Single-molecule biotechnology for protein researches

Cells employ proteins to perform metabolic functions and maintain active physiological state through charge transfer and energy conversion.These processes are carried out in a narrow space precisely and rapidly,which,no doubt,bring great difficulty for their detection and dissection.Fortunately,in recent years,the development and expansion of single-molecule technique in protein research make monitoring the dynamical changes of protein at single-molecule level a reality,which also provides a powerful tool for the further exploration of new phenomena and new mechanisms of life activities.This paper aims to summarize the working principle and essential achievements of single-molecule technique in protein research in recent five years.We focus on not only dissecting the difference of nanopores,atomic force microscope,scanning tunneling microscope,and optical tweezers technique,but also discussing the great significance of these single-molecule techniques in investigating intramolecular and intermolecular interactions,electron transport,and conformational changes.Finally,the opportunities and challenges of the single-molecule technique in protein research are discussed,which provide a new door for single-molecule protein research.