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).

Hydration film measurement on mica and coal surfaces using atomic force microscopy and interfacial interactions

The hydration film on particle surface plays an important role in bubble-particle adhesion in mineral flotation process. The thicknesses of the hydration films on natural hydrophobic coal and hydrophilic mica surfaces were measured directly by atomic force microscopy （AFM） based on the bending mode of the nominal constant compliance regime in AFM force curve in the present study. Surface and solid-liquid interfacial energies were calculated to explain the forming mechanism of the hydration film and atomic force microscopy data. The results show that there are significant differences in the structure and thickness of hydration films on coal and mica surfaces. Hydration film formed on mica surface with the thickness of 22.5 nm. In contrast, the bend was not detected in the nominal constant compliance regime. The van der Waals and polar interactions between both mica and coal and water molecules are characterized by an attractive effect, while the polar attractive free energy between water and mica （-87.36 mN/m） is significantly larger than that between water and coal （-32.89 mN/m）, which leads to a thicker and firmer hydration layer on the mica surface. The interfacial interaction free energy of the coal/water/bubble is greater than that of mica. The polar attractive force is large enough to overcome the repulsive van der Waals force and the low energy barrier of film rupture, achieving coal particle bubble adhesion with a total interfacial free energy of-56.30 mN/m.

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.

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.

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.

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.

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.

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.

Development of XY scanner with minimized coupling motions for high-speed atomic force microscope

The design and fabrication processes of a novel scanner with minimized coupling motions for a high-speed atomic force microscope （AFM） were addressed. An appropriate design modification was proposed through the analyses of the dynamic characteristics of existing linear motion stages using a dynamic analysis program, Recurdyn. Because the scanning speed of each direction may differ, the linear motion stage for a high-speed scanner was designed to have different resonance frequencies for the modes, with one dominant displacement in the desired directions. This objective was achieved by using one-direction flexure mechanisms for each direction and mounting one stage for fast motion on the other stage for slow motion. This unsymmetrical configuration separated the frequencies of two vibration modes with one dominant displacement in each desired direction, and hence suppressed the coupling between motions in two directions. A pair of actuators was used for each axis to decrease the crosstalk between the two motions and give a sufficient force to actuate the slow motion stage, which carried the fast motion stage, A lossy material, such as grease, was inserted into the flexure hinge to suppress vibration problems that occurred when using an input triangular waveforrn. With these design modifications and the vibration suppression method, a novel scanner with a scanning speed greater than 20 Hz is achieved.

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.

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.

Studying Aggregate in Lysozyme Solution by Atomic Force Microscope

The aggregates in lysozyme solution with different NaCl concentration were investigated by Atomic Force Microscope (AFM). The AFM images show that there exist lysozyme monomers, n-mers and clusters in lysozyme solution when the conditions are not suitable for crystal growth. In favorable conditions for crystal growth, the lysozyme clusters disappear and almost only monomers exist in solution.

Three-dimensional atomic force microscopy based on tailored cantilever probe with flared tip

In order to meet the requirements of nondestructive testing of true 3D topography of micro-nano structures,a novel three-dimensional atomic force microscope(3D-AFM)based on flared tip is developed.A high-precision scanning platform is designed to achieve fast servo through moving probe and sample simultaneously,and several combined nanopositioning stages are used to guarantee linearity and orthogonality of displacement.To eliminate the signal deviation caused by AFM-head movement,a traceable optical lever system is designed for cantilever deformation detection.In addition,a method of tailoring the cantilever of commercial probe with flared tip is proposed to reduce the lateral force applied on the tip in measurement.The tailored probe is mounted on the 3D-AFM,and 3D imaging experiments are conducted on different samples by use of adaptive-angle scanning strategy.The results show the roob-mean-square value of the vertical displacement noise(RMS)of the prototype is less than 0.1 nm and the high/width measurement repeatability(peak-to-peak)is less than 2.5 nm.

Monte Carlo method in optical atomic force microscopy

Scanning probe microscopy(SPM)is a branch of microscopy that forms images of surfaces using a physical probe that scans the specimen.Atomic force microscopy is one of the SPM family which is considered as a very versatile tool for surface imaging and measurements.A wide range of various samples can be measured regardless of being conductive,no-conductive,in vacuum,in air or in a fluid as a unique feature.One of the most challenges in atomic force microscopes(AFMs)is to evaluate the associated uncertainty during the surface measurements by AFMs.Here,an optical AFM is calibrated through the calibration of XYZ stage.The approach is to overcome difficulties experienced when trying to evaluate some uncertainty components which cannot be experimentally determined i.e.tip surface interaction forces and tip geometry.The Monte Carlo method is then used to determine the associated uncertainties due to such factors by randomly drawing the parameters according to their associated tolerances and their probability density functions(PDFs).The whole process follows supplement 2 to“the guide to the expression of the uncertainty in measurement”(GUM).The approach validated in the paper shows that the evaluated uncertainty in AFM is about 10 nm.

Carbon nanotubes as tips for atomic force microscopy

Ordinary AFM probes'characters prevent the AFM' s application in various scopes. Carbon nanotubes represent ideal AFM probe materials for their higher aspect ratio, larger Young's modulus, unique chemical structure, and well-defined electronic property. Carbon nanotube AFM probes are obtained by using a new method of attaching carbon nanotubes to the end of ordinary AFM probes, and are then used for doing AFM experiments. These experiments indicated that carbon nanotube probes have higher elastic deformation, higher resolution and higher durability. And it was also found that carbon nanotube probes ean accurately reflect the morphology of deep narrow gaps, while ordinary probes can not reflect.

In situ observation of surface structures of cardiovascular endothelial cells with atomic force microscope

Objective To observe the surface structures of cardiovascular endothelial cells in situ with atomic force microscope （AFM）. Methods Fresh aorta and aortic valve were dissected from 10 healthy male New Zealand white rabbits. Before fixed in 1% formaldehyde, the fresh tissues were washed in the buffer phosphate solution. Under general microscope, the fixed aorta or valve was spread on the double side stick tape which had already been stuck on the glass slide. The intima of aorta or the aorta side of valve was towards upside, Then the specimen was dried under 37 degrees centigrade in an attemperator and was washed with pure water. After dried again, the specimen was loaded on the platform ofNanoScope Ⅲa AFM and was scanned in tapping mode with the scanning speed of 0.5 HZ. Results The surface structures of endothelial cell on the fixed and dried tissue could be observed clearly in situ with AFM. aortic endothelial cells were large, branched and arranged sparsely and parallel to the direction of blood flow, whereas endothelial cells on aorta valve surface were small, less branched and arranged intensively and vertical to the direction of blood flow. When the scanning range was dwindled, granular ultra-structures could be observed on the surface of endothelial cells, and, as the scanning range was dwindled further, fissure and convolution could be seen on the surface of granules from aortic endothelial cells. Centre cavity and surrounding swelling volcano-like structure could be seen on the surface of granules from endothelial cells of aortic valve. Conclusions It＇s feasible to observe the surface ultra-structures of cardiovascular endothelial cells in situ with AFM and morphological information provided by AFM might be of clinical value in future histopathological diagnosis（JGeriatr Cardiol2009; 6：178-181）.

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.

Diatom-induced impact on shear strength characteristics of finegrained soils

Diatomaceous soils,composed of diatom microfossils with biological origins,have geotechnical properties that are fundamentally different from those of conventional non-diatomaceous fine-grained soils.Despite their high fines content,diatomaceous soils typically exhibit remarkably high shear resistance,approaching that of sandy soils.However,the exact role that diatoms play in controlling the mechanical properties of fine-grained soils and the underlying mechanisms remain unclear.In light of this,the shear strength response of diatomaceous soils was systematically investigated using consolidated undrained triaxial compression tests on diatomekaolin mixtures(DKMs)with various diatom contents and overconsolidation ratios.The micro-and nano-scale structures of the soil samples were characterized in detail using scanning electron microscope(SEM)and atomic force microscope(AFM)to interpret the abnormal shear strength parameters of diatomaceous soils.The results indicated that the presence of diatoms could contribute to significantly higher strength,e.g.the friction angle of DKMs was improved by 72.7%to 37and the value of undrained shear strength tripled with diatom content increasing from 20%to 100%.Such significant improvement in soil strength with diatom inclusion could be attribute to the hard siliceous skeleton of diatoms and the interlocking between particles with rough surfaces,which were quantitatively analyzed by the surface roughness parameters with AFM.Furthermore,a conceptual model established based on the macro-mechanical tests and microscopic observations portrays a microstructural evolution of soils with increasing diatoms.The microstructure of soils was gradually transformed from the matrix-type to the skeletal one,resulting in a continual augmentation in shear strength through mutual interactions between diatom microfossils.This paper provides new insights into the multi-scale structural properties of diatoms and significantly advances our understanding of the mechanical behavior of diatomaceous soils.