Microstructure Morphologies of Asphalt Binders using Atomic Force Microscopy

We investigated microstructure morphologies of three asphalts（SK, Karamay, and Esso） used in China using atomic force microscopy（AFM）. The topography and phase contrast images were obtained. Topographic profile and three dimensional images were described. Roughnesses of microstructure were calculated. And the chemical compositions of asphalt were tested to explain the microstructural mechanism of the asphalt. The results show that the topography and phase image in atomic force microscopy are appropriate to evaluate the microstructure of the asphalt binder. There are significant differences in microstructural morphologies including bee-like structure, topographic profile, 3D image, and roughness for three asphalts in this study. There are three different phases in microstructure of asphalt binder. The oil source and chemical composition of asphalt, especially asphaltenes content have a great influence on the microstructure.

Theory of higher harmonics imaging in tapping-mode atomic force microscopy

The periodic impact force induced by tip-sample contact in a tapping mode atomic force microscope （AFM） gives rise to the non-harmonic response of a micro-cantilever. These non-harmonic signals contain the full characteristics of tip-sample interaction. A complete theoretical model describing the dynamical behaviour of tip-sample system was developed in this paper. An analytic formula was introduced to describe the relationship between time-varying tip-sample impact force and tip motion. The theoretical analysis and numerical results both show that the timevarying tip-sample impact force can be reconstructed by recording tip motion. This allows for the reconstruction of the characteristics of the tip-sample force, like contact time and maximum contact force. It can also explain the ability of AFM higher harmonics imaging in mapping stiffness and surface energy variations.

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.

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.

Improvement of the high-k/Ge interface thermal stability using an in-situ ozone treatment characterized by conductive atomic force microscopy

In this work, an in-situ ozone treatment is carried out to improve the interface thermal stability of HfO_2/Al_2O_3 gate stack on germanium（Ge） substrate. The micrometer scale level of HfO_2/Al_2O_3 gate stack on Ge is studied using conductive atomic force microscopy（AFM） with a conductive tip. The initial results indicate that comparing with a non insitu ozone treated sample, the interface thermal stability of the sample with an in-situ ozone treatment can be substantially improved after annealing. As a result, void-free surface, low conductive spots, low leakage current density, and relative high breakdown voltage high-κ/Ge are obtained. A detailed analysis is performed to confirm the origins of the changes.All results indicate that in-situ ozone treatment is a promising method to improve the interface properties of Ge-based three-dimensional（3D） devices in future technology nodes.

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.

Antiproliferative effects of cinobufacini on human hepatocellular carcinoma HepG2 cells detected by atomic force microscopy

AIM:To investigate the antiproliferative activity of cinobufacini on human hepatocellular carcinoma HepG2 cells and the possible mechanism of its action.METHODS:HepG2 cells were treated with different concentrations of cinobufacini.Cell viability was measured by methylthiazolyl tetrazolium(MTT) assay.Cell cycledistribution was analyzed by flow cytometry(FCM).Cytoskeletal and nuclear alterations were observed by fluorescein isothiocyanate-phalloidin and DAPI staining under a laser scanning confocal microscope.Changes in morphology and ultrastructure of cells were detected by atomic force microscopy(AFM) at the nanoscale level.RESULTS:MTT assay indicated that cinobufacini significantly inhibited the viability of HepG2 cells in a dosedependent manner.With the concentration of cinobufacini increasing from 0 to 0.10 mg/m L,the cell viability decreased from 74.9% ± 2.7% to 49.41% ± 2.2% and 39.24% ± 2.1%(P < 0.05).FCM analysis demonstrated cell cycle arrest at S phase induced by cinobufacini.The immunofluorescence studies of cytoskeletal and nuclear morphology showed that after cinobufacini treatment,the regular reorganization of actin filaments in HepG2 cells become chaotic,while the nuclei were not damaged seriously.Additionally,high-resolution AFM imaging revealed that cell morphology and ultrastructure changed a lot after treatment with cinobufacini.It appeared as significant shrinkage and deep pores in the cell membrane,with larger particles and a rougher cell surface.CONCLUSION:Cinobufacini inhibits the viability of HepG2 cells via cytoskeletal destruction and cell membrane toxicity.

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).

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.

AN ATOMIC FORCE MICROSCOPY STUDY ON THE AGGREGATION OF ISOTACTIC POLY(METHYL METHACRYLATE)

Aggregation process of isotactic poly（methyl methacrylate） （i-PMMA） has been studied extensively for many years, and considerable progress has been made in both experimental and theoretical studies. They are, however, seldom sustained by real-space observations of the underlying morphology. In this paper, the aggregation process of i-PMMA in concentrated acetone solutions and the fractal structure of the resulting three-dimensional clusters were characterized on the basis of real-space AFM observations of their two-dimensional projection. It was found that spherical multiple-chain particles formed upon collapse and aggregation of the involving chains as a whole during quenching the solution to room temperature. By keeping the solution at room temperature, the initially formed particles stick together upon contact to form larger particles through reassembling very slowly. The succeeding collision of the enlarged spherical particles leads to the formation of small clusters. These newly formed small clusters grow when they meet with other clusters or single Brownian particles. This leads to the formation of large clusters with fractal dimension of 1.95 ± 0.05, which suggest a reaction-limited cluster aggregation of i-PMMA in a concentrated acetone solution. This is in accordance with the conclusion obtained by light scattering measurements.

Quantitative measurement of local elasticity of SiO_x film by atomic force acoustic microscopy

In this paper the elastic properties of SiOx film are investigated quantitatively for local fixed point and qualitatively for overall area by atomic force acoustic microscopy （AFAM） in which the sample is vibrated at the ultrasonic frequency while the sample surface is touched and scanned with the tip contacting the sample respectively for fixed point and continuous measurements. The SiOx films on the silicon wafers are prepared by the plasma enhanced chemical vapour deposition （PECVD）, The local contact stiffness of the tip-SiOx film is calculated from the contact resonance spectrum measured with the atomic force acoustic microscopy. Using the reference approach, indentation modulus of SiOx film for fixed point is obtained. The images of cantilever amplitude are also visualized and analysed when the SiOx surface is excited at a fixed frequency. The results show that the acoustic amplitude images can reflect the elastic properties of the sample.

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.

Analysis of the injection layer of PTCDA in OLEDs using x-ray photoemission spectroscopy and atomic force microscopy

Through the investigation of the sample surface and interface of 3, 4, 9, 10-perylenetetracarboxylic dianhydride （PTCDA）/indium-tin-oxide （ITO） thin films using atomic force microscopy, it has been found that the surface is complanate, the growth is uniform and the defects cover basically the surface of ITO. Furthermore, the number of pinholes is small. The analysis of the sample surface and interface further verifies this result by using x-ray photoemission spectroscopy. At the same time, PTCDA is found to have the ability of restraining the diffusion of chemical constituents from ITO to the hole transport layer, which is beneficial to the improvement of the performance and the useful lifetime of the organic light emitting diodes （OLEDs）.

Characterizing silicon intercalated graphene grown epitaxially on Ir films by atomic force microscopy

An efficient method based on atomic force microscopy（AFM） has been developed to characterize silicon intercalated graphene grown on single crystalline Ir（111） thin films. By combining analyses of the phase image, force curves,and friction–force mapping, acquired by AFM, the locations and coverages of graphene and silicon oxide can be well distinguished. We can also demonstrate that silicon atoms have been successfully intercalated between graphene and the substrate. Our method gives an efficient and simple way to characterize graphene samples with interacted atoms and is very helpful for future applications of graphene-based devices in the modern microelectronic industry, where AFM is already widely used.

Effect of Rho-kinase pathway on neurite outgrowth of rat hippocampal neurons under atomic force microscopy

Hippocampal neurons of neonatal rats were cultured in serum-free culture medium for 5 days in vitro, and treated with the Rho-kinase inducer lysophosphatidic acid. Atomic force microscopy revealed that the numbers of level-1, -2 and -3 neurites protruding from rat hippocampal neurons was significantly reduced. After treatment with the Rho kinase inhibitor Y27632, a significant increase in the numbers of these neurites was observed. Our experimental findings indicate that the Rho-kinase pathway is closely associated with the neurites of hippocampal neurons.

Investigation of Adsorption of Xanthan Gum on Enamel by Tapping Mode Atomic Force Microscopy

By using tapping mode atomic force microscopy(TMAFM), a polymer layer was found on the enamel surface after the exposure to xanthan gum solutions. The layer thickness is closely related to the exposure time and the concentration of xanthan gum solution. The thickness data were evaluated by a Kruskal-Wallis test and Box-Whisker Plot at a 95% confidence level(p<0.05), and a statistically significant difference among the thickness data groups was demonstrated. After the exposure to 1000, 400, 100 mg/L xanthan gum solutions, the mean of layer thickness at the adsorption equilibrium is in the ranges of 103.5_122.06, 82.4_88.94 and 45.27_55.55 nm, respectively. This phenomenon suggests that the viscosity modifying agents in the beverage might be adsorbed on the enamel surface during consumption, which may form a barrier that can protect the enamel from being attacked by acid and therefore reduce dental erosion.

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.

Effects of caveolin-1 on bone marrow mesenchymal stem cells differentiating into neuron-like cells An atomic force microscopy observation

Bone marrow mesenchymal stem cells （MSCs） from rats were transfected with Rn-siRNA-caveolin-1 and differentiated into neuron-like cells using fasudil hydrochloride. Membrane ultrastructural changes in MSCs were observed under atomic force microscopy. Caveolin-l-transfected rat MSCs exhibited weak nuclear refraction, dense caveolae and long finger-like cellular processes prior to fasudil hydrochloride treatment. MSCs differentiating into neuron-like cells exhibited weak nuclear refraction and large cellular processes without caveolae. We hypothesize that caveolin-1 plays an important role in the regulation of bone marrow MSC differentiating into neuron-like cells.