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.

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）.

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.

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.

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.

Effects of Environments on the Noise of Atomic Force Microscopy Cantilevers

Thermal vibration of the cantilevers is the main source of noise in atomic force microscopy(AFM).When immersed in liquids,the dynamic behavior of the cantilevers will be significantly affected by the environment.In this study,the effects of environments on the noise of AFM were investigated.The results show that the V⁃shaped cantilever exhibited very low noise in high vacuum.The noise in atmospheric environment was also satisfactory.In liquid environments,the noise dramatically increased.The systematic noise was low and dependent on the distance between the tip and substrate.As the velocity increased,the noise of V⁃shaped cantilever was increased in a similar trend.It is also found that the variation trend was more pronounced as the liquid viscosity increased.The noise of rectangular cantilever was lower than that of V⁃shaped cantilever in the same environment.The present study indicates that high vacuum is an ideal environment for single molecule force spectroscopy(SMFS)due to the lower noise and higher resolution.For a better signal⁃to⁃noise ratio,both the cantilever velocity and liquid viscosity should be as low as possible.These results will be helpful when a lower noise is desired in weak force detection.

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.

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.

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.

Environmental temperature effect on dimensional measurements of atomic force microscopy

Atomic force microscopy(AFM)is increasingly being used as a fundamental tool for dimensional measurements at the nanoscale in the laboratory and in industry.Since the environmental temperature is not controlled in many measurements,or is even varied on purpose,quantification of its effects on AFM dimensional measurements is needed.In this paper,the influences of the temperature in the entire environment of the AFM(excluding only the controller and computer)and that in the local environment around the tip–sample are investigated.The results show that lateral dimensional measurements are affected mainly by the entire environmental temperature.However,vertical measurements are influenced by the temperature of both the entire environment and the local environment.The effects become significant for temperatures higher than some threshold,here between 35 and 40 XC.

Atomic Force Microscopy Measurement in the Lignosulfonate/Inorganic Silica System:From Dispersion Mechanism Study to Product Design

Designing and preparing high-performance lignin-based dispersants are crucial steps in realizing the value-added utilization of lignin on an industrial scale.Such process depends heavily on an understanding of the dispersion mechanism of lignin-based dispersants.Here,atomic force microscopy(AFM)is employed to quantitatively investigate the dispersion mechanism of a lignosulfonate/silica(LS/SiO_(2))system under different pH conditions.The results show that the repulsive force between SiO_(2)particles in LS solution is stronger than it is in water,resulting in better dispersion stability.The Derjaguin–Landau–Verwey–Overbeek(DLVO)formula as well as the DLVO formula combined with steric repulsion is utilized for the fitting of the AFM force/distance(F/D)curves between the SiO_(2)probe and substrate in water and in LS solution.Based on these fitting results,electrostatic and steric repulsive forces are respectively calculated,yielding further evidence that LS provides strong steric repulsion between SiO_(2)particles.Further studies indicate that the adsorbance of LS on SiO_(2)(Q),the normalized interaction constant(A),and the characteristic length(L)are the three critical factors affecting steric repulsion in the LS/SiO_(2)system.Based on the above conclusions,a novel quaternized grafted-sulfonation lignin(QAGSL)dispersant is designed and prepared.The QAGSL dispersant exhibits good dispersing performance for SiO_(2)and real cement particles.This work provides a fundamental and quantitative understanding of the dispersion mechanism in the LS/inorganic particle system and provides important guidance for the development of high-performance lignin-based dispersants.

Adaptive semi-empirical model for non-contact atomic force microscopy

Non-contact atomic force microscope is a powerful tool to investigate the surface topography with atomic resolution.Here we propose a new approach to estimate the interaction between its tips and samples,which combines a semi-empirical model with density functional theory(DFT)calculations.The generated frequency shift images are consistent with the experiment for mapping organic molecules using CuCO,Cu,CuCl,and CuO_(x)tips.This approach achieves accuracy close to DFT calculation with much lower computational cost.

Nanomechanical Characterization of Bone Quality Depending on Tissue Age via Bimodal Atomic Force Microscopy

Characterization of bone quality during the healing process is crucial for successful implantation procedures and patient comfort.In this study,a bone implant specimen that underwent a 4-week healing period was investigated.Bimodal atomic force microscopy(AFM)was employed to simultaneously obtain the morphology and elastic modulus maps of the newly formed and pre-existing bone regions within the sample.Results indicate that the new bone matrix possessed lower miner-alization levels and presented larger,uneven mineral grains,exhibiting the attributes of a woven bone.On the other hand,the old bone matrix exhibited a more uniform and mineralized structure,which is characteristic of lamellar bones.The new bone had a lower overall elastic modulus than the old bone.Bimodal AFM further confrmed that the new bone displayed three regions comprising unmineralized,partially mineralized,and fully matured sections,which indicate a turbulent change in its composition.Meanwhile,the old bone exhibited two sections comprising partially mineralized and matured bone parts,which denote the fnal phase of mineralization.This study provides valuable insights into the morphological and nanome-chanical diferences between the old and new bone matrixes and presents a novel approach to investigate bone quality at diferent phases of the bone-healing process.

Substrate orientation effect in covalent organic frameworks/2D materials heterostructure by high-resolution atomic force microscopy

Heterostructures based on covalent organic frameworks(COFs)and other two-dimensional(2D)materials attract considerable attention due to their extraordinary properties and tremendous application potential.Substrate effects play a crucial role in the integration of ultrathin COF films onto 2D materials through direct polymerization.In this study,highly ordered monolayer COFs were successfully constructed on the surfaces of highly oriented pyrolytic graphite(HOPG),hexagonal boron nitride(hBN),and molybdenum disulfide(MoS_(2)).High-resolution atomic force microscopy(HR-AFM)imaging clearly reveals the substrate orientation effect in COFs/2D materials heterostructure.Honeycomb networks formed via Schiff-base reaction and boronic acid condensation reaction can epitaxially grow in specific orientations relative to the underlying substrate lattices.This work provides direct evidence for substrate effects in the on-surface synthesis of COFs and paves the way for further investigation into the intrinsic electronic properties of monolayer COFs and the development of multifunctional hybrid devices.

Histogram method for reliable thickness measurements of graphene films using atomic force microscopy(AFM)

Atomic force microscopy（AFM） is a commonly used technique for graphene thickness measurement.However, due to surface roughness caused by graphene itself and variation introduced in AFM measurement, graphene thickness is difficult to be accurately determined by AFM. In this paper, a histogram method was used for reliable measurements of graphene thickness using AFM. The influences of various measurement parameters in AFM analysis were investigated. The experimental results indicate that significant deviation can be introduced using various order of flatten and improperly selected measurement parameters including amplitude setpoint and drive amplitude. At amplitude setpoint of 100 mV and drive amplitude of 100 m V, thickness of 1 layer（1L）, 2 layers（2L） and 4 layers（4L） graphene were measured.The height differences for 1L, 2L and 4L were 1.51 ± 0.16 nm, 1.92 ± 0.13 nm and 2.73 ± 0.10 nm, respectively. By comparing these values, thickness of single layer graphene can be accurately determined to be0.41 ± 0.09 nm.

Atomic force microscopy correlates antimetastatic potentials of HepG2 cell line with its redox/energy status: effects of curcumin and Khaya senegalensis

OBJECTIVE： The fatality of cancer is mostly dependent on the possibility of occurrence of metastasis. Thus, if the development of metastasis can be prevented through novel therapeutic strategies targeted against this process, then the success of cancer treatment will drastically increase. In this study, therefore, we evaluated the antimetastatic potentials of an extract of Khaya senegalensis and curcumin on the metastatic liver cell line HepG2, and also assessed the anticancer property of the extract. METHODS： Cells were cultured and treated with graded concentrations of test substances for 24, 48, or 72 h with provisions made for negative controls. Treated cells were assessed as follows： nanotechnologically--atomic force microscopy （AFM） was used to determine cell stiffness; biochemically--cell cytotoxicity, glutathione level and adenosine triphosphate status, caspase activation and mitochondrial toxicity were considered; and microbiologically--a carrot disk assay was used to assess the anticancer property of the extract of K. senegalensis. RESULTS： Curcumin and K. senegalensis increased the cell stiffness by 2.6- and 4.0-fold respectively, indicating their antimetastatic effects. Corresponding changes in redox （glutathione level） and energy （adenosine triphosphate） status of the cells were also demonstrated. Further mechanistic studies indicated that curcumin was not mitotoxic in HepG2 cells unlike the K. senegalensis extract. In addition the extract potently inhibited the Agrobacterium tumefaciens-induced genetic transformation based on carrot disk assay. CONCLUSION： Cell elasticity measurement data, using AFM, strongly suggested, for the first time, that both curcumin and the extract of K. senegalensis exhibited antimetastatic properties on HepG2 cells.

Dynamic friction energy dissipation and enhanced contrast in high frequency bimodal atomic force microscopy

Dynamic friction occurs not only between two contact objects sliding against each other,but also between two relative sliding surfaces several nanometres apart.Many emerging micro-and nano-mechanical systems that promise new applications in sensors or information technology may suffer or benefit from noncontact friction.Herein we demonstrate the distance-dependent friction energy dissipation between the tip and the heterogeneous polymers by the bimodal atomic force microscopy(AFM)method driving the second order flexural and the first order torsional vibration simultaneously.The pull-in problem caused by the attractive force is avoided,and the friction dissipation can be imaged near the surface.The friction dissipation coefficient concept is proposed and three different contact states are determined from phase and energy dissipation curves.Image contrast is enhanced in the intermediate setpoint region.The work offers an effective method for directly detecting the friction dissipation and high resolution images,which overcomes the disadvantages of existing methods such as contact mode AFM or other contact friction and wear measuring instruments.

Atomic and Close-to-Atomic Scale Manufacturing:A Review on Atomic Layer Removal Methods Using Atomic Force Microscopy

Manufacturing at the atomic scale is the next generation of the industrial revolution.Atomic and close-to-atomic scalemanufacturing(ACSM)helps to achieve this.Atomic force microscopy(AFM)is a promising method for this purposesince an instrument to machine at this small scale has not yet been developed.As the need for increasing the number ofelectronic components inside an integrated circuit chip is emerging in the present-day scenario,methods should be adoptedto reduce the size of connections inside the chip.This can be achieved using molecules.However,connecting moleculeswith the electrodes and then to the external world is challenging.Foundations must be laid to make this possible for thefuture.Atomic layer removal,down to one atom,can be employed for this purpose.Presently,theoretical works are beingperformed extensively to study the interactions happening at the molecule-electrode junction,and how electronic transportis affected by the functionality and robustness of the system.These theoretical studies can be verified experimentally only if nano electrodes are fabricated.Silicon is widely used in the semiconductor industry to fabricate electronic components.Likewise,carbon-based materials such as highly oriented pyrolytic graphite,gold,and silicon carbide find applications inthe electronic device manufacturing sector.Hence,ACSM of these materials should be developed intensively.This paperpresents a review on the state-of-the-art research performed on material removal at the atomic scale by electrochemical andmechanical methods of the mentioned materials using AFM and provides a roadmap to achieve effective mass productionof these devices.