Effect of lateral morphology formation of polymer blend towards patterning silane-based SAMs using selective dissolution method

A number of strategies have been developed including soft lithography and photolithography for patterning various surfaces. Here we have discussed a customized strategy for surface patterning of nanosized, silane-based SAMs and monolayer thickness measurement investigated using atomic force microscope (AFM). We have utilized the versatile morphology of a binary polymer blend to generate patterned SAMs over silicon substrate by employing a selective dissolution procedure. This method was confirmed with different organosilanes with varying number of C-atoms and to other polymer blend. The samples were imaged both in tapping mode and pulsed force mode AFM.     

基于能量比模型的不相容聚合物共混体系相态研究

指出了目前不相容聚合物共混体系相态反转数学模型的不足 ,提出了能量比模型的概念 ,认为这是研究不相容聚合物共混体系相态有效的方法。初步建立了共混体系能耗速率的计算公式并对其进行了理论研究与分析 ,结果表明振动力场对控制不相容聚合物共混体系的相态具有积极作用。     

High resolution surface morphology measurements using EBSD cross-correlation techniques and AFM

The surface morphology surrounding wedge indentations in (0 0 1) Si has been measured using electron backscattered diffraction (EBSD) and atomic force microscopy (AFM). EBSD measurement of the lattice displacement field relative to a strain-free reference location allowed the surface uplift to be measured by summation of lattice rotations about the indentation axis. AFM was used in intermittent contact mode to determine surface morphology. The height profiles across the indentations for the two techniques agreed within 1 nm. Elastic uplift theory is used to model the data.     

Investigation of the friction and wear behaviors of polyoxymethylene/linear low-density polyethylene/ethylene-acrylic-acid blends

The friction and wear behavior of polyoxymethylene/linear low-density polyethylene/ethylene-acrylic acid (POM/LLDPE/EAA) blends is explored using an MM-200 wear tester. The results show that the friction and wear properties of POM were greatly improved after an amount of LLDPE and EAA was added. The friction coefficient and wear scar width of POM are much higher than those of POM/LLDPE/EAA blends under the same condition. The SEM analyses show that POM and POM/LLDPE/EAA blends exhibit totally different wear mechanisms. The wear mechanism of POM is dominated by adhesive. The transfer film of POM is formed on the surface of the steel counterpart. For POM/LLDPE/EAA blend, the lamellar debris is found on the steel ring surface sliding against POM/LLDPE/EAA blend, which helps to decrease the friction coefficient and wear scar width. The lubricate layer formed in the contact surface prevents the bulk from serious wear. Therefore the friction coefficient of POM/LLDPE/EAA blend thus reduced remarkably and anti-wear property got greatly improved.     

Variable-force tapping atomic force microscopy as a tool in the characterization of organic devices

A common method for characterizing the phase separation of materials in mixtures is tapping mode atomic force microscopy (AFM). However, AFM results are influenced by surface-energy effects and the employed tapping force, and it might therefore be difficult to attain correct information regarding the bulk with such a surface-imaging technique. In this work, we present a way of imaging material phase separation in an improved manner by recording a series of AFM images at different tapping force. More specifically, we have employed the variable-force AFM method on organic mixtures, comprising a conjugated polymer (MEH-PPV) and an ion-conducting polymer electrolyte (PEO-XCF(3)SO(3), X=Li, K, Rb), and we demonstrate that it is capable of reversibly sampling such materials not only on the surface, but also (indirectly) in the topmost part of the bulk. The analysis of the evolution of AFM phase images allows us to (indirectly) gain information about the bulk-phase separation of materials. We find that the variable-force AFM results correlate well with the device performance of light-emitting electrochemical cells employing such organic mixtures as the active material.     

Immobilization method of yeast cells for intermittent contact mode imaging using the atomic force microscope

The atomic force microscope (AFM) is widely used for studying the surface morphology and growth of live cells. There are relatively fewer reports on the AFM imaging of yeast cells [1] (Kasas and Ikai, 1995), [2] (Gad and Ikai, 1995). Yeasts have thick and mechanically strong cell walls and are therefore difficult to attach to a solid substrate. In this report, a new immobilization technique for the height mode imaging of living yeast cells in solid media using AFM is presented. The proposed technique allows the cell surface to be almost completely exposed to the environment and studied using AFM. Apart from the new immobilization protocol, for the first time, height mode imaging of live yeast cell surface in intermittent contact mode is presented in this report. Stable and reproducible imaging over a 10-h time span is observed. A significant improvement in operational stability will facilitate the investigation of growth patterns and surface patterns of yeast cells.     

人脐静脉内皮细胞形貌与表面粘附力的原子力显微镜表征

目的:探讨原子力显微镜(AFM)在研究人脐静脉内皮细胞(ECV304)表面形貌、超微结构及纳米机械性质等方面的应用,讨论ECV304超微结构和机械性质与其功能的关系。方法:利用AFM对ECV304细胞的表面形貌及生物机械性质进行表征与测量。结果:在AFM下观察到用普通光学显微镜难以观察到的ECV304细胞的独特的形态结构,如细胞骨架、伪足及细胞边缘微丝等。ECV304细胞呈现长梭形、多角形、圆形等多种形态,细胞表面平均粗糙度为320.52±75.98 nm,表面均匀分布微绒毛,细胞周围有铺展的圆盘状物质。力曲线定量分析得出针尖与细胞表面的非特异性粘附力为75±14 pN。结论:通过AFM成像和力曲线测量表明,ECV304细胞呈圆形,多角形,梭形等多种形态,针尖与细胞膜表面问的粘附力比较小,约75±14pN。     

Topographic characterization of unworn contact lenses assessed by atomic force microscopy and wavelet transform

This paper analyses the three‐dimensional (3‐D) surface morphology of optic surface of unworn contact lenses (CLs) using atomic force microscopy (AFM) and wavelet transform. Refractive powers of all lens samples were 2.50 diopters. Topographic images were acquired in contact mode in air‐conditioned medium (35% RH, 23°C). Topographic measurements were taken over a 5 µm × 5 µm area with 512 pixel resolution. Resonance frequency of the tip was 65 kHz. The 3‐D surface morphology of CL unworn samples revealed (3‐D) micro‐textured surfaces that can be analyzed using (AFM) and wavelet transform. AFM and wavelet transform are accurate and sensitive tools that may assist CL manufacturers in developing CLs with optimal surface characteristics. Microsc. Res. Tech. 78:1026–1031, 2015. © 2015 Wiley Periodicals, Inc.     

多模态动态原子力显微镜系统

动态原子力显微镜(atomic force microscope,AFM)是通过检测悬臂谐振状态的变化来对物体表面形貌进行测量的。通过对谐振状态的三种因素即振幅、相位、频率的检测,动态AFM可以分为三种工作模式,即振幅反馈、相位反馈与频率反馈模式,这三种反馈模式有着不同的扫描特点。基于硅悬臂具有高阶谐振的特性,动态原子力显微镜可以在悬臂工作于高阶谐振状态时对物体进行扫描。综合上述工作模式研制了一套多模态动态AFM,可以在三种反馈模式、不同阶谐振状态下对物体进行扫描测量。利用该系统在不同反馈模式、不同阶谐振状态下进行了扫描测试,结果显示,系统在各模式下具有亚纳米分辨力,其中在相位反馈模式,悬臂二阶谐振时可达到最优灵敏度与分辨力,分别为17.5V/μm和0.29nm,在最优灵敏度与分辨力状态下对光栅试样进行了三维扫描,得到光栅的三维形貌图。     

Phase behaviour and separation kinetics of polymer blends

The liquid–liquid phase separation kinetics and phase behaviour of hydrogenated polyethylene and deuterated polypropylene blends have been systematically studied by optical microscope. Phase diagram was constructed from the phase transition temperature. The hydrogenated polyethylene/deuterated polypropylene blend exhibits upper critical solution temperature in the melt. The time evolution of the characteristics morphology for liquid–liquid phase separation is determined for the hydrogenated polyethylene/deuterated polypropylene blend at various compositions and following a quench from initial homogenous melts at higher temperature to various lower temperatures. Liquid–liquid phase separation kinetics follows nucleation and growth mechanism. The experimental results from optical microscope measurement at various conditions are all consistent with the nucleation and growth mechanism.     

Phase imaging with intermodulation atomic force microscopy

Intermodulation atomic force microscopy (IMAFM) is a dynamic mode of atomic force microscopy (AFM) with two-tone excitation. The oscillating AFM cantilever in close proximity to a surface experiences the nonlinear tip-sample force which mixes the drive tones and generates new frequency components in the cantilever response known as intermodulation products (IMPs). We present a procedure for extracting the phase at each IMP and demonstrate phase images made by recording this phase while scanning. Amplitude and phase images at intermodulation frequencies exhibit enhanced topographic and material contrast.     

AFM studies of environmental effects on nanomechanical properties and cellular structure of human hair

Characterization of cellular structure and physical and mechanical properties of hair are essential to develop better cosmetic products and advance biological and cosmetic science. Although the morphology of the cellular structure of human hair has been traditionally investigated using scanning electron microscopy and transmission electron microscopy, these techniques provide limited capability to in situ study of the physical and mechanical properties of human hair in various environments. Atomic force microscopy (AFM) overcomes these problems and can be used for characterization in ambient conditions without requiring specific sample preparations and surface treatment. In this study, film thickness, adhesive forces and effective Young's modulus of various hair surfaces were measured at different environments (humidity and temperature) using force calibration plot technique with an AFM. Torsional resonance mode phase contrast images were also taken in order to characterize the morphology and cellular structure changes of human hair at different humidity. The correlation between the nanomechanical properties and the cellular structure of hair is discussed.     

Study of silane-based antiwear additives: Wear and chemistry

The chemistry and wear performance of a silane-containing additive in combination with conventional commercial engine oil additives such as zinc dialkyldithiophosphate (ZDDP), calcium-type detergent (Ca detergent), and B- and N-containing dispersant were investigated. The tribological behavior of the low-sulfur base stock 100 N blended with the above additives was investigated using a pin-on-disc Plint friction and wear tester at 100 °C. The wear scar width (WSW) of the upper steel pins was determined using an optical microscope. X-ray absorption near-edge structure (XANES) spectroscopy and X-ray photoelectron spectroscopy (XPS) were used to analyze the chemistry and thickness of the thin tribofilm formed on the disc. The morphologies of the wear scars on the lower steel discs were observed using an atomic force microscope (AFM). It was found when the silane additive is mixed with Ca detergent and B- and N-containing dispersant, the antiwear performance of the blend was greatly improved, while the friction coefficient remained almost unchanged. Indeed, the wear performance was comparable to or better than ZDDP on its own, and much better than a commercial oil blend. The silane additive is converted to hydrous SiO₂ by the water in the oil, and this SiO₂ then interacted chemically with the surface and Ca in the detergent under sliding to form a relatively thick tribofilm containing mainly a Ca silicate species. The incorporation of Si and B had little effect on the tribochemistry of ZDDP in the oil blends. When ZDDP and B- and N-containing dispersants were mixed with the silane additive, polyphosphate-type tribofilms, similar to that of ZDDP alone, were formed. However, addition of ZDDP had adverse effects on the wear performance of the silane-based blend.     

Advances in phase‐sensitive acoustic microscopy studies of polymer blend films: annealing effects and micro‐elastic characterization of PS/PMMA blends

The unique phase‐sensitive acoustic microscope is used for the structural and mechanical characterization of thin films of polystyrene/polymethylmethacrylate blends. The effect of annealing on blends of polystyrene/polymethylmethacrylate spin coated from different solvents unto a substrate is studied. Varying the solvents according to vapour pressure and spin coating at different speeds (for thickness variation) led to changes in phase domain distributions and overall structural properties before annealing. Annealing in vacuum at 190°C for 48 h resulted in the elimination of solvent effects with all samples reverting to a similar morphology irrespective of common solvent and thickness. The Young's moduli at specific points on the film (E_polystyrene= 3.4 ± 0.3 GPa, E_{polymethylmethacrylate}= 4.2 ± 0.4 GPa) and over a given area (E_{polystyrene/polymethylmethacrylate}= 3.9 ± 0.4 GPa) were determined by combinatory use of the atomic force microscope and phase‐sensitive acoustic microscope. These results demonstrate a minimally invasive method for the quantitative characterization of polymer blend films.     

The analysis of morphological distortion during AFM study of cells

Atomic force microscopy (AFM) has been widely applied in cellular morphology study. However, morphological information including volume and roughness obtained by AFM are usually affected by different kinds of factors, which include the microscopic system itself, imaging mode, or external factors such as AFM probe or tip condition. In this study, based on red blood cell model, the dependence of cellular morphology, volume, and roughness on several parameters of the imaging was evaluated and, furthermore, a general rule and resolution for trustful analysis had been suggested. In addition, the potential effects that resulted from sample itself had also been analyzed based on adhesive force analysis. The results indicated that the scanning range and the imaging mode affect cellular volume and roughness, and the distorted images should be ascribed to blunt tip, contaminated tip, and the shape of tip. The analysis of morphological distortion during AFM investigation of cells provides a reference for researchers using AFM.     

Cleaning AFM colloidal probes by mechanically scrubbing with supersharp “brushes”

Contamination control of atomic force microscope (AFM) tips (including standard but supersharp imaging tips and particle/colloidal probes) is very important for reliable AFM imaging and surface/interface force measurements. Traditional cleaning methods such as plasma, UV–ozone and solvent treatments have their shortcomings. Here, we demonstrate that calibration gratings with supersharp spikes can be employed to scrub away contaminants accumulated on a colloidal sphere probe by scanning the probe against the spikes at high load at constant-force mode. The present method is superior to traditional cleaning methods in several aspects. First, accumulated lump-like organic/inorganic material can be removed; second, removal is non-destructive and highly efficient based on a “targeted removal” strategy; third, removal and probe shape/morphology study can be completed in a single step (we report, to our best knowledge, the first evidence of the wear of the colloidal sphere during force measurements); and fourth, both colloidal/particle probes and standard but supersharp AFM imaging tips can be treated.     

LED蓝宝石衬底抛光表面原子台阶形貌及其周期性研究

LED蓝宝石衬底的表面质量会极大影响到后续外延质量,进而影响到LED器件性能。蓝宝石研磨片经Al2O3磨粒粗抛液、SiO2磨粒精抛液下进行化学机械抛光(CMP),最终表面经原子力显微镜(AFM)所测表面粗糙度达到0.101nm,获得亚纳米级粗糙度超光滑表面,并呈现出原子台阶形貌。同时,通过使用Zygo表面形貌仪、AFM观察蓝宝石从研磨片经Al2O3粗抛液、SiO2精抛液抛光后的表面变化,阐述蓝宝石表面原子台阶形貌的形成原因,提出蓝宝石原子级超光滑表面形成的CMP去除机理。通过控制蓝宝石抛光中的工艺条件,获得a-a型、a-b型两种不同周期规律性的台阶形貌表面,并探讨不同周期规律性台阶形貌的形成机理。     

Surface micromorphology of dental composites [CE‐TZP]‐[Al2O3] with Ca+2 modifier

The objective of this study was to characterize the three‐dimensional (3D) surface micromorphology of the ceramics produced from nanoparticles of alumina and tetragonal zirconia (t‐ZrO₂) with addition of Ca⁺² for sintering improvement. The 3D surface roughness of samples was studied by atomic force microscopy (AFM), fractal analysis of the 3D AFM‐images, and statistical analysis of surface roughness parameters. Cube counting method, based on the linear interpolation type, applied for AFM data was used for fractal analysis. The morphology of non‐modified ceramic sample was characterized by the rather big (1–2 μm) grains of α‐Al₂O₃ phase with a habit close to hexagonal drowned in solid solution of t‐ZrO₂ with smooth surface. The pattern surfaces of modified composite content a little amount of elongated prismatic grains with composition close to the phase of СаСеAl₃О₇ as well as hexahedral α‐Al₂O₃‐grains. Fractal dimension, D, as well as height values distribution have been determined for the surfaces of the samples with and without modifying. It can be concluded that the smoothest surface is of the modified samples with Ca⁺² modifier but the most regular one is of the non‐modified samples. A connection was observed between the surface morphology and the physical properties as assessed in previous works. Microsc. Res. Tech. 78:840–846, 2015. © 2015 Wiley Periodicals, Inc.     

Investigation of morphological change of green tea polysaccharides by SEM and AFM

The objective of this study is to investigate the morphological structure and its change of green tea polysaccharides (GTPS) before and after enzyme reaction by scanning electron microscope (SEM) and atomic force microscope (AFM). Before enzyme reaction, with the novel sample preparation method SEM images of GTPS have obtained many branches and network structures. After enzyme reaction, the morphological structure of GTPS changed, and surface roughness increased. The microstructure of GTPS from SEM with the novel sample preparation method was in accordance with the results from AFM with the tapping mode. The results indicate that the novel sample preparation of GTPS for SEM is a simple, feasible, and reliable method for observing the surface morphology.     

Chemical force microscopy of self-assembled monolayers on sputtered gold films patterned by phase separation

Patterned self-assembled monolayers (SAMs) were formed on gold films and observed by friction force microscopy (FFM) and adhesive force mapping with pulsed-force mode atomic force microscopy (PFM-AFM). The substrate gold films were prepared by sputtering gold on flat surfaces of osmium-coated cover glass with surface roughness, Ra, of 0.3 nm. The patterned samples with the CH3 and COOH terminated regions were prepared using the Langmuir-Blodgett (LB) method, partial removal of the LB film by ultrasonication, and SAM formation. The CH3 and COOH terminated regions of the patterned SAMs in air and in water were observed by mapping friction and adhesive forces with FFM and PFM-AFM, respectively, using gold-coated AFM tips chemically modified with a thiol compound terminating in CH3 or COOH. The adhesive forces measured in air increased in the order of CH3/CH3, CH3/COOH (or COOH/CH3) and COOH/COOH, while those in water increased in reverse order. The enormous high adhesive force observed in water for CH3/CH3 was attributed to hydrophobic interaction between the CH3 tip and the CH3 terminated sample surface. With CH3 tip, the lower friction force was observed, however, in water on the CH3 terminated region than on the COOH terminated region. This experimental finding raises a question as to what is the effective normal load in friction measurements in water.