Surface roughness, mechanical and tribological properties of ultrathin tetrahedral amorphous carbon coatings from atomic force measurements

Atomic force microscope (AFM), lateral force microscope and AFM-based scratch and wear testing techniques were used to evaluate and compare the surface roughness, tribological and mechanical properties of thin (2.7-43 nm) tetrahedral amorphous carbon coatings prepared by pulsed cathodic arc discharge. It was found that surface roughness of ultrathin (2-8 nm) coatings was mainly determined by the roughness of the Si substrate and their average density strongly depended on their thickness. Poor friction, mechanical properties of thinner (2.7-15 nm) coatings can be associated with their low average density. The dense coatings (>15 nm) had lower friction coefficient, better scratch and wear resistance properties that were independent of their thickness. It appears that the over 15-nm coatings studied are feasible for some wear-resistant and tribological applications.     

Investigations of local electrical properties using tunneling/atomic force microscope with a quartz tuning fork nearfield sensor

Ability to determine local electric surface properties with a high resolution is a key issue in many modern industrial applications. In this article, authors will describe low-cost and reliable methods for investigations of electrical surface properties with a nanoscale resolution using a homebuilt modular tunneling/atomic force microscope with a quartz tuning fork as a probe. We will present the architecture of the designed system and the calibration method of the applied sensor. In our work, the usage of the tunneling atomic force microscope in the high-resolution investigations of the surface topography and identification of local spots where the tunneling current is observed will be demonstrated. We will also present current-voltage (I-V) spectroscopy performed on a gold thin film sputtered on silicon substrate and a highly oriented pyrolitic graphite (HOPG) surface, which we obtained in air ambient and at room temperature.     

Thin films of porphyrin molecules imaged with the atomic force microscope

The assembly of two-dimensional molecular structures of zinc porphyrin molecules arising from the dewetting of a porphyrin solution on mica and graphite is investigated using atomic force microscopy. Both a near equilibrium nucleation and growth process, and a far from equilibrium spinodal dewetting process are observed. Nucleation and growth around pre-existing surface defects on mica produces single layer disks, ∼ 10 μm in diameter, of densely packed molecules. Spinodal dewetting gives rise to the formation of much smaller, single layer, molecular islands of various sizes on both mica and graphite.     

Atomically resolved surface structures of vapor deposited amorphous silicon-carbon alloys: An atomic force microscopy and spectroscopic study

Silicon carbide alloys are widely used in high-tech applications due to their interesting combination of chemical, mechanical and electronic properties. Growing thin films of this material in a simple and controlled way is a hot topic in modern material's science. In particular, the possibility to tailor the film properties just by tuning the deposition temperature would be an important progress. In the present work amorphous silicon-carbon alloys thin films have been deposited by electron beam sublimation of a poly-crystalline silicon carbide target in vacuum environment. The deposition temperature was varied from Room Temperature to about 1300 K. The resulting films were analyzed by means of Ultra High Vacuum-Atomic Force Microscopy (UHV-AFM) down to even atomic resolution. The observed features agree with literature data, e.g. interatomic bond lengths, as achieved by others methods, and the structural arrangements of silicon and carbon atoms as concluded from IR and Raman spectroscopy measurements carried out on the same samples. The results not only allow a correlation between film properties and deposition temperature but also support the notion of the UHV-AFM images of the amorphous surfaces being atomically resolved.     

恒撞击力轻敲模式AFM的设计及研究

在轻敲模式AFM中,利用DMT模型与光探针点衍射理论结合来检测微探针的振动,并对振动信号进行频率域分析,通过检测和控制信号中高次谐波分量使针尖-样品间撞击力保持恒定。测试实验表明,该系统具有结构简单、可测不同材料的样品和对软质材料样品损伤小的优点,其测量重复性可达1%,分辩力可达1~5nm。     

A novel application of atomic force microscope to identify the Ag and I planes of β-AgI single crystals

 Atomic Force Microscopy is used to determine the crystallographic polarity of the surfaces of β-AgI single crystals. The studies reveal that the hexagonal packed Ag⁺ plane is the (001) and the I^– plane is the (001–). This observation is also consistent with the earlier x-ray diffraction measurements and chemical etching techniques as well as the polarizability and electronegativity of the ions. Received: 27 October 1997/Accepted: 28 October 1997     

Interfacial energy between carbon nanotubes and polymers measured from nanoscale peel tests in the atomic force microscope

The future development of polymer composite materials with nanotubes or nanoscale fibers requires the ability to understand and improve the interfacial bonding at the nanotube–polymer matrix interface. In recent work [Strus MC, Zalamea L, Raman A, Pipes RB, Nguyen CV, Stach EA. Peeling force spectroscopy: exposing the adhesive nanomechanics of one-dimensional nanostructures. Nano Lett 2008;8(2):544–50], it has been shown that a new mode in the Atomic Force Microscope (AFM), peeling force spectroscopy, can be used to understand the adhesive mechanics of carbon nanotubes peeled from a surface. In the present work, we demonstrate how AFM peeling force spectroscopy can be used to distinguish between elastic and interfacial components during a nanoscale peel test, thus enabling the direct measurement of interfacial energy between an individual nanotube or nanofiber and a given material surface. The proposed method provides a convenient experimental framework to quickly screen different combinations of polymers and functionalized nanotubes for optimal interfacial strength.     

In situ studies of the atomic layer deposition of thin HfO2 dielectrics by ultra high vacuum atomic force microscope

We studied in situ the initial stages of atomic layer deposition (ALD) of HfO₂ by an ultra high vacuum atomic force microscope working in frequency-modulation mode. The ALD cycles, made by using tetrakis-di-methyl-amido-Hf and water as precursors, were performed on the Si(001)/SiO₂ substrate maintained at 230 °C. After each ALD cycle we studied the influence of the HfO₂ growth on the surface height histogram, the root mean square roughness, the surface fractal dimension and the autocorrelation function. This detailed analysis of the surface topography allowed us to confirm the completion of the first HfO₂ layer after four ALD cycles.     

原子力声显微镜的原理及应用

原子力声显微镜结合了超声检测技术的三维成像能力与原子力显微镜的纳米尺度成像的近场显微技术。它在商用的原子力显微镜设备的基础上加以压电超声传感器产生声激励,并使用锁相放大器对数据进行收集分析,既可得到三维的纳米级的清晰形貌图,又能通过建模分析样品表面的接触刚度及样品的弹性模量。目前,原子力显微镜被广泛应用于材料领域,用于检测样品的机械性能,比如样品的接触刚度、薄膜高分子材料的弹性模量,同时还运用于医学生物领域,用于观察细胞的超微结构及其表面和亚表面的弹性模量等。     

Roughness determination of plasma-modified surface layers with atomic force microscopy

Graphite surfaces exposed to the deuterium plasma in the TEXTOR tokamak were characterized in detail by means of scanning probe microscopy, ion beam analysis and colorimetry methods. The aim is to study the composition and structure of thin layer deposits formed on surfaces subjected to the tokamak plasma. The surface roughness was measured and parametrized in terms of fractal dimension and scaling constant. Several different methods for the fractal analysis of plasma-exposed surfaces have been critically evaluated. The main emphasis of this paper is on the correlation between surface roughness (fractal parameters), the amount of deposited atoms and the layer thickness.     

Microstructural and micromechanical characterisation of TiAl alloys using atomic force microscopy and nanoindentation

Different microstructures were generated in the Ti–45Al–4.6Nb–0.2B–0.2C and Ti–45Al–1Cr alloys (at.%) by heat treatment. The microstructures were investigated using nanoindentation and atomic force microscopy which was compared with transmission electron microscopy. Topographic contrast is usually used for phase identification in the atomic force microscope. However, it was found that the topographic order of the phases changes with different microstructures and specimen preparations. Nanoindentation measurements provided local hardness values not obtainable by other methods and enabled clear distinction of the phases. The hardness values can give information on surrounding microstructure and solid solution hardening. The mean lamellar spacing of the colonies was measured using both atomic force microscopy and transmission electron microscopy. Atomic force microscopy was found to be suitable to determine the spacing between α₂/γ-interfaces offering the advantages of easier sample preparation and fewer specimens compared to evaluation by TEM analysis.     

新型大扫描范围原子力显微镜的研究

研制了一种大扫描范围原子力显微镜(AFM)。设计了新的扫描驱动电路,使单幅图像的扫描范围大幅度提高;用步进电机和扫描器配合扫描,得到序列图像,序列图像拼接后获得大范围样品图像。实验结果表明,采用这一方法,在±150V 的电压驱动下,AFM 的扫描范围可增大到10 ìm?1 mm 的量级,同时保持 1 nm 量级的测试分辨力。     

Measurement of elastic properties of calcium silicate hydrate with atomic force microscopy

Atomic force microscopy (AFM) based indentation is compared to conventional nanoindentation for measuring mechanical properties of cement pastes. In evaluating AFM as a mechanical characterization tool, various analytical and numerical modeling approaches are compared. The disparities between the numerical self-consistent approach and analytical solutions are determined and reported. The measured elastic Young’s modulus determined from AFM indentation tests are compared to elastic Young’s modulus determined from nanoindentation tests of cement paste. These results indicate that the calcium silicate hydrate (C-S-H) phase of hydrated Portland cement has different properties on the different length scales probed by AFM versus nanoindenters. Packing density of C-S-H particles is proposed as an explanation for the disparity in the measured results.     

一种用于纳米计量的原子力显微镜测头的设计

介绍了我们研制的一种高精度、具有计量学意义的原子力显微镜测头.该显微测头与其它部件协同工作在50 mm×50 mm×2 mm的测量范围内实现纳米级精度的测量.测头采用光束偏转法检测探针悬臂的微小偏移,由单模保偏光纤引入半导体激光作为光源.该测头安装有3个立体反射镜作为激光干涉仪的参考镜.样品与原子力显微镜测头的相对位置可以由激光干涉仪直接读数,可溯源到米国际定义及国家基准上.激光干涉仪的布置无阿贝误差.测头采用立体光路设计,结构紧凑.测头厚度小于20 mm,质量约200 g,却实现了100 mm的反射光程.使用该测头测得与量块表面的力-距离曲线,还测得标称高度300 nm SiO2台阶样板的图像,分辨率优于0.05 nm.     

A simple atomic force microscopy method for the visualization of polar and non-polar parts in thin organic films

Here we present a scanning probe microscopy method that allows for the identification of regions of different polarity (i.e. hydrophilicity) in thin organic films. This technique is based on the analysis of the difference between phase images generated at different applied bias voltages in tapping-mode atomic force microscopy. We show that, without any chemical modification of the microscope tip, it is possible to investigate surface properties of complex macromolecular layers, yielding new insight into the functional properties of the photosynthetic electron transport macromolecular complex, Photosystem I.     

Improvement of ultrathin polystyrene film stability by addition of poly(styrene-stat-chloromethylstyrene) copolymer: An atomic force microscopy study

A method to improve the stability of ultrathin polystyrene (PS) films on SiO_x/Si substrate is introduced. In this method, interfacial interactions between PS film and substrate are enhanced by addition of poly(styrene-stat-chloromethylstyrene(ClMS)) copolymer containing 5 mol% of ClMS group. The resulting slight structural modification of the copolymer does not cause phase separation in the polymer blend. On the other hand, the existence of polar ClMS groups provides anchoring sites on the polar SiO_x surface via dipolar interactions. In this study, ratios of the copolymers are varied from 0 to 40 wt.% in the thin films resulting in a systematic increase of the interfacial interactions. The dewetting behaviors of all films subjected to the same annealing conditions are explored via atomic force microscopy. The analyses of root mean square roughness and dewetting area as a function of annealing time and copolymer ratio provide information about the film stability. Our results indicate that blending small quantity of the copolymer with PS significantly increases the stability of ultrathin films.     

Direct measurement of interaction force between hydrophilic silica surfaces in triblock copolymer solutions with salt by atomic force microscopy

Triblock copolymers composed of polyethylene oxide (PEO) and polypropylene oxide (PPO) are used in various fields as nonionic surfactants. In this study, we measured interaction forces between untreated hydrophilic silica surfaces in solutions with two typical triblock copolymers, Pluronic P123 (PEO₂₀PPO₇₀PEO₂₀) and F127 (PEO₉₉PPO₆₅PEO₉₉), in the presence of 1 mM and 500 mM NaCl using atomic force microscopy (AFM). In solutions at the copolymer concentration of 1 µM, which is below the critical micelle concentration (CMC), the measured interaction forces were monotonically repulsive in the presence of 1 mM NaCl, which suggested the brush-like conformation of copolymers on the surfaces. When the concentration of NaCl was increased to 500 mM, interaction forces became attractive, which indicated the bridging of adsorbed polymers onto surfaces, the strength of which varied depending on the affinity and adsorption density of copolymers. The interactions at the copolymer concentration of 1 mM, which were above the CMC of both copolymers, were steric repulsions between adsorbed micelles on the surfaces with 1 mM of NaCl. For 500 mM of NaCl, an attractive jump after a steric repulsion was observed only in the force curve for P123, which inferred that the displacement of micelles from the surfaces was presumably due to a decrease in the strength of adsorption caused by the dehydration of EO groups. These results indicated that the length of the EO group considerably affected the interactions.     

Atomic force microscopy and atomic force acoustic microscopy characterization of photo-induced changes in some Ge-As-S amorphous films

Amorphous Ge₂₇As₁₃S₆₀, Ge₁₄As₂₇S₅₉ and Ge₁₆As₂₆S₅₈ thin films were prepared by thermal evaporation. Well annealed films were photodarkened by the photons with energy little exceeding the band gap energy. Using Atomic Force Microscopy we observed significant photoexpansion of studied films. Atomic Force Acoustic Microscopy revealed domains like structure of the surface and near surface parts of the samples which one was found to be more disintegrated after illumination.     

Formation and characterization of thin films from phthalocyanine complexes: An electrosynthesis study using the atomic-force microscope

(μ-Cyano)(phthalocyaninato)metal(III) [PcMCN]_n species with a central transition metal ion, such as Fe(III) and Co(III), were used to prepare molecular films on a highly oriented pyrolytic graphite electrode substrate by using the cyclic voltammetry technique. In order to investigate the influence of the ligand on the film properties, 1,8-dihydroxyanthraquinone and 2,6-dihydroxyanthraquinone as bivalent ligands were employed. The structure of the molecular materials was analyzed by infrared spectroscopy. The in situ film formation, texture, composition and conductivity of each film were further investigated using atomic force microscopy, scanning electron microscopy, energy-dispersive X-ray spectroscopy and the four-probe technique, respectively. The [PcMCN]_n complexes provided conductive films with an electrical conductivity of 1 × 10^− 6 Ω^− 1 cm^− 1 at 298 K.