Dynamic variations in adhesion of self-assembled monolayers on nanoasperities probed by atomic force microscopy

Octadecyltriethoxysilane (OTE) self- assembled monolayers (SAMs) and their effects on friction and adhesion have been investigated on various combinations of functionalized and unfunctionalized silicon oxide surfaces including the oxidized surface of crystalline Si(100), silica nanoparticle films, and oxidized Si atomic force microscopy (AFM) tips. Force-distance spectroscopy was utilized to probe and compare the properties of the OTE SAMs on silica asperities with nanoscale curvature against these same monolayers on surfaces with sub-1 nm roughness (flat surfaces). It was found that adhesion between SAMs and silicon oxide surfaces can vary significantly when assembly takes place on surfaces with nanoscopic curvature as compared to flat surfaces. Observations indicate that the SAM structure present during force measurements is dynamic in nature, which yields different adhesion values when measured with variations of both tip-sample contact time and tip-approach/retract rates. These results point the need in reporting a number of measurement parameters when probing adhesion by SAM functionalized tips.     

Adhesion and Friction Studies of Nano-textured Surfaces Produced by Self-Assembling Au Nanoparticles on Silicon Wafers

This article presents the results of nanoscale friction and adhesion of nanoparticle-textured surfaces (NPTS) using atomic force microscope (AFM). The effects of coverage ratio, texture height, and packing density on the adhesion and friction of the NPTS were investigated. The nano-textured surfaces were produced by self-assembling Au nanoparticles (NPs) with diameters of 20 nm and 50 nm on the silicon (100) surfaces, respectively. Surface morphology of the NPTS was characterized by field emission scanning electron microscopy and AFM. The results show that the NPTS significantly reduced the adhesive force compared to the smooth surface. The adhesion of NPTS is mainly dependent on the coverage ratio of NPs rather than the texture height and higher coverage ratio resulted in smaller adhesive force. The reduced adhesion of textured surfaces was attributed to the reduced real area of contact. The friction of NPTS is mainly dependent on the spacing between asperities. The lowered frictional force was obtained when the spacing between asperities is less than the size of AFM tip, because of the effectively reduced real area of contact between the AFM tip and the NPTS surface.     

Wetting study of patterned surfaces for superhydrophobicity

Superhydrophobic surfaces have considerable technological potential for various applications due to their extreme water-repellent properties. A number of studies have been carried out to produce artificial biomimetic roughness-induced hydrophobic surfaces. In general, both homogeneous and composite interfaces are possible on the produced surface. Silicon surfaces patterned with pillars of two different diameters and heights with varying pitch values were fabricated. We show how static contact angles vary with different pitch values on the patterned silicon surfaces. Based on the experimental data and a numerical model, the trends are explained. We show that superhydrophobic surfaces have low hysteresis and tilt angle. Tribological properties play an important role in many applications requiring water-repellent properties. Therefore, it is important to study the adhesion and friction properties of these surfaces that mimic nature. An atomic/friction force microscope (AFM/FFM) is used for surface characterization and adhesion and friction measurements.     

Wettability and Nanotribological Property of Multiply Alkylated Cyclopentanes (MACs) on Silicon Substrates

The geometrical microstructure together with the chemical composition of the surface governs the wettability of solid surfaces, which is very important in the study of nanoadhesion and nanofriction properties of surfaces. Multiply alkylated cyclopentane(MAC), a novel hydrocarbon mobile lubricant, was deposited on silicon by a dip-coating method. In order to investigate the influence of the surface microstructures on the wettability of MACs, silicon substrates were treated by different cleaning and etching processes. Measurements of an atomic force microscope and a contact angle meter indicate that the wettabilities of MACs on the hydroxylated silicon and the hydrogenated silicon are better than the wettability on the cleaned silicon, and that superiority is mainly caused by topological structure changes of the surface. Furthermore, the nanoadhesion and nanofriction properties were investigated. The different behaviors in adhesion and friction forces are due to the different surface energies of these silicon substrates.     

Nanotribological properties of silicon nano-pillars coated by a Z-DOL lubricating film

This paper reports a novel approach for improving the nanotribological properties of silicon (Si) surfaces by topographically and chemically modifying the surfaces. In the first step, Si (100) wafers were topographically modified into nano-pillars by using the photolithography and reactive ion etching (RIE) techniques. Various patterns, including nano-pillars of varying diameters and pitches (distance between pillars), were fabricated. Then, the patterns were coated with a Z-DOL (perfluoropolyether (PFPE)) lubricating film using a dipcoating technique, and this process was followed by thermal treatment. These modified surfaces were tested for their nanotribological properties, namely adhesion and friction forces, using an atomic force microscope (AFM). The results showed that the topographical modification and Z-DOL coating each independently reduced the adhesion and friction forces on the Si surfaces. However, the combination of the two surface treatments was most effective in reducing these forces. This is attributed to the combined effects of the reduction in the real area of contact due to patterning and the low surface energy of the Z-DOL lubricant. Further, it was found that adhesion and friction forces of the surfaces with combined modification varied significantly depending on the diameter of the pillars and the pitch. It is proposed that such a combination of surface modifications promises to be an effective method to improve the nanotribological performance of miniaturized devices, such as MEMS, in which Si is a typical material.     

Adhesion and friction studies of a nano-textured surface produced by spin coating of colloidal silica nanoparticle solution

This paper presents the results of adhesion and friction studies on a nano-textured surface. The nano-textures were produced by spin coating colloidal silica nanoparticle solution on a flat silicon substrate. Surface morphology was characterized by environmental scanning electron microscopy (ESEM) and scanning probe microscopy (SPM). Adhesion and friction studies were conducted using a TriboIndenter employing diamond tips with 5 μm and 100 μm nominal radii of curvature. The results show that the adhesion forces and coefficients of friction of the nano-textured surface measured by the 100 μm tip were reduced up to 98 and 88%, respectively, compared to those of a baseline silicon oxide film surface.     

Surface characterization and adhesion and friction properties of hydrophobic leaf surfaces

Super-hydrophobic surfaces as well as low adhesion and friction are desirable for various industrial applications. Certain plant leaves are known to be hydrophobic in nature. These leaves are hydrophobic due to the presence of microbumps and a thin wax film on the surface of the leaf. The purpose of this study is to fully characterize the leaf surface and to separate out the effects of the microbumps and the wax on the hydrophobicity. Furthermore, the adhesion and friction properties of the leaves, with and without wax, are studied. Using an optical profiler and an atomic/friction force microscope (AFM/FFM), measurements on the hydrophobic leaves, both with and without wax, were made to fully characterize the leaf surface. Using a model that predicts contact angle as a function of roughness, the roughness factor for the hydrophobic leaves has been calculated, which is used to calculate the contact angle for a flat leaf surface. It is shown that both the microbumps and the wax play an equally important role in the hydrophobic nature as well as adhesion and friction of the leaf. This study will be useful in developing super-hydrophobic surfaces.     

Adhesion and Friction Studies of a Selectively Micro/Nano-textured Surface Produced by UV Assisted Crystallization of Amorphous Silicon

This paper presents a novel methodology of producing selectively micro/nano-textured surfaces for applications in micro/nano-electro-mechanical systems, and friction and adhesion/stiction studies on the micro/nano-textured surfaces. The selective textures were produced by ultraviolet-assisted aluminum-induced crystallization of plasma-enhanced chemical vapor deposited amorphous silicon. Friction and adhesion/stiction studies were conducted using a TriboIndenter. The results show that the surface texturing technique significantly reduces both adhesion/stiction forces and coefficients of friction.     

Adhesion and Friction Enhancement of Film-Terminated Structures against Rough Surfaces

A number of biomimetic and bioinspired micron-scale surface structures have been developed in recent years with unique surface properties such as highly enhanced and switchable adhesion and friction against smooth surfaces. However, few studies have examined the effect of roughness on mechanisms for property enhancement, although this is of critical importance for applications. Here, we investigate the effect of roughness on adhesion and friction of a family of film-terminated fibrillar and ridge/channel microstructures. Although increasing roughness uniformly attenuates adhesion and friction, we find that the film-terminated structures maintain their enhancement compared to flat controls against a variety of rough surfaces (including natural stones). The principal mechanisms underlying property enhancement against smooth surfaces remain operative against rough surfaces. We show how the effect of roughness on surface mechanical properties of structured surfaces can be understood as a combination of known effects due to structure and roughness.     

Tribological properties of adsorbed water layer on silicon surfaces

Tribological properties of adsorbed water layer on solid surface in sliding contact have not yet been fully understood. In this regard, it is important to better understand how surface hydrophilicity and humidity influence the tribological behavior of adsorbed water-mediated microcontact. In this study, we investigated the influence of adsorbed water layer and capillary force on friction as a function of relative humidity for silicon surfaces with different water affinity. Friction of the silicon surface with different water affinity was examined under various humid environments in a wearless sliding condition (low contact pressure) against a glass sphere. Numerical analysis was also conducted to calculate capillary force and interfacial shear strength for each surface as a function of relative humidity. The friction of the hydrophobic Si surface was low and stable, and almost independent of relative humidity whereas that of the hydrophilic surfaces were significantly influenced by relative humidity. These behaviors were explained in terms of capillary wetting and the role of confined water layer in the contact area. The influence of confined water layer became more dominant over capillary force as relative humidity increased. There was a good correlation between the calculated shear strength and the measured friction force for all surfaces regardless of their hydrophilicity and humidity condition.     

Surface charges and adhesion measured by atomic force microscope influence on friction force

A good correlation has been found between friction force measured using a ball-on-disc tribometer (normal load 200 mN) and adhesion hysteresis measured by atomic force microscopy. Both adhesion and friction forces were investigated in liquid media (water, ethanol, formamide, ethylene glycol) and involved interactions between silicon nitride and several materials (Si(1 0 0), Si(1 1 1), silica glass, DLC and TiN coatings). Despite the difference between the two scales of measurement, comparison between the measured friction force and the dissipated energy during the adhesion process has shown that the two quantities follow the same trend. Additional experiments were conducted in NaCl 10⁻³ M at various pH values in order to investigate surface charge effect on adhesion and friction.     

Tribological properties of asperity arrays coated with self-assembled monolayers

The effects of a self-assembled monolayer (SAM) coating on the friction and pull-off forces were determined by using two-dimensional asperity arrays on silicon wafers. The arrays were coated with SAM composed of one of five different alkylchlorsilanes. First, two-dimensional asperity arrays were created by using a focussed ion beam (FIB) system to mill patterns on silicon plates. Each silicon plate had different patterns of equally spaced asperities. Each pattern (5 × 5 μm²) had a different radius of curvature of the asperity peaks, ranging from about 200 to 2500 nm. Then, each silicon plate was immersed in a solution of a different alkylchlorsilane in hexane (either hexyltrichlorosilane, octyltrichlorosilane, dodecyltrichlorosilane, tetradecyltrichlorosilane, or octadecyltrichlorosilane), thus coating the asperity arrays with SAM. The friction and pull-off forces on the SAM-coated arrays were measured by using an atomic force microscope (AFM) that had a square flat probe. The pull-off force for SAM-coated silicon was roughly proportional to the radius of curvature of the asperity peaks. The magnitude of the pull-off force corresponded approximately to the capillary force calculated by using the contact angle of water on the surface of SAM. The friction coefficient correlated with the inverse of the alkyl-chain length of the SAM.     

Rolling friction and adhesion between smooth solids

Rolling friction has been explained in terms of crack propagation through an adhesive joint. The contact between a smooth cylinder and flat has been regarded as an adhesive junction bounded by two cracks moving in the same direction at the same speed, one crack continually opening and one closing. Propagation of these cracks requires a force which is calculated from crack theory and shown to be equal to the friction.The theory has been verified experimentally using glass cylinders rolling on smooth rubber. Results show that rolling friction is closely connected with peel adhesion. Moreover, this adhesion interpretation of rolling friction between smooth surfaces explains several observations: (a) the existence of a static rolling friction, (b) the unusually high value of friction and its independence from load and roller radius, (c) the marked effect of lubricant or dust.     

Ni nanodot-patterned surfaces for adhesion and friction reduction

Surface nano-patterning with Ni nanodot arrays was investigated for adhesion and friction reduction of contacting interfaces. Self-assembled anodized aluminum oxide (AAO) templates in conjunction with thermal evaporation was used to fabricate nano-patterned surfaces with ordered Ni nanodot arrays on Si substrates. Surface morphology of the Ni nanodot-patterned surfaces (NDPSs) was characterized by scanning electron microscopy (SEM). Adhesion and friction studies on a Ni NDPS and a baseline smooth Si(100) surface were conducted using a TriboIndenter employing a diamond tip with 100 μm nominal radius of curvature. The results show that the ordered Ni nanodot-patterning reduced the adhesion forces and coefficients of friction up to 92 and 83%, respectively, compared to those of the smooth silicon surface. Surprisingly, the nanoscale multi-asperity contact between the diamond tip and inhomogeneous Ni NDPSs under low loads follows a continuum contact mechanics model.     

Microscopic Friction Studies on Metal Surfaces

Atomically flat and clean metal surfaces exhibit a regime of ultra-low friction at low normal loads. Atomic force microscopy, performed in ultra-high vacuum on Cu(100) and Au(111) surfaces, reveals a clear stick-slip modulation in the lateral force but almost zero dissipation. Significant friction is observed only for higher loads (∼4–6 nN above the pull-off force) together with the onset of wear. We discuss the minor role of thermal activation in the low friction regime and suggest that a compliant metallic neck between tip and surface is formed which brings upon the low, load-independent shear stress.     

Reducing Friction Force of Si Material by Means of Atomic Layer-Deposited ZnO Films

With excellent lubricating property, zinc oxide (ZnO) films are promising candidates to act as protective coatings in Si-based microelectromechanical system devices for the purpose of decreasing friction forces of silicon (Si) material. In this paper, the nanotribological behavior of ZnO films prepared by atomic layer deposition on a Si (100) substrate is investigated by an atomic force microscope. The ZnO films have various thicknesses ranging from 10.0 to 182.1 nm. With the increase of film thickness, the root-mean-square roughness of the films increases, while the ratio of hardness to Young’s modulus (H/E) decreases. Due to their large surface roughness, the thick ZnO films are low in adhesion force. The friction force of the ZnO films is smaller than that of the Si (100) substrate and is greatly influenced by their adhesion force and mechanical property. In a low-load condition, the friction force is dominated by the adhesion force, and thus, the friction force of the ZnO films decreases as film thickness increases. While in a high-load condition, the friction force is dominated by plowing. Films with higher H/E possess smaller friction force, and thus, the friction force increases with the decreasing film thickness.     

Investigation of tribo-chemistry by means of stable isotopic tracers: Mechanism for durability of monomolecular boundary film

A monomolecular film of octadecanoic acid on a Si(1 0 0) surface was prepared using a computer-controlled Langmuir trough. The tribological properties were acquired by a ball-on-flat type tribo-tester under reciprocating motion. Considerable effects of ball material on lifetime for low friction were observed; a glass ball was excellent while a steel ball was poor. The rubbed surfaces on ball and flat were studied by time-of-flight secondary ion mass spectroscopy. Transfer of the carboxylic acid and silicon onto the ball surface from the flat specimen was found. The role of the transferred acid that prolongs the lifetime of low friction was proposed. It should be emphasized that deuterium-labeled carboxylic acid makes the target of TOF-SIMS analysis clear.     

核主泵备用机械密封材料的摩擦性能研究

采用Falex-1506摩擦磨损试验机,研究了水润滑、室温条件下,载荷和速度对核主泵用机械密封材料:无压烧结碳化硅(WNV2)和碳化硅加碳(CHV1)、反应烧结碳化硅(R)和碳化硅加碳(R2)、石墨(MSMG)在不同配副条件下摩擦学特性的影响规律。使用扫描电镜(SEM),对磨损表面进行了观察和分析。研究结果表明,碳化硅和石墨材料自身的孔隙,在高载荷下容纳了更多的润滑流体,因此,不同配副条件下的摩擦系数均随载荷的增加而减小。另外,滑动速度引起的温度改变通过影响表面层性质影响摩擦力,而碳化硅和石墨在很宽的温度范围内机械性质保持不变,所以摩擦系数随速度的增加基本不变。     

Tribological properties of bio-mimetic nano-patterned polymeric surfaces on silicon wafer

Nano-patterns made of poly(methyl methacrylate) (PMMA) were fabricated on silicon wafer using a capillarity-directed soft lithographic technique. Patterns with three different aspect ratios were investigated for their adhesion and friction properties at nano-scale and for friction at micro-scale. The patterned samples exhibited superior tribological properties, at both these scales when compared to those of flat PMMA thin films.     

Surface modification of AFM silicon probes for adhesion and wear reduction

Tip wear of silicon probes used for an atomic force microscope (AFM) is a critical issue. Wear can result in an increase of tip radius and adhesion between tip and sample, thus reducing the image resolution and introducing artifacts. In order to reduce adhesion, friction, and wear so as to reduce tip related artifacts, liquid lubricant (Z-TETRAOL), self-assembled monolayers (pentafluorophenyltriethoxysilane (PFPTES)), and fluorocarbon polymer (Fluorinert™) were applied on the silicon probe. A comprehensive investigation of adhesion, friction, and wear of the uncoated/coated tips in both ambient air and various humidity levels as well as the influence of the coatings on the image resolution was performed. Experiments showed that the coatings reduced the adhesion, friction, and wear of the silicon tip, improved the initial image resolution, and exhibited less deterioration as compared to that of uncoated tip in the long-term test.