Micro- to nanoscale surface morphology and friction response of tribological polyimide surfaces

Sintered polyimide surfaces that were worn under macroscale conditions at different temperatures, were further characterised by contact-mode atomic force microscopy for getting insight in the tribophysical and -chemical processes at the micro- to nanoscale. Depending on the temperature, either mechanical interaction (23 °C < T < 100 °C), hydrolysis (120 °C < T < 140 °C), or imidisation (180 °C < T < 260 °C) results in different microscale surface characteristics. At low temperatures, surface brittleness and inter-grain fracture has been observed with an almost homogeneous friction pattern. At intermediate temperatures, the formation of a protecting local film leads to smoother surfaces with local lubricating properties. At high temperatures, different topographical and frictional patterns are observed depending on local imidisation or degradation. From AFM scans at the sub-micronscale, local debris depositions are observed and correspond to surface locations with locally reduced friction. From AFM scans at the nanoscale, polymer chain orientation is observed with formation of zig-zag or stretched molecular conformation: the latter is not induced by purely mechanical surface interactions or hydrolysis, but mainly results from tribochemically induced imidisation at high sliding temperatures. The present investigation describes the influences of local tribological interactions onto the macroscale wear behaviour of a polymer, and therefore aims at contributing to a better understanding of scaling between macro- to nanolevel tribological response.     

Surface roughness and friction coefficient in peened friction stir welded 2195 aluminum alloy

The tribological properties of friction stir welded 2195 aluminum alloy joints were investigated for several laser- and shot-peened specimens. The first portion of this study assessed the surface roughness changes at different regions of the weld resulting from the various peening processes and included an atomic force microscopy (AFM) study to reveal fine structures. The second portion investigated the friction characteristics for various conditions when slid against a 440C ball slider. Shot peening resulted in significant surface roughness when compared to the unpeened and laser-peened samples. The initial friction for all types of specimens was highly variable. However, long-term friction was shown to be lowest for samples with no peening treatment. Laser peening caused the friction to increase slightly. The shot peening process on the other hand resulted in an increase of the long-term friction effects on both sides of the weld.     

Tribological Properties of MACs-APS Films

Multiply-alkylated cyclopentanes (MACs) with different molecular structure were deposited on single crystal silicon wafers coated with a thin aminopropyltrimethoxylsilane (APS) film as an adhesive layer to form MACs-APS films. The thickness, wetting behavior and nano-scale morphologies of the films were characterized by means of ellipsometry, contact angle measurement, and atomic force microscopy (AFM). The friction and wear behaviors of the thin films sliding against a Si₃N₄ ball were examined on a UMT-2MT tribometer in a ball-on-disk contact mode. The worn surfaces of the MACs-APS films and the counterpart Si₃N₄ balls were investigated with a scanning electron microscope (SEM). It was found that the water contact angles on the MACs-APS film increased with the MACs alkyl chain-length. The MACs-APS film exhibited higher load-carrying capacity and better friction reduction and anti-wear behavior as compared with the APS film. This is suggested to occur because the APS acts as a strongly bonded lubricant phase and MACs as a mobile lubricant phase in the MACs-APS film. The increase of the chain-length of the alkyl substituent in the MACs compounds resulted in improved tribological properties of MACs-APS film. It is suggested that the longer alkyl chains are much more flexible and can dissipate the mechanical energy during the shearing process more easily than the short chain compounds. MACs with the longer chains have stronger chain-chain interactions and the larger MAC molecules have stronger intermolecular interactions, resulting in the good tribological properties of MACs-APS film.     

Observed transition from linear to non-linear friction-load behavior using a lateral force microscope

The most commonly observed friction behavior for sliding systems is that described by Amontons laws of friction. In this case, sliding friction is independent of the gross or apparent area of contact between the materials and a linear function of the applied normal load, where the constant of proportionality is called the friction coefficient. However, for dry sliding solids in contact via a single-asperity junction, Amontons (linear) friction-load behavior is not strictly relevant. In experiments measuring sliding friction between a silicon tip and a quartz surface using an atomic force microscope (AFM), a transition from linear to non-linear friction-load behavior has been observed. This is proposed to result from a nanoscale ‘conditioning’ of a multiple-contact tip-surface interface to form a single-asperity contact.     

Tribological behaviors of self-assembled 3-aminopropyltriethoxysilane films on silicon

3-Aminopropyltriethoxysilane (APTES) thin films were prepared on the hydroxylated silicon substrate by a self-assembling process from formulated solution. Chemical compositions of the films were detected by X-ray photoelectron spectrometry (XPS). The thickness of the films was determined with an ellipsometer, while the morphologies of the original and worn surfaces of the samples were analyzed by means of atomic force microscopy (AFM) and scanning electron microscopy (SEM), respectively. The tribological properties of APTES thin films sliding against GCr15 steel ball were evaluated on a UMT-2MT reciprocating friction and wear tester. It was found that the macroscopic friction coefficients for coating times more than 1 h ranged from 0.177 to 0.3 whereas the value for short coating time was as high as 0.8. It was also found that the tribological behaviors of APTES films were sensitive to normal load and sliding velocity. SEM observation of the morphologies of worn surfaces indicates that the wear of silicon is characteristic of brittle fracture and severe abrasion. Differently, abrasion and micro-crack dominate the wear of APTES–SAM. The superior friction reduction and wear resistance of APTES films compared to the silicon substrate are attributed to good adhesion of the films to the substrate.     

Adhesion studies of latex film surfaces on the meso- and nanoscale

In this paper the effects of surface roughness and annealing temperature (T) of latex coating films on adhesion are discussed for the different stages of the film formation process. The surface free energy of latex films was assessed in terms of practical work of adhesion (W) (or adherence) using a custom-built adhesion-testing device (ATD), atomic force microscopy (AFM), and contact angle measurements. For preannealed latex films surface roughness averages (R_a) were determined from AFM height images and were related to the values of W obtained from ATD measurements at room temperature. The results obtained using these tests exhibiting surface behavior on different length scales indicate a dependence of the measured adhesion on surface roughness and temperature, as well as on the length scale of the measurements.First preannealed samples were studied, which were obtained by heat treatment above the respective glass transition temperatures (T_g). Increasing the temperature of preannealing resulted in a decrease of the adherence observed in ATD experiments at room temperature. However, on the nanoscale, using AFM, no significant variation of the adherence was observed. This observation can be explained by roughness arguments. Preannealing decreases roughness which results in lower adherence values measured by ATD while for essentially single asperity AFM experiments roughness has an insignificant effect. Specimens were also annealed over a constant period of time (90 min) at different temperatures. At the end of the heat treatment, adhesion was measured at the treatment temperature by ATD. The amplified effect of temperature observed in this case on adherence is attributed to the combination of roughness decrease and increasing test temperature. In a third set of experiments completely annealed samples were studied by ATD as well as by AFM as a function of temperature. With increasing T values ATD showed a decrease in adherence, which is attributed to a decreasing surface free energy of the annealed films at elevated T values. AFM, on the other hand, showed an opposite trend which is assigned to increasing penetration of the tip into the tip/wetting polymer samples versus increasing temperature. Finally, annealing isotherms as a function of time were investigated by ATD in situ at different temperatures. This last set of experiments allowed us to optimize annealing time and temperature to achieve complete curing.     

Tribological Behavior of Multiply-Alkylated Cyclopentanes (MACs)-Cu Nanoparticles Composite Thin Film

Multiply-alkylated cyclopentanes (MACs) composite thin films containing Cu nanoparticles are fabricated on the octadecyltrichlorosilane (OTS)-modified substrate by a spin-coating technique. The thickness, wetting behavior, and nanoscale morphologies of the films are characterized by means of ellipsometry, contact angle measurement, and atomic force microscope (AFM). The friction and wear behaviors of the thin films sliding against Si₃N₄ ball are examined on a UMT-2MT tribometer in a ball-on-disk contact mode. The worn surfaces of the OTS-MAC-Cu composite film and the counterpart Si₃N₄ balls are investigated with a scanning electron microscope. Water contact angle on OTS-MAC-Cu composite film is higher than that of OTS-MAC film. OTS-MAC-Cu composite film exhibits higher load-carrying capacity and better friction reduction and antiwear behavior as compared with OTS-MAC film. This may be attributed to the load-carrying and self-repairing property of the Cu nanoparticles in the composite film and the formation of a transfer layer composed of OTS, MAC, and Cu on the rubbing surface of the counterpart ball.     

Tribological carbon-based coatings: An AFM and LFM study

In this work some carbon-based coatings were studied by atomic force microscopy (AFM) and lateral force microscopy (LFM) techniques in order to evaluate their microstructure and friction properties at the micro and nanoscale. With this aim, four samples were prepared by magnetron sputtering: an amorphous carbon film (a-C), two nanocomposites TiC/a-C with different phase ratio (∼1:1 and ∼1:3) and a nanocrystalline TiC sample. Additionally, a highly oriented pyrolytic graphite (HOPG) and an amorphous hydrogenated carbon coating (a-C:H) were included to help in the evaluation of the influence of the roughness and the hydrogen presence respectively. The topography (roughness) of the samples was studied by AFM, whereas LFM was used to measure the friction properties at the nanoscale by two different approaches. Firstly, an evaluation of possible friction contrast on the samples was done. This task was performed by subtraction of forward and reverse images and lately confirmed by the study of lateral force profiles in both directions and the histograms of the subtraction images. Secondly, an estimation of the average friction coefficient over the analysed surface of each sample was carried out. To take into account the tip evolution/damaging, mica was used as a reference before and after each sample (hereafter called sandwich method), and samples-to-mica friction ratios were calculated. The LFM was shown to be a useful tool to characterise a mixture of phases with different friction coefficients. In general, the friction ratios seemed to be dominated by the amorphous carbon phase, as it was impossible to distinguish among samples with different proportions of the amorphous phase (friction ratios between 1.5 and 1.75). Nevertheless, it could be concluded that the differences in friction behaviour arose from the chemical aspects (nature of the phase and hydrogen content) rather than surface characteristics, since the roughness (Ra values up to 5.7 nm) does not follow the observed trend. Finally, the Ogletree method was employed in order to calibrate the lateral force and estimate the friction coefficient of our samples. A good agreement was found with macroscopic and literature values going from ∼0.3 for TiC to ∼0.1 for pure carbon.     

Contact mechanics analysis of oscillatory sliding of a rigid fractal surface against an elastic–plastic half-space

Oscillatory sliding contact between a rigid rough surface and an elastic–plastic half-space is examined in the context of numerical simulations. Stick-slip at asperity contacts is included in the analysis in the form of a modified Mindlin theory. Two friction force components are considered – adhesion (depending on the real area of contact, shear strength and interfacial adhesive strength) and plowing (accounting for the deformation resistance of the plastically deformed half-space). Multi-scale surface roughness is described by fractal geometry, whereas the interfacial adhesive strength is represented by a floating parameter that varies between zero (adhesionless surfaces) and one (perfectly adhered surfaces). The effects of surface roughness, apparent contact pressure, oscillation amplitude, elastic–plastic properties of the half-space and interfacial adhesion on contact deformation are interpreted in the light of numerical results of the energy dissipation, maximum tangential (friction) force and slip index. A non-monotonic trend of the energy dissipation and maximum tangential force is observed with increasing surface roughness, which is explained in terms of the evolution of the elastic and plastic fractions of truncated asperity contact areas. The decrease of energy dissipation with increasing apparent contact pressure is attributed to the increase of the elastic contact area fraction and the decrease of the slip index. For a half-space with fixed yield strength, a lower elastic modulus produces a higher tangential force, whereas a higher elastic modulus yields a higher slip index. These two competing effects lead to a non-monotonic dependence of the energy dissipation on the elastic modulus-to-yield strength ratio of the half-space. The effect of interfacial adhesion on the oscillatory contact behaviour is more pronounced for smoother surfaces because the majority of asperity contacts deform elastically and adhesion is the dominant friction mechanism. For rough surfaces, higher interfacial adhesion yields less energy dissipation because more asperity contacts exhibit partial slip.     

Tribological Behaviors of Fluorinated Polyimides at Different Temperatures

4,4′-(hexafluoroisopropylidene) diphthalic anhydride (6FDA)-based copolyimides were synthesized and the tribological properties of the copolyimides with different heat histories were studied at different temperatures. Fluoride-containing polyimide (PI) showed better thermal stability, decreased friction coefficients, and postponed the consequence of friction variation, which depended on temperature, than nonfluorinated PI. Thermal treatments seemed to increase the friction coefficients of copolyimides, and reduced the tensile strengths of the materials. The effects of applied load (P) and sliding speed (V) on tribological behaviors of thermally treated copolyimides were also examined and the variations of friction coefficient depending on PV values were investigated for clear understanding of its relationship between PV value and friction coefficient with different thermal treating time. Distortions of net structures of the chains and molecular motion contributed to variations of tribological properties of thermal treated copolyimides.     

The effect of substrate roughness on the static friction of CuO nanowires

The dependence of static friction on surface roughness was measured for copper oxide nanowires on silicon wafers coated with amorphous silicon. The surface roughness of the substrate was varied to different extent by the chemical etching of the substrates. For friction measurements, the nanowires (NWs) were pushed by an atomic-force microscope (AFM) tip at one end of the NW until complete displacement of the NW was achieved. The elastic bending profile of a NW during this manipulation process was used to calculate the ultimate static friction force. A strong dependence of static friction on surface roughness was demonstrated. The real contact area and interfacial shear strength were estimated using a multiple elastic asperity model, which is based on the Derjaguin–Muller–Toporov (DMT) contact mechanics. The model included vertical elastic flexure of NW rested on high asperities due to van der Waals force.     

Tribological properties of chemically bonded polyimide films on silicon with polyglycidyl methacrylate brush as adhesive layer

Polyimide thin films, which possess good stability and film uniformity, are successfully fabricated on single crystal silicon wafers coated with a thin polymer brush by suface-initiated polymerization (SIP) as an adhesive layer. The growth kinetic of polyglycidyl methacrylate (PGMA) brush was studied by the means of ellipsometry. The nano-scale morphology and chemical composition of PGMA brush and polyimide film were studied with atomic force microscopy (AFM), Fourier transform infrared spectrum (FT-IR), and X-ray photoelectron spectroscopy (XPS). The tribological behaviors of the thin films sliding against AISI-52100 steel ball were examined on a static-dynamic friction precision measurement apparatus and UMT-2MT tribometer. The worn surface of the polyimide thin films was investigated with scanning electron microscopy (SEM). The results indicated that the chemically bonded polyimide films exhibited better friction reduction and antiwear behavior compared to the polymide films on bare silicon surface. At a load of 0.5 N and sliding speed of 20 mm s⁻¹, the durability life of the polyimide thin films is over 25,000 sliding cycles and the friction coefficient is about 0.08.     

Friction,adhesion and wear durability of an ultra-thin perfluoropolyether-coated 3-glycidoxypropyltrimethoxy silane self-assembled monolayer on a Si surface

The tribological properties, such as coefficient of friction, adhesion and wear durability of an ultra-thin (<10?nm) dual-layer film on a silicon surface were investigated. The dual-layer film was prepared by dip-coating perfluoropolyether (PFPE), a liquid polymer lubricant, as the top layer onto a 3-glycidoxypropyltrimethoxy silane self-assembled monolayer (epoxy SAM)-coated Si substrate. PFPE contains hydroxyl groups at both ends of its backbone chain, while the SAM surface contains epoxy groups, which terminate at the surface. A combination of tests involving contact angle measurements, ellipsometry, atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS) was used to study the physical and chemical properties of the film. The coefficient of friction and wear durability of the film were investigated using a ball-on-disk tribometer (4?mm diameter Si₃N₄ ball as the counterface at a nominal contact pressure of ～330?MPa). AFM was used to investigate the adhesion forces between a sharp Si₃N₄ tip and the film. This dual-layer film had a very low coefficient of friction, adhesion and wear when compared to epoxy SAM-coated Si only or bare Si surface. The reasons for the improved tribological performance are explained in terms of the lubrication characteristics of PFPE molecules, low surface energy of PFPE, covalent bonding between PFPE and epoxy SAM coupled with reduced mobile PFPE. The low adhesion forces coupled with high wear durability show that the film has applications as a wear resistant and anti-stiction film for microcomponents made from Si.     

Friction and Wear of Polyphenylene Sulfide (PPS), Polyethersulfone (PES) and Polysulfone (PSU) Under Different Cooling Conditions

The friction and wear properties of polyphenylene sulfide (PPS), polyethersulfone (PES) and polysulfone (PSU), which have similar molecular structure, were investigated using an end-face contact tribometer in three different cooling ways: sliding without air cooling, sliding with air cooling, and sliding in water. The worn surface and wear debris were observed using a scanning electron microscope (SEM). The effect of frictional heat on the tribological properties of the polymers was comparatively studied. When sliding in air, with increasing applied load, the wear rate of PPS decreased slightly initially then increased later while the wear rate of PES and PSU increased through out. The results suggested that the friction coefficient was mainly affected by the temperature of the worn polymer that was controlled by the balance of heat flow of the whole sliding contact system. When sliding in water, the friction coefficients of the three polymers decreased compared to that sliding in air and remained relatively steady through the whole process under different load. The wear rates of the three polymers had a close value and, remarkably, increased compared to that sliding in air. The water cooling and lubrication role decreased the tribological properties difference between the polymers.     

DLC nano-dot surfaces for tribological applications in MEMS devices

With the invention of miniaturized devices like micro-electro-mechanical systems (MEMS), tribological studies at micro/nano-scale have gained importance. These studies are directed towards understanding the interactions between surfaces at micro/nano-scales, under relative motion. In MEMS devices, the critical forces, namely adhesion and friction restrict the smooth operation of the elements that are in relative motion. These miniaturized devices are traditionally made from silicon (Si), whose tribological properties are not good. In this paper, we present a short investigation of nano- and micro-tribological properties of diamond-like carbon (DLC) nano-dot surfaces. The investigation was undertaken to evaluate the potential of these surfaces for their possible application to the miniaturized devices. The tribological evaluation of the DLC nano-dot surfaces was done in comparison with bare Si (1 0 0) surfaces and DLC coated silicon surfaces. A commercial atomic force microscope (AFM) was used to measure adhesion and friction properties of the test materials at the nano-scale, whereas a custom-built micro-tribotester was used to measure their micro-friction property. Results showed that the DLC nano-dot surfaces exhibited superior tribological properties with the lowest values of adhesion force, and friction force both at the nano- and micro-scales, when compared to the bare Si (1 0 0) surfaces and DLC coated silicon surfaces. In addition, the DLC nano-dot surfaces showed no observable wear at the micro-scale, unlike the other two test materials. The superior tribological performance of the DLC nano-dot surfaces is attributed to their hydrophobic nature and the reduced area of contact projected by them.     

Tribological behavior of micro/nano-patterned surfaces in contact with AFM colloidal probe

In effort to investigate the influence of the micro/nano-patterning or surface texturing on the nanotribological properties of patterned surfaces, the patterned polydimethylsiloxane (PDMS) surfaces with pillars were fabricated by replica molding technique. The surface morphologies of patterned PDMS surfaces with varying pillar sizes and spacing between pillars were characterized by atomic force microscope (AFM) and scanning electron microscope (SEM). The AFM/FFM was used to acquire the friction force images of micro/nano-patterned surfaces using a colloidal probe. A difference in friction force produced a contrast on the friction force images when the colloidal probe slid over different regions of the patterned polymer surfaces. The average friction force of patterned surface was related to the spacing between the pillars and their size. It decreased with the decreasing of spacing between the pillars and the increasing of pillar size. A reduction in friction force was attributed to the reduced area of contact between patterned surface and colloidal probe. Additionally, the average friction force increased with increasing applied load and sliding velocity.     

Atomic force microscopy studies of chemical–mechanical processes on silicon(100) surfaces

Atomic force microscopy (AFM) is used to examine chemical–mechanical processes on Si(100) surfaces. The AFM tip serves as a single asperity contact to exert tribological forces as well as an imaging tool. By scanning in chemically aggressive solutions, material removal can be observed directly. In the silicon system, high-force scans are used to remove oxide and initiate etching in selected locations, followed by low-force scans to image the resulting surfaces. Material removal rates were measured as a function of applied load, number of scans, solution composition, and time. In basic solution, places where the underlying silicon is exposed etch rapidly, producing structures 100 nm or less in size. Although the surface roughness initially increases during etching, the final surfaces are smooth. The oxide is extremely sensitive to applied stress: even very light scanning accelerates oxide dissolution. Once the oxide is removed, chemical etching proceeds through the underlying silicon with or without AFM scanning; but the silicon etches more rapidly if AFM scanning is continued, due to true chemical–mechanical (tribochemical) effects.     

Ultraviolet or Atomic Oxygen Effects on Tribological Properties of the Carbon Fibers/Polyimide Composites

Carbon fibers-reinforced polyimide composites (CF-PI) were fabricated by means of a hot press molding technique. To contrast the effects of ultraviolet and atomic oxygen irradiation under high vacuum on the tribological properties of CF-PI composites, the friction and wear properties of the composites sliding against GCr15 steel ball before and after irradiation were conducted in high vacuum on a ball-on-disk test rig. The experimental results revealed that CF-PI composites exhibited higher modulus and lower coefficient of friction and worn rate value than pure polyimide under high vacuum. However, the coefficient of friction of composites increased and the worn rate value decreased after ultraviolet or atomic oxygen irradiation, which slightly affected the tribological properties of CF-PI composites. The chemical composition of the composites changed after irradiation was inspected by X-ray photoelectron spectroscopy. Microstructure of the worn surfaces of the tested composites was investigated by scanning electron microscopy to reveal the wear mechanism.     

Study on the Tribological Properties of Carbon Fabric/Polyimide Composites Filled with SiC Nanoparticles

Carbon fabric reinforced thermoplastic polyimide composites have significant applications in the field of tribology. However, there are relatively few studies that have been focused on the investigation of these materials. In the present study, carbon fabric/polyimide (CF/PI) composites, reinforced further with SiC nanoparticles, were prepared by dip-coating and hot press molding methods. Rockwell hardness and flexural testing of the composites were conducted. The friction and wear behavior of the resulting carbon fabric composites were evaluated in a ring-on-block contact mode under dry sliding condition. The results showed that the SiC nanoparticles significantly improved the hardness and flexural strength when compared to the CF/PI composites without the SiC additions. The CF/PI composites reinforced with 5 vol% SiC nanoparticles demonstrated the most beneficial mechanical and tribological properties compared to the composites with greater and lesser SiC nanoparticles. Scanning electron microscopy (SEM) and optical microscopy (OM) were employed in order to study the mechanism of tribological behavior. A continuous and thin transfer film formed during the friction test of the composites led to a significant improvement of the tribological properties.     

Tribological behaviors of lanthanum-based phosphonate 3-aminopropyltriethoxysilane self-assembled films

Lanthanum-based thin films deposited on the phosphonate 3-aminopropyltriethoxysilane (APTES) self-assembled monolayer (SAM) were prepared on the hydroxylated glass substrate by a self-assembling process from specially formulated solution. Chemical compositions of the films and chemical state of the elements were detected by X-ray photoelectron spectrometry (XPS). The thickness of the films was determined with an ellipsometer, while the morphologies of the original and worn surfaces of the samples were analyzed by means of atomic force microscopy (AFM) and scanning electron microscopy (SEM), respectively. The tribological properties of the films sliding against GCr15 steel ball were evaluated on a UMT-2MT reciprocating friction and wear tester. As the results, the target film was obtained and reaction may have taken place between the film and the glass substrate. The tribological results show that lanthanum-based thin films are superior in reducing friction and resisting wear compared with APTES-SAM and phosphorylated APTES-SAM. SEM observation of the morphologies of worn surfaces indicates that the wear of APTES-SAM and the phosphorylated APTES-SAM is characteristic of brittle fracture and severe abrasion. Differently, slight abrasion and micro-crack dominate the wear of lanthanum-based thin films. The superior friction reduction and wear resistance of lanthanum-based thin films are attributed to the enhanced load-carrying capacity of the inorganic lanthanum particles in the lanthanum-based thin films as well as good adhesion of the films to the substrate.