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Organisationseinheit der BAM
The sliding behavior of an amorphous silica sample between two rigid surfaces is in the focus of the present paper. Molecular Dynamics using a classical Tersoff’s potential and a recently developed ReaxFF potential was applied for simulating sliding within a thin film corresponding to a tribofilm formed from silica nanoparticles. The simulations were performed at different temperatures corresponding to moderate and severe tribological stressing conditions. Simulations with both potentials revealed the need of considering different temperatures in order to obtain a sound interpretation of experimental findings. The results show the striking differences between the two potentials not only in terms of magnitude of the resistance stress (about one order of magnitude) but also in terms of friction mechanisms. The expected smooth sliding regime under high temperature conditions was predicted by both simulations, although with Tersoff’s potential smooth sliding was obtained only at the highest temperature. On the other hand, at room temperature Tersoff-style calculations demonstrate stick-slip behavior, which corresponds qualitatively with our experimental findings. Nevertheless, comparison with a macroscopic coefficient of friction is not possible because simulated resistance stresses do not depend on the applied normal pressure.
A gray cast iron disc, which had been submitted to a heavy duty automotive brake test, was examined with energy filtered transmission electron microscopy. A graphite flake in a convenient angular position showed the shear interaction of graphite layers with the iron matrix in nano-scale resolution. Atomic layers of graphite were wedged into the ferritic bulk, allowing the entrance of oxygen and the subsequent formation of magnetite. The exfoliated few-layer graphene batches deformed heavily when forced into the matrix. When Raman spectra from the disc surface, which show distinctive carbonaceous bands, were compared with Raman spectra from graphite subjected to deformation in a shaker mill with different milling times, it could be seen that the shear stress on the brake surface was much more effective to induce disorder than the milling, where compressive and impact forces had been additionally exerted on the sample. During shear load the high anisotropy of elastic modulus in the graphite crystalline structure and the low adhesion between graphite basal planes allowed the exfoliation of wrinkled few-layer grapheme batches, causing the formation of more defect related Raman bands than the mechanical stress during high-energy milling.
Silica nanowires spanning 10 μm-deep trenches are fabricated from different types of silsesquioxane-based precursors by direct e-beam patterning on silicon followed by release through deep reactive ion etching. Nanowire aspect ratios as large as 150 are achieved with a critical dimension of about 50 nm and nearly rectangular cross-sections. In situ bending tests are carried out inside a scanning electron microscope, where the etch depth of 10 mm provides sufficient space for deformation. Silica NWs are indeed observed to exhibit superplastic behavior without fracture with deflections reaching the full etch depth, about two orders of magnitude larger than the nanowire thickness. A large-deformation elastic bending model is utilized for predicting the deviation from the elastic behavior. The results of forty different tests indicate a critical stress level of 0.1–0.4 GPa for the onset of plasticity. The study hints at the possibility of fabricating silica nanowires in a monolithic Fashion through direct e-beam patterning of silsesquioxane-based resins. The fabrication technology is compatible with semiconductor manufacturing and provides silica nanowires with a very good structural integrity.
Nanoscale building blocks impart added functionalities to microelectromechanical systems (MEMS). The integration of silicon nanowires with MEMS-based sensors leading to miniaturization with improved sensitivity and higher noise immunity is one example highlighting the advantages of this multiscale approach. The accelerated pace of research in this area gives rise to an urgent need for batch-compatible solutions for scaling to nano. To address this challenge, a monolithic fabrication approach of silicon nanowires with 10-lm-thick silicon-on-insulator (SOI) MEMS is developed in this work. A two-step Si etching approach is adopted, where the first step creates a shallow surface protrusion and the second step releases it in the form of a nanowire. It is during this second deep etching step that MEMS—with at least a 2-order-of-magnitude scale difference - is formed as well. The technique provides a pathway for preserving the lithographic resolution and transforming it into a very high mechanical precision in the assembly of micro- and nanoscales with an extreme topography. Validation of the success of integration is carried out via in situ actuation of MEMS inside an electron microscope loading the nanowire up to its fracture. The technique yields nanowires on the top surface of MEMS, thereby providing ease of access for the purposes of carrying out surface processes such as doping and contact formation as well as in situ observation. As the first study demonstrating such monolithic integration in thick SOI, the work presents a pathway for scaling down to nano for future MEMS combining multiple scales.
The primary crystallite size of titania powder relates to its properties in a number of applications. Transmission electron microscopy was used in this interlaboratory comparison (ILC) to measure primary crystallite size and shape distributions for a commercial aggregated titania powder. Data of four size descriptors and two shape descriptors were evaluated across nine laboratories. Data repeatability and reproducibility was evaluated by analysis of variance. One-third of the laboratory pairs had similar size descriptor data, but 83% of the pairs had similar aspect ratio data. Scale descriptor distributions were generally unimodal and were well-described by lognormal reference models. Shape descriptor distributions were multi-modal but data visualization plots demonstrated that the Weibull distribution was preferred to the normal distribution. For the equivalent circular diameter size descriptor, measurement uncertainties of the lognormal distribution scale and width parameters were 9.5% and 22%, respectively. For the aspect ratio shape descriptor, the measurement uncertainties of the Weibull distribution scale and width parameters were 7.0% and 26%, respectively. Both measurement uncertainty estimates and data visualizations should be used to analyze size and shape distributions of particles on the nanoscale.
Copper, magnetite and graphite particles were mixed in order to observe their impact on the coefficient of friction (CoF) during pin-on-disc tests and on the tribofilm formation after testing. Pure magnetite powder provided a value of CoF of 0.4. Magnetite-copper mixtures tested at 400 °C revealed lower CoF values (~0.4) than those at room temperature (~0.6). Magnetite-graphite and magnetite-graphite-copper mixtures presented lower CoF values (~0.3). All systems formed a magnetite-based tribofilm and patches of metallic copper were found on the tribosurfaces of the mixtures containing copper. Carbon layers and graphite nanoinclusions were observed in the graphite mixtures. The incorporation of zirconia particles, a by-product of ball milling mixing, prevented the selective transfer of graphite and copper to the tribosurfaces of some of the samples.
The method of movable cellular automata (MCA) was applied to simulate the stress-strain behavior of a nano composite consisting of an epoxy matrix and 6 vol. % silica nano particles. The size of the elements used for modelling was fixed at 10 nm, corresponding approximately to the diameter of the filler particles. Since not only the stress-strain response of the two constituents but also debonding of neighboring particles and granular flow was taken into account, plastic deformation as well as crack initiation and propagation could be simulated with the model. Modelling results were compared with tensile test results of both, pure epoxy as well as the epoxy-6 vol. % SiO2 composite. Since assuming bulk properties of the two constituents did not yield satisfactory results, slight modifications of the nanoparticle response functions and nanostructures were tested numerically. Finally, it was observed that only the assumption of slightly increased strength properties of the epoxy yielded good correlation between experimental and modelling results. This was attributed to an increased cross linking of the epoxy caused by the presence of silica nano particles.
This review article comprises of three parts. Firstly, reports of brake manufacturers on the beneficial impact of solid lubricants for pad formulations are surveyed. Secondly, since tribofilms were identified to play a crucial role in friction stabilization and wear reduction, the knowledge about tribofilm structures formed during automotive braking was reviewed comprehensively. Finally, a model for simulating the sliding behavior of tribofilms is suggested and a review on modelling efforts with different model structures related to real tribofilms will be presented. Although the variety of friction composites involved in commercial brake systems is very broad, striking similarities were observed in respect to tribofilm nanostructures. Thus a generalization of the tribofilm nanostructure is suggested and prerequisites for smooth sliding performance and minimal wear rates have been identified. A minimum of 13 vol.% of soft inclusions embedded in an iron oxide based tribofilm is crucial for obtaining the desired properties. As long as the solid lubricants or their reaction products are softer than magnetite, the main constituent of the tribofilm, the model predicts smooth sliding and a minimum of wear.
Excellent tribological properties of an advanced polymer matrix composite were obtained by a combination of micro- and nano-sized fillers. Surface features and the nanostructure of tribofilms were characterized by advanced microscopic techniques, and correlated with the macroscopic behavior in terms of wear rate and friction evolution. A model based on movable cellular automata was applied for obtaining a better understanding of the sliding behavior of the nanostructured tribofilms. The failure of the conventional composite without silica nanoparticles could be attributed to severe oxidational wear after degradation of an initially formed polymer transfer film. The hybrid composite preserves its antiwear and antifriction properties because flash temperatures at micron-sized carbon fibers, lead to polymer degradation and subsequent release of nanoparticles. It has been shown that the released particles are mixed with other wear products and form stable films at the disc surface thus preventing further severe oxidational wear. Furthermore, the released wear product also is embedding carbon fibers at the composite surface thus preventing fiber fragmentation and subsequent third body abrasion. With nanoscale modelling we were able to show that low friction and wear can be expected if the nanostructured silica films contain at least 10 vol.% of a soft ingredient.