TY - JOUR A1 - Wollschläger, Nicole A1 - Österle, Werner A1 - Häusler, Ines A1 - Stewart, M. T1 - Ga+ implantation in a PZT film during focused ion beam micro-machining N2 - The objective of the present work was to study the impact of Focused Ion Beam (FIB) machining parameters on the thickness of the damaged layer within a thin film PZT. Therefore, different Ga+- ion doses and ion energies were applied to a standard PZT film (80/20 lead zirconium titanate) under two beam incidence angles (90° and 1°). The thicknesses of the corresponding Ga+-implanted layers were then determined by cross-sectional TEM in combination with energy dispersive spectroscopic (EDS) line-scans and correlated with polarisation hysteresis loops. The results show a decrease of Ga+-implanted layer thickness with decreasing inclination angle, whereas ion energy and ion dose could be correlated with gallium concentration in the implanted layers.. Under the most unfavorable conditions the depth of the affected zone was 26 nm, it was only 2 nm for the most favorable conditions. KW - PZT KW - Focused ion beam KW - Gallium implantation KW - Polarisation-electric field loop PY - 2015 DO - https://doi.org/10.1002/pssc.201400096 SN - 1610-1634 SN - 1862-6351 SN - 1610-1642 VL - 12 IS - 3 SP - 314 EP - 317 PB - Wiley-VCH CY - Berlin AN - OPUS4-32872 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Österle, Werner A1 - Deutsch, Cornelius A1 - Gradt, Thomas A1 - Orts Gil, Guillermo A1 - Schneider, Thomas A1 - Dmitriev, A.I. T1 - Tribological screening tests for the selection of raw materials for automotive brake pad formulations N2 - A modified pin-on-disc test was applied to determine tribological properties of typical brake pad constituents. Ball-milling of these ingredients together with iron oxide and graphite provided model materials displaying the main features of real third bodies. Solid lubricants like graphite affected the friction and wear behaviour of Fe3O4 powders considerably whereas further addition of hard nanoparticles induced only minor effects. This was corroborated by comparison with modelling results. MoS2 played a dual role. Depending on special conditions, this ingredient either reduced or increased friction. The latter could be explained, after nanoscopic characterization, by oxidation and destruction of the wear-protecting tribofilm. KW - Brake pad formulation KW - Raw materials KW - Third body KW - Pin-on-disc test PY - 2014 DO - https://doi.org/10.1016/j.triboint.2014.01.017 SN - 0301-679X VL - 73 SP - 148 EP - 155 PB - Butterworth-Heinemann CY - Oxford AN - OPUS4-30221 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nikonov, A. Y.. A1 - Dmitriev, A. I. A1 - Österle, Werner T1 - Molecular dynamics study of slip mechanisms of nickel with amorphous-like Ni-P coating N2 - In the paper by using molecular dynamics method we investigate behavior of nickel-phosphorus compound in amorphous-like state under conditions of shear loading at the constant velocity. Samples with an amorphous layer of pure nickel and nickel-phosphorus compound were considered. The analysis showed that forces of shear resistance in the sample with an amorphous layer containing phosphorus in about 3 times less than the sample with a layer of pure nickel. Thus, it was shown that nickel-phosphorous coating in amorphous-like state may exhibit low friction properties, and, therefore, serve as the solid lubricant material. T2 - International Conference on Advanced Materials with Hierarchical Structure for New Technologies and Reliable Structures CY - Tomsk, Russia DA - 19.09.2016 KW - Local structural transformations KW - Lattice PY - 2016 DO - https://doi.org/10.1063/1.4966457 VL - 1783 SP - 020164-1 EP - 020164-4 AN - OPUS4-38932 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dmitriev, A. I. A1 - Österle, Werner T1 - Sliding simulation of automotive brake primary contact with variable amounts of copper and graphite nanoparticles N2 - Copper is one of the most important components in brake pads and its amount can reach up to 14%. In spite of a number of positive features copper usage in brake pad formulations has recently become the subject of considerable discussions, primarily due to concerns about potential risks related to environmental impacts of copper particles. So, for developing new pad formulations with possible replacements of copper content, it is very important to understand the functionality of copper additions to brake friction materials. In the paper theoretical investigation of the role of copper as a pad ingredient was carried out on the basis of modelling by the method of movable cellular automata (MCA). In the study the concentration of copper particles in a Fe3O4-matrix was varied. The sliding simulations were performed while assuming material properties at 500 degrees C in order to assess the beneficial role of copper during severe braking conditions corresponding to fading cycles during dynamometer testing. T2 - International Conference on Advanced Materials with Hierarchical Structure for New Technologies and Reliable Structures CY - Tomsk, Russia DA - 19.09.2016 KW - Polymer matrix composite KW - Silica nanoparticles KW - Friction KW - Wear PY - 2016 DO - https://doi.org/10.1063/1.4966337 VL - 1783 SP - 020044-1 EP - 020044-4 AN - OPUS4-38933 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rodrigues, A.C.P. A1 - Österle, Werner A1 - Gradt, Thomas A1 - Azevedo, César Roberto de Farias T1 - Impact of copper nanoparticles on tribofilm formation determined by pin-on-disc tests with powder supply: Addition of artificial third body consisting of Fe3O4, Cu and graphite N2 - 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. KW - Brake pad materials KW - Sliding friction KW - Transfer layer KW - Surface analysis KW - Model friction tests PY - 2017 DO - https://doi.org/10.1016/j.triboint.2017.02.014 SN - 0301-679X VL - 110 SP - 103 EP - 112 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-40104 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yilmaz, M. A1 - Wollschläger, Nicole A1 - Esfahani, M. N. A1 - Österle, Werner A1 - Leblebici, Y. A1 - Alaca, B. E. T1 - Superplastic behavior of silica nanowires obtained by direct patterning of silsesquioxane-based precursors N2 - 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. KW - Silica nanowires KW - HSQ KW - Superplasticity KW - In situ bending tests PY - 2017 DO - https://doi.org/10.1088/1361-6528/aa5b80 SN - 0957-4484 SN - 1361-6528 VL - 28 IS - 11 SP - Article 115302, 1 EP - 10 AN - OPUS4-39166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yilmaz, M. A1 - Kilinc, Y. A1 - Nadar, G. A1 - Tasdemir, Z. A1 - Wollschläger, Nicole A1 - Österle, Werner A1 - Leblebici, Y. A1 - Alaca, B. E. T1 - Top-down technique for scaling to nano in silicon MEMS N2 - 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. KW - Nanowires KW - Silicon KW - Top-down KW - MEMS PY - 2017 DO - https://doi.org/10.1116/1.4978047 SN - 1071-1023 VL - 35 IS - 2 SP - 022001-1 EP - 022001-7 PB - America Vacuum Society AN - OPUS4-39370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, G. A1 - Österle, Werner A1 - Jim, B. A1 - Häusler, Ines A1 - Hesse, Rene A1 - Wetzel, B. T1 - The role of surface topography in the evolving microstructure and functionality of tribofilms of an epoxy-based nanocomposite N2 - The topographic effect of steel counterface, finished by mechanical grinding with Ra ranging from 0.01 to 0.95 µm, on the structure and functionality of the tribofilm of a hybrid nanocomposite, i.e. epoxy matrix filled with monodisperse silica nanoparticles, carbon fibers and graphite, was systematically investigated. The nanostructure of the tribofilm was comprehensively characterized by using combined focused ion beam and transmission electron microscope analyses. It was identified that oxidation of the steel surface, release, compaction and tribosintering of silica nanoparticles and deposition of an epoxy-like degradation product as well as fragmentation of carbon fibers are main mechanisms determining the structure and functionality of the tribofilm. The size of roughness grooves determines the type and size class of wear particles to be trapped at the surface. An optimum groove size leading to a maximum of surface coverage with a nanostructured tribofilm formed mainly from released silica nanoparticles was identified. KW - hybrid nanocomposite KW - tribological performance KW - topographic effect KW - tribofilm KW - nanostructure PY - 2016 DO - https://doi.org/10.1016/j.wear.2016.06.012 VL - 364-365 SP - 48 EP - 56 PB - Elsevier B.V. AN - OPUS4-37937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Häusler, Ines A1 - Dörfel, Ilona A1 - Peplinski, Burkhard A1 - Dietrich, Paul A1 - Unger, Wolfgang A1 - Österle, Werner T1 - Comprehensive characterization of ball-milled powders simulating a tribofilm system N2 - A model system was used to simulate the properties of tribofilms which form during automotive braking. The model system was prepared by ball milling of a blend of 70 vol.% iron oxides, 15 vol.% molybdenum disulfide and 15 vol.% graphite. The resulting mixture was characterized by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and various transmission electron microscopic (TEM) methods, including energy dispersive X-ray spectroscopy (EDXS), high resolution investigations (HRTEM) with corresponding simulation of the HRTEM images, diffraction methods such as scanning nano-beam electron diffraction (SNBED) and selected area electron diffraction (SAED). It could be shown that the ball milling caused a reduction of the grain size of the initial components to the nanometer range. Sometimes even amorphization or partial break-down of the crystal structure was observed for MoS2 and graphite. Moreover, chemical reactions lead to a formation of surface coverings of the nanoparticles by amorphous material, molybdenum oxides, and iron sulfates as derived from XPS. KW - Tribofilm model system KW - Ball milling KW - X-ray powder diffraction KW - Transmission electron microscopy PY - 2016 DO - https://doi.org/10.1016/j.matchar.2015.11.024 SN - 1044-5803 SN - 1873-4189 VL - 111 SP - 183 EP - 192 PB - Elsevier CY - New York, NY AN - OPUS4-35051 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dmitriev, A.I. A1 - Österle, Werner A1 - Wetzel, B. A1 - Zhang, G. T1 - Mesoscale modeling of the mechanical and tribological behavior of a polymer matrix composite based on epoxy and 6 vol.% silica nanoparticles N2 - A model based on movable cellular automata (MCA) is described and applied for simulating the stress–strain and sliding behavior of a nanocomposite consisting of an epoxy matrix and 6 vol.% of homogeneously distributed silica nanoparticles. Tensile tests were used for verification of the model. It was realized that a slight modification of epoxy properties due to the addition of silica nanoparticles had to be taken into account in order to obtain good correlation between experimental and modeling results. On the other hand, sliding simulations revealed no susceptibility of results to slight modifications of matrix properties, but a significant impact of nanoparticles on the interface structure and smoothness of sliding mechanism. Furthermore, assuming both possibilities, bond breaking and rebinding of automata pairs, can explain different friction levels of polymer materials. KW - Nanocomposite KW - Stress–strain behavior KW - Movable cellular automata KW - Sliding simulation KW - Mechanically mixed layer KW - Coefficient of friction PY - 2015 DO - https://doi.org/10.1016/j.commatsci.2015.08.029 SN - 0927-0256 VL - 110 SP - 204 EP - 214 PB - Elsevier CY - Amsterdam AN - OPUS4-34013 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -