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Organisationseinheit der BAM
Eingeladener Vortrag
- nein (6)
Optical and electron metallography have been used to investigate the development of different microstructures in Armco Fe after rolling reductions between 0 and 90%. Simultaneously, the orientation distribution functions have been calculated from pole figures obtained by X-ray diffraction. Different stages of texture development could be assigned to typical microstructures. Strain inhomogeneities, such as microbands and shear bands, caused some broadening of the texture and a slight deviation of one skeleton line from the predicted fibre texture component. The decomposition of orientations near {111} < 121 > , and the strengthening of {211} < 011 > after high rolling reductions, was not due to mechanical twinning but could rather be explained by assuming {211} < 111 > slip. 30 ref.--AA
The formation of a third body layer on a conventional friction material during braking tests was studied in some detail using TEM, SEM, and X-ray photoelectron spectroscopy (XPS) techniques. Plate shaped micro-contact areas representing a compositional mix of all components of the tribocouple and exhibiting a nanocry stalline microstructure were identified after a run-in period.
Die volle Leistung einer auf Reibung basierenden Bremse wird erst nach einem Einlaufvorgang erreicht. Dieser ist notwendig, um auf Belag und Scheibe eine sogenannte Reibschicht aufzubauen. Da diese Zwischenschicht das Reibungsverhalten des Systems maßgeblich bestimmt, ist es wichtig, sich Klarheit über ihre chemische Zusammensetzung, Mikrostruktur und die daraus resultierenden Eigenschaften zu verschaffen.
Als Basismaterial diente ein phenolharzgebundener Belag Jurid 57-62, der mit verschiedenen Parametern (Flächenpressung und Umdrehungsgeschwindigkeit) gegen eine Stahlscheibe getestet wurde. Es wurden Dauerbremsungen von jeweils einer Stunde bzw. bis zu einem maximalen Belagverschleiß von 1 mm simuliert, wobei die Entwicklung der Reibzahl und die Oberflächentemperatur der Scheibe registriert wurde.
Zur Analyse der Reibschichten auf dem Bremsbelag wurden mehrere Methoden parallel angewandt. So wurden Verschleißpartikel, die aus der Reibschicht stammen, gesammelt bzw. abgekratzt und nach Dispergieren auf Kohlefolien direkt im Transmissionselektronenmikros-kop (TEM) untersucht. Ferner wurden von einigen ausgesuchten Belagproben Mikrotom-schnitte sowie dünne Querschnittsfolien für die TEM-Untersuchung präpariert, um den Verbund Reibschicht-Grundmaterial darstellen zu können. Als Ergänzung wurden ferner oberflächenmorphologische und –analytische Verfahren wie REM/EDX und ESCA eingesetzt.
Die Ergebnisse deuten darauf hin, dass die Reibschicht nanokristallin ist, und dass fast alle anorganischen Bestandteile des Bremsbelags sowie Eisenoxid von der Bremsscheibe in sehr fein verteilter Form vorliegen. Bei Belägen ohne Metallanteil bildet eine Barium-Eisen-Sulfatphase offenbar die Grundstruktur der Reibschicht, während auf eisenhaltigen Belägen Eisenoxid dominierend ist. Die nanokristalline Mikrostruktur entsteht, ähnlich wie beim mechanischen Legieren, durch einen Mahlvorgang von Verschleißpartikeln zwischen den Reibpartnern. Bei Überlastung des Belags tritt Zersetzung der Polymer-Bindephase ein, was zu einem raschen Anstieg der Verschleißrate führt.
A rather new tool, the focused ion beam (FIB) technique, was used to characterise superficial layers at micro-contact areas of a commercial brake pad. The friction material was a polymer matrix composite (PMC) with approximately 50% metal content (semi-metallic) and the counter part was a cast iron rotor. Though the contact areas were not visible as topographic features, they could be identified with the aid of their increased secondary electron emission during FIB-scanning of the surface after tribological activation. Target preparation of micron-sized cross-sections with the FIB enabled the study of superficial layers at predetermined sites at high magnification.
Depending on the constituent of the pad, one, two or three layers were identified. The three layer structure comprised: (i) a 100 nm thick friction film containing nanocrystalline metal oxides and an amorphous phase which was enriched with sulphur, (ii) a nanocrystalline friction layer of compacted wear debris accommodating surface roughness and (iii) a severely deformed layer if the supporting constituent was a metal particle. Though the majority of loose wear particles was iron oxide, the friction film which adhered tightly to the pad surface contained a large amount of copper and sulphur, whereas zinc was transferred to the cast iron rotor.
The surfaces of a brake pad and rotor were investigated after a run-in period during which a stable coefficient of friction had developed. The Focused Ion Beam Technique (FIB) was used to reveal tribologically induced surface films and for cross-sectional preparation of superficial layers. Additional information was obtained by TEM/EDS of thin lamellae prepared with the FIB and by surface analytical methods (GDOS, XPS and RS). Microscopic contact areas of the pad showed bright contrast in Scanning Ion Microscopy (SIM). This was attributed to severe plastic deformation finally leading to a nanocrystalline microstructure. Metallic particles of the pad, the so-called primary contact areas, were mostly covered with a smooth oxide layer of less than 1 µm thickness. Above this layer a thin (100 nm) partly amorphous film was often observed. The film was not only restricted to the metal particles, but also spread over adjacent regions, suggesting that secondary plateaus had formed. Similar layers and films, although with slightly different composition and structure, were also observed at the surface of the rotor.
Patches of white etching layers on rail surfaces were investigated using sophisticated techniques like cross-sectional transmission electron microscopy (XTEM) and synchroton X-ray diffraction. Optical microscopy failed to resolve the microstructure, but in the TEM submicron grains with high dislocation densities and occasional twins, which are characteristic features of high carbon martensite, were observed. The martensitic structure was confirmed by evaluation of synchroton X-ray diffraction line profiles. The latter technique also allowed to determine dislocation densities of the order of 1012 cm-2 and residual compressive stresses of about 200 MPa.
Cross-sectional transmission electron microscopy, in combination with energy dispersive X-ray spectroscopy and focused beam microdiffraction, was applied to study the solid-state reactions taking place during contact formation of the system Ge(115 nm)/Pd(50 nm)In0.53Ga0.47As. In order to get information about the sequence of the different processes, rapid thermal, annealing experiments in the range 225400 °C were performed. The following features were observed: at 225 °C Pd reacted with the substrate forming the quaternary phase PdxIn0.53Ga0.47As (x 4), and with the Ge-layer forming mainly PdGe and Pd2Ge. Between PdxIn0.53Ga0.47As and In0.53Ga0.47As, a 5 nm thick amorphous Pd-In-Ga-As layer remained, indicating that the first reaction step was solid-state amorphization. After annealing at 350 °C, PdxIn0.53Ga0.47As disappeared and regrowth of In0.53Ga0.47As occured. Finally, at 400 °C, residual Ge from the amorphous top layer diffused to the interface and grew epitaxially on the regrown In0.53Ga0.47As, thus separating the IIIV compound semiconductor from the Pd-Ge reaction products. The interface remained flat, while only about 10 nm of the active In0.53Ga0.47As layer had been modified during the annealing processes.
Copper is a major ingredient in friction materials used for automotive braking. The purpose of this study was to find out how copper contributes to good brake performance properties in addition to providing good thermal conductivity. Microstructural investigations of copper chips at the surfaces of brake pads revealed a zone of severe plastic deformation which provides high hardness, but there is also evidence of recrystallized copper nano-particles which are incorporated into friction layers as soft ingredient once detached from the pad surface. Thus copper seems to play a dual role, firstly as reinforcing element of the brake pad providing primary contact sites, and secondly as solid lubricant by contributing to the formation of a layer of granular material providing velocity accommodation between the rotating disc and fixed pad. Confirmation for this hypothesis was obtained by modelling contact sites on the nanometre scale with the method of movable cellular automata. Results show both, the similarity of steel fibres and copper macro-particles in respect to providing primary contact sites, as well as similar sliding behaviours of friction layers containing either copper or graphite as soft inclusions. Furthermore, it is shown that not only material properties, but also the concentration of solid lubricant particles in the friction layers, determine conditions for friction force stabilization and smooth sliding behaviour.
The unique nanostructure formed during severe as well as moderate braking on the surface of brake discs was investigated by conventional and analytical Transmission Electron Microscopy. In both cases nanocrystalline magnetite mixed with carbon nanoinclusions and minor amounts of other pad constituents were identified. On the basis of these observations the friction performance of a single micro-contact was simulated with the method of Movable Cellular Automata. Inspite of a simplified nanostructure which was examined in two dimensions only, the calculated mean coefficient of friction fitted well to the value usually demanded for automotive braking. Furthermore, the model predicts that oxide films without soft nanoinclusions are not capable of providing smooth velocity accommodation at the pad–disc interface and thus lead to unstable friction behaviour.
Different, partly complementary and partly redundant characterization methods were applied to study the transition of magnetite, graphite and MoS2 powders to mechanically alloyed nanostructures. The applied methods were: Transmission electron microscopy (TEM), Mössbauer spectroscopy (MS), Raman spectroscopy (RS), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The main objective was to prepare a model material providing the essential features of a typical tribofilm forming during automotive braking, and to assess the impact of different constituents on sliding behaviour and friction level. Irrespective of the initial grain size, the raw materials were transferred to a nanocrystalline structure and mixed on a nanoscopic scale during high energy ball milling. Whereas magnetite remained almost unchanged, graphite and molybdenum disulphide were transformed to a nanocrystalline and highly disordered structure. The observed increase of the coefficient of friction was attributed to a loss of lubricity of the latter ingredient due to this transformation and subsequent oxidation.
The sliding behaviors of two simplified tribofilms with amorphous structure consisting either of SiO₂ molecules or C atoms were simulated by molecular dynamics modeling. The objective was to identify mechanisms explaining the experimentally observed lubricating properties of the two amorphous films. The impacts of layer thickness, normal pressure, temperature and different substrate materials were studied systematically, while the sliding velocity was kept constant at 30 m/s. While the layer thickness was not critical, all the other parameters showed special effects under certain conditions. Normal pressure impeded void formation and could even eliminate voids if applied at high temperature. Stick-slip sliding was changed to smooth sliding at high temperature due to void healing. Considering the carbon film, high friction forces and shearing of the entire film was observed with diamond substrates, whereas interface sliding at low friction forces and an amorphous layer of iron mixed with carbon was observed if the supporting substrates consisted of α-Fe. Both films show a decrease of friction forces and smooth sliding behavior at elevated temperature, corresponding well to the tribological behavior of and advanced nanocomposite sliding against a steel disc under severe stressing conditions when high flash temperatures can be expected.
XTEM and TFXRD investigations of ohmic Ti/Al/Ti/Au/WSiN contacts on AlGaN/GaN HFET layer systems
(2002)
The microstructural features of the high-temperature-stable ohmic contact system Ti/Al/Ti/Au/WSiN on AlGaN/GaN were investigated using analytical transmission electron microscopy and thin film x-ray diffraction. For two typical rapid thermal annealing steps at 750 °C (non-ohmic behaviour) and 850 °C (ohmic behaviour) the intermetallic phases at the metal-semiconductor interface are presented. Increased annealing leads to the transformation of an Al2Au-AlAuTi phase mixture to a mixture of Al2Au-Al3Au8 phases and the formation of Ti-Al-nitride layers at the interfaces. In light of these results the electrical contact properties are discussed.