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X-ray photoelectron spectroscopy (XPS) and cross-sectional transmission electron microscopy (XTEM) were used to study the formation of AlN films by N+2 ion implantation of aluminium at energies of 3 keV and 100 keV. In both cases, a two-stage mechanism was found, comprising first the oriented precipitation of small particles of the hexagonal AlN-phase, followed by growth and coalescence finally forming a continuous AlN-layer while increasing the implantation dose from 1×1017 cm-2 to 2×1017 cm-2. The results of both methods are in excellent agreement and furthermore provide complementary information concerning chemical composition and binding energies as well as microstructural details.
Transmission electron microscopy study of rapid thermally annealed Pd/Ge contacts on IN0.53Ga0.47As
(1996)
This work focuses on surface changes induced by repeated brake applications and tries to provide explanations, how such material modifications might affect friction and wear properties of automotive disc brakes. Surface films were investigated locally by transmission electron microscopy (TEM) after having prepared thin cross-sections with a focused ion beam instrument (FIB). Since the observed friction layers revealed a nanocrystalline structure, modelling with the method of movable cellular automata (MCA) was performed by assuming an array of linked nanometer-sized particles. In spite of complicated material combinations at the pad surface, two very characteristic features were always observed at both the pad and disc surface, namely a steel constituenteither ferritic (pad) or pearlitic (disc), partly covered with patches of nanocrystalline iron oxide, on a zone of severe plastic deformation with fragmented grain structure. When using an automata size of 10 nm, reasonable values for the mean coefficient of friction (COF) were obtained, namely 0.35 and 0.85 for oxide-on-oxide and metal-on-metal contacts, respectively. Immediately after brake application mass-mixing and bond-breaking was observed within a narrow zone at both surfaces.
Ti/TiN multilayer coatings with multilayer periods in the range 550 nm and a final thickness of 2 µm were deposited on steel substrates by cyclic modulation of nitrogen gas flow into the chamber of a PVD sputtering device. Coating characterization was performed by cross-sectional transmission electron microscopy, glancing-angle X-ray diffraction and instrumental indentation testing. Individual a-titanium and titanium nitride layers were always observed, although for the finer microstructures, the TiN layers were thicker than the Ti layers by a factor three. The plastic hardness of the films increased steadily with decreasing layer spacing, following a HallPetch relationship. Finally, a hardness value of 42 GPa was reached, which is similar to that of a thick TiN monolayer, prepared under the same coating conditions.
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.
TEM-Untersuchungen der Randzonenschädigung von Aluminiumoxidkeramiken nach Schleifbearbeitung
(1996)
Es werden elektronenmikroskopische Untersuchungsergebnisse an Al2O3-Keramiken, die verschiedenen Oberflächenbearbeitungsverfahren unterworfen wurden, vorgestellt.
Die Untersuchungen dienen dem Ziel der Optimierung der Oberflächenbearbeitung von keramischen Werkstoffen, wobei der Einfluß leistungsfähiger Bearbeitungsverfahren auf die Ausbildung möglichst schädigungsarmer Oberflächenschichten, die keinen negativen Einfluß auf Festigkeitskennwerte aufweisen, betrachtet wird.
Die Wirkung verschiedener Schleif- und Polierprozesse auf Oberflächenveränderungen bearbeiteter Werkstücke wird dargestellt. Es wurde sowohl die Mikrostruktur der geschädigten Randzonenschicht als auch die des unbeeinflußten Grundmaterials mit elektronenmikroskopischen Methoden charakterisiert. Die verschiedenen Schädigungsstadien gestatten eine Einschätzung der Stärke des Störungseintrages in das Material durch verschiedene Schleif- und Polierprozesse.
Different wear-resistant coatings produced by physical vapour deposition (PVD) were characterized with the aid of cross-sectional transmission electron microscopy (XTEM). All coating systems were optimized by the producers and exhibited good properties with respect to their special applications. The microstructure, texture and chemical composition of binary and ternary systems produced by the arc process [TiN, CrN, Cr2N (Ti, Cr)N on steel substrates] and magnetron sputtering process [TiN, CrN on steel substrates, (Ti, Al)N on Si-substrate] were investigated. All coatings had a more or less columnar microstructure, which was interrupted by interlayers in some cases. Whereas arc coatings always did show some kind of substrate modification, the latter was not observed after magnetron sputtering. Electron diffraction normally revealed a mono-phase fcc structure, except at sites very near to the interface. Only for the systems CrN and (Ti, Cr)N were different additional phases observed at low nitrogen partial pressures.
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.