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Transmission electron microscopy study of rapid thermally annealed Pd/Ge contacts on IN0.53Ga0.47As
(1996)
Single walled carbon nanotubes (SWNT) have been produced in an electric arc discharge by using a graphite rod as anode which is filled with a powder mixture of graphite and metallic catalysts like nickel and yttrium. The soot material containing approximately a third of SWNT was collected from the cathode region as a soft, voluminous material. The main by-products in this process are amorphous carbon and graphitic nanoparticles which have to be removed by an appropriate purification process. The as-produced soot material was purified by gas phase oxidation in air at 355 °C. The oxidation of amorphous carbon in air is advantageous against wet chemical methods because it is better controllable. Thermogravimetric analysis and electron microscopy were used to investigate the oxidation behavior of the different kinds of carbon. Oxidation of SWNT and amorphous carbon occurs simultaneously even at moderate temperatures, whereas amorphous carbon is more rapidly oxidized than SWNT. For optimizing the purification procedure by gas phase oxidation, kinetic studies were used to determine the oxidation time for each component in the soot at a given temperature. So it is possible to remove the amorphous carbon quantitatively with minimal losses of SWNT. But it was found that graphitic nanoparticles have the highest stability against oxidation and could therefore not be quantitatively removed by this method without the complete destruction of SWNT. Therefore, the electric arc discharge process has to be a controlled process for minimum production of graphitic nanoparticles to obtain a material with a high content of SWNT.
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.
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.
The transformation of doped or seeded pseudoboehmite to corundum was studied by combining thermal analysis, X-ray diffraction, transmission electron microscopy, and electron paramagnetic resonance spectroscopy. The temperature of phase transformation to corundum was lowered by about 130 °C when Fe3+ or corundum seeds were added to the sols. Action of Fe3+ ions depends on the actual degree of thermally induced transformation of pseudoboehmite via transition aluminas to corundum and the ability of these alumina phases to incorporate Fe3+ ions. These ions tend to aggregate with increasing iron concentration of the alumina phases and can work as nucleation centers. Small (not, vert, similar20 nm) corundum particles act as active nucleation sites whereas larger grains (200400 nm) also present in the samples are less effective. For the first time trapping and stabilization of NO2 molecules in transition aluminas formed by a solgel route was shown.
The microstructures of two samples of a Zr(C,N) coating on steel, which unexpectedly differed in their tribological properties, were investigated by analytical transmission electron microscopy. The samples were produced by a cathodic arc evaporation process in two commercial coating devices under similar coating conditions with the exception of the number of Zr targets.
The source of the differing tribological properties of the samples was detected by analytical transmission electron microscopy (TEM) methods energy-dispersive X-ray spectroscopy (EDX), energy filtering TEM (EFTEM), electron diffraction, high resolution electron microscopy, and high angel annular dark field. The TEM preparation and the results of the TEM investigations are shown in detail. The origin of the unexpected behavior was determined to be a nano-scale multilayer structure that existed only in the tribologically superior specimen. EDX and EFTEM investigations indicated enrichment in oxygen at the interface between coating and steel substrate in the tribologically inferior sample. Findings of the microstructural configuration were obtained by taking a closer look at the structure and comparing the results of the several analytical TEM techniques. This allows the allocation of the concentration fluctuations in N, C, and Zr to the two thickness fractions of the nano multilayers and a local correlation of the identified minority phase Zr3(C,N)4 to the higher N content in the narrower type of the multilayer fraction of the sample with the excellent tribological properties. The minority phase Zr3(C,N)4 is randomly distributed in the sample with the defective tribological properties.
Coating conditions are not topic of this work, but after discussion of the TEM results, the fact that one of the coating devices worked with one Zr target and the other one with two, could be identified as cause for the formation of the nano multilayer structure in the sample with the superior tribological properties.