Antiferromagnetic NiO films used for pinning layers in spin valve systems were prepared by reactive sputtering from an NiO target with variation of the oxygen/argon mixture in the sputter gas. Using XPS depth profiling we investigated the NiO x overstoichiometry (x > 1) in the films that was found by other methods and the chemical changes in the films during annealing. A direct detection of Ni 3+ failed because of strong preferential sputtering with the formation of metallic Ni during sputtering. By means of factor analysis a qualitative description of the overstoichiometry is possible. Indirectly it could be shown that metallic Ni is already formed in the oxide layers during annealing. It can be concluded that the stability of the NiO x films decreases with increasing deviation from stoichiometry (x > 1).
Mechanical properties of sputtered AlCu(0.5 wt %) thin films, 0.2–2.0 μm thick, were determined by tensile testing. For comparison, tensile tests were also performed on bulk samples of the same composition. The films were deposited on thin polyimide foils. They were characterized with respect to the surface, microstructure, residual stress, and concentration of copper and oxygen. Stress-strain curves of the films were obtained by separating the force working on the polyimide foil from that working on the metal-polyimide compound. Young’s modulus of the films almost corresponded to the bulk value. Films with a thickness >1.5 μm broke by formation of macrocracks while thinner films showed formation of microcracks. The Hall–Petch model, additional strengthening by small grain size, and the role of grain boundary sliding for crack formation are discussed.
The stress evolution during and after dc magnetron sputter deposition of Cu thin films with thicknesses of 20 and 300 nm and deposited with a constant rate of 0.1nm∕s onto Si (100) substrates is studied for various sputtering pressures (0.05–6 Pa). The stress was determined by means of in situ wafer curvature measurements using an optical two-beam deflection method. To correlate the stress evolution with the microstructure development, microstructure investigations were performed by scanning electron microscopy, atomic force microscopy, and electron backscatter diffraction. The results show the transition from tensile to compressive stress with decreasing sputtering pressure at different stages of the deposition. The features of the stress evolution during the early stage of deposition can be ascribed to the Volmer–Weber mechanism. For thicker films, three regions of the sputtering pressure can be distinguished concerning their effect on the stress evolution. The transition from compressive to tensile stress was correlated with the evolution from a dense to an open microstructure and with increasing surface roughness by increasing sputtering pressure. The results of the stress and microstructure evolution are interpreted in the context of the mechanisms being discussed in the literature.
The electrical resistivity (semiconductor–metal transition), the thermoelectric power, and the magnetic susceptibility of well‐characterized VO2 monocrystals and powdered samples in the range of homogeneity were measured. The physical properties gave no hint of an extension of the range of homogeneity towards oxygen excess. An oxygen deficit (VO1.994) strongly influence the semiconductive properties of VO2 below the phase transition temperature, but hardly influences the metallic properties above the transition temperature. This behaviour may be explained by the formation of vanadium interstitial atoms and a rise in the concentration of mobile electrons connected with it. These results explain discrepancies in the data of the physical properties in literature, and show how the properties of VO2 can be purposefully changed.
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