Energy-filtered TEM (EFTEM) mapping of cross-section images and argon ion sputter depth profiling XPS analysis revealed both a broad intermixing between the Ti and Pd layers and an extensive inter-diffusion of Si from the substrate into the film bulk area. It was found that the surface and bulk morphology of the bi-layer film as well as that of the Si substrate material undergo a microstructural and chemical conversion after annealing and annealing-induced deuterium evolution from the TiD y phase. Both the preparation and annealing of the TiD y/Pd bi-layer films were performed in situ under UHV conditions. Using a combination of TEM and XPS, we made an analysis of the complex high-temperature annealing effect on ultrathin titanium deuteride (TiD y) films evaporated on a Si(100) substrate and covered by an ultrathin palladium layer.
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