Vacuum annealing phenomena in ultrathin TiDy/Pd bi-layer films evaporated on Si(100) as studied by TEM and XPS

W.F. Lisowski, Enrico G. Keim

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Using a combination of TEM and XPS, we made an analysis of the complex high-temperature annealing effect on ultrathin titanium deuteride (TiDy) films evaporated on a Si(100) substrate and covered by an ultrathin palladium layer. Both the preparation and annealing of the TiDy/Pd bi-layer films were performed in situ under UHV conditions. 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 TiDy phase. 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. Segregation of Ti at the Pd top layer surface was found to occur by means of angle-resolved XPS (ARXPS) and the EFTEM analyses. Selected area diffraction (SAD) and XPS provided evidence for the formation of a new PdTi2 bimetallic phase within the top region of the annealed film. Moreover, these techniques allowed to detect the initial stages of TiSi phase formation within the film–substrate interlayer.
Original languageUndefined
Pages (from-to)2804-8
Number of pages2797
JournalAnalytical and bioanalytical chemistry
Issue number8
Publication statusPublished - 2010


  • IR-104590
  • METIS-272526

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