Anal Bioanal Chem. 2007 Nov;389(5):1489-98. doi: 10.1007/s00216-007-1594-3. Epub 2007 Sep 22.

Microstructural and chemical transformation of thin Ti/Pd and TiDy/Pd bilayer films induced by vacuum annealing.

Analytical and bioanalytical chemistry

W Lisowski, E G Keim, Z Kaszkur, A H J van den Berg, M A Smithers

PMID: 17891384 DOI: 10.1007/s00216-007-1594-3

Abstract

Using a combination of scanning electron microscopy, transmission electron microscopy (TEM), X-ray diffraction and X-ray photoelectron spectroscopy (XPS), we made a comparative study of the high-temperature annealing impact on thin titanium deuteride (TiD(y)) films covered by an ultrathin Pd layer, and on Ti/Pd bilayer films. The bilayer films were prepared under ultrahigh vacuum conditions and were in situ annealed using the same annealing procedure. It was found that the surface and the bulk morphology of both films undergo different annealing-induced transformations, leading to an extensive intermixing between the Ti and Pd layers and the formation of a new PdTi(2) bimetallic phase. Energy-filtered TEM imaging and energy-dispersive X-ray spectrometry analysis, as well as XPS depth profiling all provided evidence of a different distribution of Pd and Ti in the annealed TiD(y)/Pd film compared with the annealed Ti/Pd film. Our results show that thermal decomposition of TiD(y), as a consequence of annealing the TiD(y)/Pd film, modifies the intermixing process, thereby promoting Ti diffusion into the Pd-rich top layer of the TiD(y) film and thus providing a more likely path for the formation of the PdTi(2) phase than in an annealed Ti/Pd film.

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• Journal Article