TY - JOUR
T1 - Application of TEM and XPS in the interpretation of the kinetics of deuterium evolution from ultra TiD y/pd films evaporated on quartz
AU - Lisowski, W.
AU - Keim, E.G.
PY - 2009
Y1 - 2009
N2 - The kinetics of thermal evolution of deuterium from ultrathin TiD y /Pd bilayer films has been studied by means of thermal desorption mass spectrometry (TDMS). Using a combination of transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy, we made a study of the complex structural and chemical transformations of the TiD y /Pd film as a result of TDMS-induced evolution of deuterium and simultaneous annealing of this film. Both preparation and TDMS processing of the TiD y /Pd bilayer films were performed in situ under UHV conditions. It was found that the high-temperature TDMS processing of an ultrathin TiD y /Pd film, which was carried out in a relatively short time, leads to a significant film structure transformation. Energy-filtered TEM mapping of cross-section images and EDX analysis revealed extensive interdiffusion of Ti and Pd within the Ti–Pd bi-layer film. This process leads to a progressive change in chemical composition within the surface and subsurface area of the film during the TDMS processing. As the temperature of TDMS heating increases, segregation of Ti at the Pd top layer surface becomes significant. As a result, the kinetics of deuterium desorption is progressively changed during TDMS; at lower temperatures, the kinetics is limited by recombinative processes at the Pd surface, at temperatures beyond 500 K, it becomes dominated by interdiffusion of Ti into the Pd surface.
AB - The kinetics of thermal evolution of deuterium from ultrathin TiD y /Pd bilayer films has been studied by means of thermal desorption mass spectrometry (TDMS). Using a combination of transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy, we made a study of the complex structural and chemical transformations of the TiD y /Pd film as a result of TDMS-induced evolution of deuterium and simultaneous annealing of this film. Both preparation and TDMS processing of the TiD y /Pd bilayer films were performed in situ under UHV conditions. It was found that the high-temperature TDMS processing of an ultrathin TiD y /Pd film, which was carried out in a relatively short time, leads to a significant film structure transformation. Energy-filtered TEM mapping of cross-section images and EDX analysis revealed extensive interdiffusion of Ti and Pd within the Ti–Pd bi-layer film. This process leads to a progressive change in chemical composition within the surface and subsurface area of the film during the TDMS processing. As the temperature of TDMS heating increases, segregation of Ti at the Pd top layer surface becomes significant. As a result, the kinetics of deuterium desorption is progressively changed during TDMS; at lower temperatures, the kinetics is limited by recombinative processes at the Pd surface, at temperatures beyond 500 K, it becomes dominated by interdiffusion of Ti into the Pd surface.
U2 - 10.1007/s00216-009-2638-7
DO - 10.1007/s00216-009-2638-7
M3 - Article
SN - 1618-2642
VL - 393
SP - 1923
EP - 2642
JO - Analytical and bioanalytical chemistry
JF - Analytical and bioanalytical chemistry
IS - 8
ER -