Oxidation-induced stress evolutions in Ta thin films were investigated using ex situ microstructure analyses and in situ wafer curvature measurements. It was revealed that Ta thin films are oxidized to a crystalline TaO2 layer, which is subsequently oxidized to an amorphous tantalum pentoxide (a-Ta2O5) layer. Initial layered oxidation from Ta to TaO2 phases abruptly induces high compressive stress up to about 3.5 GPa with fast diffusion of oxygen through the Ta layer. Subsequently, it is followed by stress relaxation with the oxidation time, which is related to the slow oxidation from TaO2 to Ta2O5 phases. The initial compressive stress originates from the molar volume expansion during the layered formation of TaO2 from the Ta layer, while the relaxation of the compressive stresses is ascribed to the amorphous character of the a-Ta2O5 layer. According to Kissinger's analysis of the stress evolution during an isochronic heating process, the oxygen diffusion process through the a-Ta2O5 layer is the rate-controlling stage in the layered oxidation process of forming a a-Ta2O5/TaO2/Ta multilayer and has an activation energy of about 190.8 kJ/mol.
Substantial improvement of microvolume UV absorption spectrometry in sensitivity, robustness and ease of operation was achieved for routine biological applications. A unique microtubing-based absorption cell (208 μm internal diameter) featuring enhanced light transmission with a liquid core waveguide technique provided dramatically enhanced absorption sensitivity, proportional to the extended path length (50 mm, from the typical 1 mm), while robust measurement performance was attained by implementation of preventive measures against bubble trapping along the light path. For pBR322 plasmid DNA, absorbance at 260 nm was reliably measurable down to 0.1 ng/μl with repeatability typically 2–3% RSD. The detection limit was 0.03 ng/μl dsDNA, far lower than the current state-of-the-art ∼1 ng/μl. Sample consumption for each measurement was 2.4 μl. Automated operation implemented for the first time in microvolume spectrophotometry facilitated the ease in handling with small-volume biological samples.
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