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Paper des Monats
- ja (1)
In this work, thin iron doped tin oxide layers (3–6 nm) were investigated with regard to gas sensitivity by means of surface plasmon resonance (SPR) effect with ellipsometric readout. The experimental set-up was a Kretschmann configuration with gold as metal layer. The sensor system was exposed to different concentrations of methane in the low ppm range and the sensor response of an uncoated gold layer compared to a gold layer coated with iron doped tin oxide. The additional layer effects stability with regard to drift behavior of the sensor and an increase in sensitivity. Furthermore, the sensor is able to detect the toxic gas carbon monoxide in low concentration range (down to 0.5 ppm). The thin layers were investigated by X-ray photoelectron spectroscopy, secondary electron microscopy and spectroscopic ellipsometry. The possible mechanisms taking place on the surface are discussed.
A gas sensor system based on the surface plasmon resonance (SPR) effect in a 44 nm Au layer was studied. The usability of this sensor system was investigated for several analyte gases and gas mixtures which are interesting due to their flammability, toxicity or greenhouse effect. The SPR effect of gold was measured in nitrogen and compared with the gaseous alkane series which caused a shift of the position of the SPR effect. For in situ measurements, the phase shift Δ at the SPR angle (ψ minimum) in the analyte gas mixtures was measured for investigated gases in comparison with nitrogen. With this method, detection limits of different gases could be determined, which lie in a range interesting for safety engineering. Furthermore the aging effect of the gold layers which leads to loss in sensitivity of the sensor was investigated.
An ellipsometric gas sensor based on the surface Plasmon resonance (SPR) effect of ~ 43 nm thick gold layers was investigated. To protect the gold layer from contamination and to improve the detection limits, the gold layers were top-coated with 5–6 nm thick layers of organic a-C:H or with inorganic metal oxides TiO2 or ZrO2. The additional layers increased the long-term stability, whereas the metal oxide layers protect better than a-C:H. Furthermore, the additional layers decreased the detection limits by one order of magnitude in case of a-C:H and two orders of magnitude in case of the oxides. It could be shown that the detection limits also depend on the kind of preparation (sol–gel process or physical vapour deposition) of the additional layers.
The thermodynamic behavior of thin PVME films including the irreversible adsorbed layer on the substrate is investigated. In a first step, the growth kinetics of the adsorbed layer was studied combining a leaching technique and atomic force microscopy. Further, it was shown that there is a critical initial film thickness for the formation of a surface-filling adsorbed layer. Additionally, spectroscopic ellipsometry measurements were carried out to investigate the influence of the adsorbed layer on the glass transition temperature of the thin films. For 30 nm films and below, the influence of the adsorbed layer percolates strongly to the bulk-like layer of the film. Finally, the molecular dynamics of the adsorbed layer was studied by broadband dielectric spectroscopy, employing nanostructured-electrode systems. One process was revealed, which was assigned either to molecular fluctuations taking place in a loosely-bounded the part of the adsorbed layer, or to the desorption/adsorption of segments at the substrate.
The discussions on the nanoconfinement effect on the glass transition and glassy dynamics phenomena have yielded many open questions. Here, the thickness dependence of the thermal glass transition temperature of thin films of a PVME/PS blend is investigated by ellipsometry. Its thickness dependence was compared to that of the dynamic glass transition (measured by specific heat spectroscopy), and the deduced Vogel temperature (T0). While and T0 showed a monotonous increase, with decreasing the film thickness, the dynamic glass transition temperature () measured at a finite frequency showed a non-monotonous dependence that peaks at 30 nm. This was discussed by assuming different cooperativity length scales at these temperatures, which have different sensitivities to composition and thickness. This non-monotonous thickness dependence of disappears for frequencies characteristic for T0. Further analysis of the fragility parameter, showed a change in the glassy dynamics from strong to fragile, with decreasing film thickness.
The glass transition behavior of thin films of poly(bisphenol A carbonate) (PBAC) was studied employing ellipsometry. The glass transition temperature increases with the reduction of the film thickness. This result is attributed to the formation of an adsorbed layer with a reduced mobility compared to bulk PBAC. Therefore, for the first time, the growth kinetics of the adsorbed layer of PBAC was investigated, prepared by leaching samples from a 200 nm thin film which were annealed for several times at three different temperatures. The thickness of each prepared adsorbed layer was measured by multiple scans using atomic force microscopy (AFM). Additionally, an unannealed sample was measured. Comparison of the measurements of the unannealed and the annealed samples provides proof of a pre-growth regime for all annealing temperatures which was not observed for other polymers. For the lowest annealing temperature after the pre-growth stage only a growth regime with a linear time dependence is observed. For higher annealing temperatures the growth kinetics changes from a linear to a logarithmic growth regime at a critical time. At the longest annealing times the films showed signs of dewetting where segments of the adsorbed film were removed from the substrate (dewetting by desorption). The dependence of the surface roughness of the PBAC surface on annealing time also confirmed that the films annealed at highest temperatures for the longest times desorbed from the substrate.