Rod−coil diblock copolymers of 2-hydroxyethyl methacrylate (HEMA) with well-defined
oligofluorene initiator were synthesized using the atom transfer radical polymerization (ATRP) technique.
The resulting copolymers were characterized using spectroscopic (1H NMR, GPC), optical (UV, photoluminesence), and thermal (DSC) techniques. The incorporation of the initiator into the polymeric chain
was confirmed by spectroscopic methods, while strong evidence for microphase separation was obtained
both from DSC and AFM. A detailed AFM study of the surface morphology in thin films was performed
using rod−coil diblock copolymers having different flexible blocks, namely HEMA and polystyrene.
Common solvents for both rod and coil blocks were used as a function of the solutions concentration of
the diblock copolymers. By increasing the concentration of a selective solvent, formation of either islands,
a stringlike morphology, and honeycomblike structures was observed. The optical properties of the HEMA
copolymers from THF solution show no change in the emission spectra as we move from solution to the
solid state. However, when ethanol was used as a solvent, a red shift of 10 nm was observed going from
solution to the solid state, which is a strong indication for phase separation and organization of the diblock
copolymers in alcoholic solutions. Annealing of the copolymers at 160 °C for 30 min resulted in green
light emission due to the appearance of a new band at 535 nm in the case of OFPHM 6.0, while when
polystyrene was used as coil block in OFPS copolymer pure blue light is emitted even after this treatment.
A novel monomer incorporating the quinoline moiety as the side group was synthesized and polymerized by employing free radical as well as atom-transfer radical polymerization (ATRP) techniques. In the latter case, two different initiators were used, resulting in dibenzyloxy-or dimethylester-end-functionalized polyquinolines. All polymers were characterized primarily using 1 H NMR, gel permeation chromatography, UV-vis photoluminescence spectroscopy, and cyclic voltammetry. A systematic luminescence study was performed in different solvents and concentrations, showing that the optical properties of the newly synthesized polymers depend on both the solution's concentration and the ionic strength of the solvent. In addition, atomic force microscopy and scanning electron microscopy techniques also confirmed the close correlation between the film morphology and the solvent used for their preparation.
This paper demonstrates the results of the comparison of step-scan FT-IR photoacoustic spectroscopy with other established spectroscopic and microscopic techniques in the quantitative depth profile determination of micrometer- and submicrometer-thick multilayered thin coatings. The power of the phase rotation and phase spectrum analytical methods to clearly distinguish the infrared signature of submicrometer-thick coatings is demonstrated. The thickness determined by the step-scan FT-IR photoacoustic method is in very reasonable agreement with optical microtomy/microscopy measurements performed at-line during the coating process. The former technique described in detailed here offers substantial benefits in terms of measurement time and operator dependency, while not sacrificing the accuracy of the measurement. The problem of saturation and its effect on "real-life" samples is also discussed.
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