Broadband dielectric spectroscopy method

Broadband Dielectric Spectroscopy provides a direct experimental access to the molecular relaxations of polymers over a broad frequency and temperature range. It is also especially suitable for the investigation of thin polymer films, because it does not suffer sensitivity loses with decreasing sample amount. This technique does require a special sample preparation for thin films, because of the need to have metal electrodes and good electrical contacts at both interfaces. Spin-coating, one of the most commonly employed methods for the preparation of... 

For thin polystyrene films annealed for 12 hours at 150 °C in high vacuum (10-6 mbar) and measured in a pure nitrogen atmosphere the dynamic glass transition was characterized using two experimental techniques capacitive scanning dilatometry and Broadband Dielectric Spectroscopy. Data from the first method are presented in Fig. 15a, showing the real part of the complex capacity at 1 MHz as a function of temperature for a thin PS film of 33 nm. 

The successful development of the time-domain dielectric spectroscopy method (generally called time-domain spectroscopy, TDS) [79-86] and broadband dielectric spectroscopy (BDS) [3,87-90] have radically changed the attitude towards DS, making it an effective tool for investigation of solids and liquids on the macroscopic, mesoscopic, and, to some extent, microscopic levels. 

Broadband dielectric spectroscopy is a powerful tool to investigate polymeric systems (see [38]) including polymer-based nanocomposites with different nanofillers like silica [39], polyhedral oligomeric silsesquioxane (POSS) [40-42], and layered silica systems [43-47] just to mention a few. Recently, this method was applied to study the behavior of nanocomposites based on polyethylene and Al-Mg LDH (AlMg-LDH) [48]. The properties of nanocomposites are related to the small size of the filler and its dispersion on the nanometer scale. Besides this, the interfacial area between the nanoparticles and the matrix is crucial for the properties of nanocomposites. Because of the high surface-to-volume ratio of the nanoparticles, the volume fraction of the interfacial area is high. For polyolefin systems, this interfacial area might be accessible by dielectric spectroscopy because polyolefins are nonpolar and, therefore, the polymeric matrix is dielectrically invisible [48]. 

The information on molecular order and dynamics of LC polymers is usually obtained by a combination of methods which complement each other, such as Nuclear Magnetic Resonance (NMR) and broadband dielectric spectroscopy.Proton Nuclear Magnetic Resonance ( H-NMR) is especially suitable in this field, because after selective labeling the different fragments of the molecule (backbone, spacer, and mesogenic group) can be monitored separately. 

Han and coworkers [38] determined the phase behavior of the ternary system consisting of [bmim][PFJ,TX-100, and water at 25 °C. By cyclic voltammetry method using potassium ferrocyanide, K Fe(CN)g, as the electroactive probe, the water-in-[bmim][PFJ, bicontinuous, and [bmim][PFJ-in-water microregions of the microemulsions were identified (Fig. 16.7). The hydrodynamic diameter of the [bmim] [PFJ-in-water microemulsions is nearly independent of the water content bnt increases with increasing [bmim] [PF ] content due to the swelling of the micelles by the IL. Sarkar and coworkers [39-41] reported the solvent and rotational relaxation studies in [bmim][PFJ-in-water microemulsions and water-in-[bmim][PFJ microemulsions using different types of probes, coumarin 153 (C-153), coumarin 151 (C-151), and coumarin 490 (C-490). The solvent relaxation time is retarded in the IL-in-water microemulsion compared to that of a neat solvent. The retardation of solvation time of water in the core of the water-in-IL microemulsion is several thousand times compared to pnre water. Nozaki and coworkers [42] reported a broadband dielectric spectroscopy study on a microemnlsion composed of water. 

Bias-induced reverse piezoelectric response Broadband dielectric spectroscopy (BDS) Dielectric permittivity spectrum Dielectric resonance spectroscopy Elastic modulus Ferroelectrets Electrical breakdown Acoustic method Characterization Dynamic coefficient Interferometric method Pressure and frequency dependence of piezoelectric coefficient Profilometer Quasistatic piezoelectric coefficient Stress-strain curves Thermal stability of piezoelectricity Ferroelectric hysteresis Impedance spectroscopy Laser-induced pressure pulse Layer-structure model of ferroelectret Low-field dielectric spectroscopy Nonlinear dielectric spectroscopy Piezoelectrically generated pressure step technique (PPS) Pyroelectric current spectrum Pyroelectric microscopy Pyroelectricity Quasistatic method Scale transform method Scanning pyroelectric microscopy (SPEM) Thermal step teehnique Thermal wave technique Thermal-pulse method Weibull distribution... 

In conclusion, when a WGM is excited in a dielectric microresonator, its evanescent component provides a convenient probe of the microresonator s surroundings. Various ways to implement evanescent-wave sensing have been devised, but the emphasis of this chapter has been on microcavity-enhanced absorption spectroscopy. The techniques described here have broad applicability, can even be used with broadband sources, and lend themselves well to further enhancement methods. We are looking forward to continuing our development of these sensors. 

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