Dielectric thermal

An alternative method of studying the molecular motions of a polymeric chain is to measure the complex permitivity of the sample, mounted as dielectric of a capacitor and subjected to a sinusoidal voltage, which produces polarization of the sample macromolecules. The storage and loss factor of the complex permitivity are related to the dipolar orientations and the corresponding motional processes. The application of the dielectric thermal analysis (DETA) is obviously limited to macromolecules possessing heteroatomic dipoles but, on the other hand, it allows a range of frequency measurement much wider than DMTA and its theoretical foundations are better established. 

The relaxation methods employed are Dynamic Mechanical Thermal Analysis (DMTA) and Dielectric Thermal Analysis (DETA). Generally in both cases a single excitation frequency is used and the temperature is varied,... 

In an analogous manner to DMA, dielectric thermal analysis (DETA) represents a technique to apply an alternating electric field across the tested sample, which contributes to a polarization of the material with consequent current flow. DETA enables measurement of dielectric properties, which can further be related to material properties and thermal transitions as described below. 

Figure 18.26. Dielectric thermal analysis scans of polycarbonate at 1Hz and at a heating rate of 3°Cmin 1. Reproduced from Foreman et al. (1995), by permission of TA Instruments, Inc.

Figure 18.27. Dielectric thermal analysis online monitoring of a resin transfer molding process at 1000 Hz. Reproduced from Mcllhagger et al. (2000), by permission of Elsevier, Ltd.

Thermal analysis is a group of techniques in which a physical property of a substance is measured as a function of temperature when the sample is subjected to a controlled temperature program. Single techniques, such as thermogravimetry (TG), differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), dielectric thermal analysis, etc., provide important information on the thermal behaviour of materials. However, for polymer characterisation, for instance in case of degradation, further analysis is required, particularly because all of the techniques listed above mainly describe materials only from a physical point of view. A hyphenated thermal analyser is a powerful tool to yield the much-needed additional chemical information. In this paper we will concentrate on simultaneous thermogravimetric techniques. 

Differential scanning calorimetry (DSC) Modulated or stepwise DSC Dielectric thermal analysis (DETA)... 

EMAA Zn salt (70-30) / EPDM-SO3 Zn salt (30-70) internal mixer at 170°C / mechanical properties / DMA / dielectric thermal analyses / FTIR / effects of multiple thermal histories Kurian etal., 1996... 

The relaxation methods employed are Dynamic Mechanical Thermal Analysis (DMTA) and Dielectric Thermal Analysis (DETA). Generally in both cases a single excitation frequency is used and the temperature is varied, typically over a range between — 100 °C and +200 °C. Changes in molecular motion, and hence 7, are detected by both techniques, but in the case of DETA the process has to involve movement of dipoles or fully developed electrical charges on the polymer in order to be detected. Thus the two techniques can be used to complement each other, since transitions can be detected on DMTA and assigned as due to dipoles according to whether or not they also occur with DETA. 

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