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Abstract  

This work reports on the curing kinetics of unsaturated polymer resins (UPRs) cured with styrene, studied by differential scanning calorimetry and Fourier transform infrared spectroscopy. The data lead to determination of the experimental conditions with which to obtain a fully cured material and open the way for study of the relaxation phenomena by means of thermally stimulated depolarization current analysis (TSDC). In relaxation studies on fully cured resins, the TSDC spectra revealed important overlapping of the main relaxation peak with an extra upper peak. The importance of this extra peak a priori prevents further analysis of the main relaxation. To identify the origins of this peak (space charge or other), the purity of the resin was checked by X-ray fluorescence spectroscopy. The use of UPR specimens with different compositions (in terms of the resin/activator/initiator ratio) demonstrated that the bulk of the impurities Cl, K, Ca, Sr, Zr and Ba are due to the promoter. Decoupling of the mixed peaks (α-relaxation and extra) revealed that the a peak is independent of the proportion of the promoter in the resin and that the extra peak is principally due to the presence of these impurities.

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able to answer the above questions. Thermally stimulated discharge current (TSDC) technique is applied in variety of material for the study of dispersion phases such as disperse and porous metal oxides, polymers, liquid crystals, amorphous and

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Abstract  

Polyurethane acrylate resins cured by two different ways, a thermal way and a photochemical way, are investigated by means of differential scanning calorimetry (DSC) and thermally stimulated depolarization currents (TSDC). Even if both curing methods lead to the same material from a chemical point of view, we show that important differences exist between the thermocured resin and the photocured resin in terms of molecular relaxation behaviour.

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Abstract  

Pyrolysis of normally insulating aromatic polyimide is known to impart electrical conductivity to the polymer due to the formation of carbonized regions in an insulating matrix with a concomitant change in the polymer’s structural arrangement. The wholly pyrolyzed polyimide is potentially useful for specific applications in certain types of semiconductor devices because of the polyimide’s insulator/conductor transition which creates a barrier type conduction. Pyrolysis, however, degrades the required mechanical integrity of the polyimide for construction of such devices. In order to evaluate the fundamental aspects of barrier conduction by high voltage electron transfer from metal contact that can still produce measurable current in thermally treated non-pyrolyzed polyimide, the nature of depolarization in Kapton was assessed by the thermally stimulated depolarization current (TSDC) technique. The results show that thermal treatment of polyimide without pyrolysis and therefore without loss of mechanical integrity offers a viable means of steady electron conduction for semiconductor operation.

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Abstract  

A logical approach to electron transport studies for barrier conduction in layered structures was adopted by thermally stimulated discharge current (TSDC) measurement. The scope and applicability of this technique to the evaluation of the thermoelectric parameters of relaxation time, detrapping energy and depolarization rates are demonstrated here. These are characterized by the controlling factors of layer resistance and the resultant thermal and voltage gradients which apply to the drift of electrons arising from both dipolar and interfacial charges. The methodologies used in this study are suitable for parametric evaluation of structured electronic devices.

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Abstract  

Investigations involving thermally stimulated depolarization currents were performed on unsaturated polyester resins cured with styrene. Samples containing different amounts of Co octoate promoter were studied. The complex spectra revealed the classical β and the α dipolar relaxations. The peak characterizing the α dipolar relaxation was overlapped by a ρ peak of appreciable magnitude, due to the presence of impurities in the promoter solution [1]. However, study of the elementary spectra as concerns both α and β peaks for various samples containing different amounts of Co octoate demonstrated that the relaxation kinetics, and particularly the values of the apparent activation energies, do not depend on these impurities.

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Abstract  

The relaxation of electric field-induced polar orientation in a side-chain-bearing liquid-crystalline polysiloxane was measured by means of thermally stimulated depolarization currents. Different relaxation mechanisms were identified and characterized: the glass transition cooperative relaxation exhibits compensation behaviour. On the other hand, lowerT g and upperT g discharges were observed and their molecular nature is discussed.

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Abstract  

The thermally stimulated discharge current (TSC) and differential scanning calorimetry (DSC) spectroscopy have been recorded in 25 μm thick samples of pristine polycarbonate (PC) and zinc oxide nano particle-filled polycarbonate. Polycarbonate (PC)/zinc oxide (ZnO) nanocomposites of different mass ratio (e.g., 1, 3, and 5%) were prepared by sol–gel method, followed by film casting. The glass transition temperature of nanocomposite samples increases with increase in concentration of ZnO nano fillers. It is due to the strong interaction between inorganic and organic components. The TSC peaks of nanocomposite and pristine PC indicate the multiple relaxation process. It has been observed that the magnitude of TSC decreases with increase in concentration of nanofillers. The TSC characteristics of 5% filled nanocomposites shows exponential increase of current at higher temperature region. This increase in current is caused by formation of charge-transfer complex between inorganic phase (e.g., ZnO) and organic phase (e.g., PC). Thus, the nano material like zinc oxide transfers the charge carriers from inorganic phase to organic phase rapidly and resultant current increases exponentially. This current is known as leakage current or breakdown current. TSC peak height is observed as a function of the polarizing field. The height of TSC peak increases as the field increases in pristine PC, while TSC peak height is suppressed in nanocomposite samples. This indicates the amount of space charge is smaller in the nanocomposites with a proper addition of ZnO nano fillers than in the pristine PC.

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current (TSDC) in short and open-circuit configurations, designed for the investigations of charged dielectrics. TSDC is a powerful technique that helps in the understanding of the charge storage, charge decay, and structure of polymers (i.e., semi

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The glass transition

Correlation of DSC and TSDC investigations

Journal of Thermal Analysis and Calorimetry
Authors: E. Dargent, C. Cabot, J. M. Saiter, J. Bayard, and J. Grenet

This work deals with a comparison of data obtained from differential scanning calorimetry (DSC) and thermally stimulated depolarization current (TSDC) investigations. Measurements were performed on various poly(ethylene terephthalate) films: a wholly amorphous, a thermally crystallized and drawn samples.

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