With thermally stimulated depolarization currents, we researched the relaxations of crosslinked polyethylene as it is used in medium-voltage cable insulation. Through conventional polarization two heteropolar peaks stand up in the spectra, at 80 and 105°C. As the sample is annealed, a homopolar peak is developed at about 99°C. With window polarization, our results indicated that the 80°C peak is a structured peak related to polar crosslinking subproducts and impurities. The 105 and 99°C peaks are fitted to the general kinetic-order model because the 105°C peak is related to free-charge detrapping at the crystalline phase, in the bulk and maybe at the amorphous-crystal interphases, and the peak that is observed at 99°C is due to injected charge. Annealing at high temperatures promotes the creation of traps in the material. Charge trapping at T Ͻ 70°C seems to be related to the increased insulator resistivity with annealing time.

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: Relaxations in poly(etherimide) PEI Ultem 1000 have been analysed by di †erential scanning calorimetry (DSC), dynamic mechanical spectroscopy (DMS), dielectric relaxation spectroscopy (DRS) and thermally stimulated depolarization current (TSDC) measurements. DMTA and DRS results show three distinct relaxations c, b and a in the temperature range [140 to 250¡C. The Ðrst one depends strongly on the water content in the sample as will be discussed in more detail in the second paper of this series. These results are in good agreement with those observed by TSDC of conventionally polarized electrets. In addition to these three relaxations, TSDC measurements show : (1) a peak (o) at which is attributed to space charge temperatures above the a relaxation, (2) indications of structure in the b relaxation zone. In the case of electrets formed by the windowing polarization method, the resulting TSDC spectra allow us to discern the Ðne structure of the b relaxation, which is formed by three subrelaxations. In this work, the activation energies calculated by the di †erent techniques are compared, and a molecular origin for each relaxation is proposed.1998 SCI. Polym. Int. 46, 11È19 (1998)

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The glass transition in amorphous poly(ethylene terephthalate) is studied by thermally stimulated depolarization currents (TSDC) and differential scanning calorimetry (DSC). The ability of TSDC to decompose a distributed relaxation, as the glass transition, into its elementary components is demonstrated. Two polarization techniques, windows polarization (WP) and non-isothermal windows polarization (NIW), are employed to assess the influence of thermal history in the results. The Tool-Narayanaswami-Moynihan (TNM) model has been used to fit the TSDC spectra. The most important contributions to the relaxation comes from modes with non-linearity (x) around 0.7. Activation energies yield by this model are located around 1 eV for polarization temperature (T p ) below 50 • C and they raise up to values higher than 8 eV as T p increases (up to 80 • C). There are few differences between results obtained with WP and NIW but, nonetheless, these are discussed. The obtained kinetic parameters are tested against DSC results in several conditions. Calculated DSC curves at several cooling and heating rates can reproduce qualitatively experimental DSC results. These results also demonstrate that modelization of the non-equilibrium kinetics involved in TSDC spectroscopy is a useful experimental tool for glass transition studies in polar polymers.

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Dynamic electrical analysis shows that at high temperatures (above the glass transition temperature), the electrical properties of polyetherimide are strongly influenced by space charge. In this article we have studied the relaxation of space charge in two commercial varieties of polyetherimide: Ultem 1000 and Ultem 5000. Their conductive properties were determined by dynamic electrical analysis, using the electric modulus formalism. The complex part of the electric modulus was fitted to Coelho’s model which considers ohmic conductivity and diffusion as the prevailing charge transport mechanisms. The complex part of the electric modulus exhibits a peak in the low frequency range that can be associated with space charge. A good agreement between experimental and calculated data is observed after the fitting process to Coelho’s model. Differences in the electrode behavior were required: blocking electrode conditions in the case of Ultem 5000 and partially blocking electrode for Ultem 1000. In both cases the conductivity determined is thermally activated and it increases with the temperature due to an increasing mobility, as their carrier densities do not vary significantly in the temperature range studied.