The dielectric permittivity, e', and loss, s", during the crosslinking or curing of diglycidyl ether of bisphenol-A with diamino diphenyl methane and various amounts of an elastomer, amine-terminated butadiene acrylonitrile (ATBN), have been measured from their sol to gel to glass-formation regions. As the elastomer-containing thermoset cures, both e' and e" initially decrease and then increase with time. e' finally decreases to a value near 3, but e" goes through a sharp minimum followed by a peak and ultimately decreases to about 10- 3. The initial increase in both e' and e" has been interpreted as an onset of liquid-liquid phase separation, which becomes nearly complete before the monotonic decrease in e' begins as a result of network formation in the curing thermoset. The time for the onset of phase separation is relatively insensitive to the amount of elastomer in the thermoset, and indicates the time of cure at which the network structure reaches a molecular weight when the elastomer becomes immiscible in it. Both the conductivity and permittivity increase with the increase in the elastomer content, with the consequence that the onset of gelation, which is marked by an approach of conductivity to near zero, is masked by the dipolar relaxation process. Corresponding analysis in the electrical modulus formalism confirms these observations and shows further that the conductivity follows a Maxwell relaxation. The e" of the cured thermoset plotted against temperature shows broad peaks and shoulders to these peaks. These are a combination of the sub-Tg relaxations in both the elastomer and the thermoset's network structure and the a-relaxation of the elastomer which appears at 240 K at 1 kHz. The permittivity and dielectric loss of the cured thermoset increase with an increase in the weight fraction of ATBN.
Посилання на статтю:
Relaxations in thermosets: 15. Curing kinetics and dielectric behaviour of butadiene-acrylonitrile-containing epoxide thermosets / Manli Wang and G. P. Johari // Polymer. – 1992. – Vol 33. – P. 4747-4755.