화학공학소재연구정보센터
Polymer, Vol.41, No.15, 5949-5955, 2000
Understanding vitrification during cure of epoxy resins using dynamic scanning calorimetry and rheological techniques
The gelation and vitrification transitions during cure of an epoxy-amine system are examined using rheological, modulated differential scanning calorimetry (DSC) and FTIR techniques. The results from dynamic mechanical analysis show that gelation is observed before vitrification at all temperatures where it can be theologically defined. By comparing different rheological criteria for vitrification, it is seen that the vitrification transition is a gradual process that extends over a large part of cure at all temperatures where it occurs. Results from modulated DSC measurements show that the calorimetric vitrification times are longer than the vitrification times obtained from rheological measurements at cure temperatures above 100 degrees C, but that at lower temperatures calorimetric vitrification occurs before, or at the same time as, rheological vitrification. Theoretical gelation times, estimated from FTIR conversion data, were found to be consistently shorter than the observed gelation times. Theoretical vitrification times agreed well with the observed times. The magnitude of the vitrification transition, expressed either as amount of change in heat capacity or as maximum value of loss tangent, was found to decrease approximately linearly with increasing cure temperature.