Network development during epoxy curing: experimental ultrasonic data and theoretical predictions

Abstract

Ultrasonic waves propagation acts as a dynamic mechanical deformation on a material. When, during ultrasonic wave propagation, chemical or physical changes occurs, the evolution of an elastic modulus can be monitored. Therefore, this technique can be considered a powerful tool for non-destructive cure monitoring with a potential for “in situ” applications. In this work, the isothermal cure of a model epoxy resin cured with an amine is studied using propagation of longitudinal ultrasonic wave. The epoxy to amine ratio is optimized in order to reach full conversion of the amine groups during curing. The relative changes in the ultrasonic velocity and attenuation, measured by the transmission technique, have been applied to the calculation of the longitudinal modulus. The ultrasonic modulus has been compared with the degree of reaction measured using Differential Scanning Calorimetry (DSC). Furthermore a correlation between the ultrasonic modulus and the crosslinking density is presented combining DSC data with the stoichiometry of reactants according with the statistical theory of Miller and Macosko. The plot of the ultrasonic modulus as a function of the crosslinking density suggested that the theory of rubber elasticity can not be applied to the ultrasonic bulk longitudinal modulus as a consequence of the small deformation involved in the propagation of the ultrasonic waves.