Experimental investigation for modeling the hardening of thermosetting polymers during curing

During curing of thermosetting polymers, crosslinking results in hardening or stiffening of the material. In electronics, for example in encapsulating integrated circuits (die bonding), thermosets are fully cured in a controlled environment (under UV-light or within a thermal oven) such that the highest stiffness possible has been achieved. In building materials, specifically in thermosets used in fastening systems (adhesive anchoring), hardening occurs at environmental temperature. Daily temperature variations alter the curing process and possibly lead to a lower stiffness. We demonstrate a modeling approach for the mechanical response dependency on the degree of cure by means of rheometer measurements under a specific temperature profile. Precisely, we perform oscillatory rheometric tests and convert the storage and loss moduli to material parameters depending on the degree of cure. Moreover, the temperature dependency as well as chemical shrinkage have been determined by the same experimental protocol. The presented approach has been applied to a commercially available (epoxy) thermoset used as an adhesive. We have observed a hardening after a gelation point of 0.7 and an adequate fit for mechanical response by polynomial functions of degree four