Novel axial dynamic mechanical analysis setup for thermo-analytical study and curing kinetics optimization of thermoset adhesives

Abstract

Thermo-analytical studies of thermoset adhesives, either during research and development or in quality assurance activities, involve the application of various analytical equipment for adhesive characterization, from initial mixing to final product decomposition. Gelation is usually measured with rheometers or dynamic mechanical analyzers (DMAs); curing, post-curing, and curing kinetics are often studied using differential scanning calorimetry (DSC). Glass transition temperature ( Tg) is measured via DSC or DMA, and finally, thermal decomposition measurements are done using thermal gravimetric analysis. Here, we present a new curing kinetics optimization module (C-KOM), an extension to an axial DMA, and a protocol for its usage, which combines elements from all of the above thermo-analytical techniques into one tool. As a case study, we apply C-KOM to investigate the effect of the curing temperature on the physical properties of an epoxy adhesive including gelation and end of cure points as well as its Tg. The data collected via C-KOM were used to extract the adhesive’s curing reaction rates and its activation energy. Our research allowed us to compare and evaluate previously suggested curing procedures and assess their validity. As a final step, the thermal decomposition temperature of the epoxy adhesive was also identified via C-KOM. The newly suggested C-KOM setup provides a fast path toward characterization and optimization of the curing processes of thermoset materials in a way that was not available before.