RheoDSC: A hyphenated technique for the simultaneous measurement of calorimetric and rheological evolutions

Abstract

A newly developed hyphenated technique is presented combining an existing rheometer and differential scanning calorimeter into a single experimental setup. Through the development of a fixation accessory for differential scanning calorimeter (DSC) crucibles and a novel rotor, the simultaneous measurement is performed inside the well-controlled thermal environment of a Tzero DSC cell. Hence, the evolution of thermal and flow properties of a material can be simultaneously measured using steady or oscillatory shear measurements and regular or modulated temperature DSC measurements. Along with the construction of a prototype, a validation of the design was performed. The technique offers interesting opportunities for the investigation of flow-induced transitions, for instance, crystallization or phase separation, and provides an asset for high-throughput screening of materials. The potential of the novel technique is demonstrated by two case studies: the chemorheology during the cure of a thermosetting epoxy-amine system and the flow-induced crystallization of syndiotactic polypropylene.