RheoDSC: design and validation of a new hybrid measurement technique

Abstract

A newly developed hyphenated technique is presented that combines an existing rheometer and differential scanning calorimeter (DSC) into a single experimental setup. Through the development of a fixation accessory inside the cell of the calorimeter and the introduction of an add-on unit for the rheometer, the simultaneous calorimetric and rheological measurement inside the well-controlled thermal environment of a Tzero™ DSC cell opens new experimental possibilities. The evolution of thermal and flow properties of a material can be simultaneously monitored during steady or oscillatory shear flow and regular or modulated temperature DSC measurements. The technique offers interesting opportunities for the investigation of flow-induced transitions, such as crystallization or phase separation, and provides a possibility for high-throughput screening of materials. The signal quality of the novel technique in comparison to the stand-alone techniques is demonstrated by the evaluation of the calibration factors and by measurements on standard materials. Finally, combined rheological and calorimetric melting and crystallization experiments on polycaprolacton are performed.