Kiewiet S, Janssens V, Miltner H E, Van Assche G, Van Puyvelde P, Van Mele B
Department of Materials and Chemistry-Physical Chemistry and Polymer Science, Vrije Universiteit Brussel, Pleinlaan 2, 1050 Brussels, Belgium.
Rev Sci Instrum. 2008 Feb;79(2 Pt 1):023905. doi: 10.1063/1.2838585.
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.
本文介绍了一种新开发的联用技术，该技术将现有的流变仪和差示扫描量热仪整合到一个单一的实验装置中。通过开发一种用于差示扫描量热仪（DSC）坩埚的固定附件和一种新型转子，在Tzero DSC池的良好控制的热环境中进行同步测量。因此，可以使用稳态或振荡剪切测量以及常规或调制温度DSC测量同时测量材料的热性能和流动性能的演变。随着原型的构建，对设计进行了验证。该技术为研究流动诱导的转变（例如结晶或相分离）提供了有趣的机会，并为材料的高通量筛选提供了一种手段。通过两个案例研究证明了该新技术的潜力：热固性环氧-胺体系固化过程中的化学流变学以及间规聚丙烯的流动诱导结晶。
