Glor Ethan C, Fakhraai Zahra
Department of Chemistry, University of Pennsylvania.
Department of Chemistry, University of Pennsylvania;
J Vis Exp. 2016 Jan 26(107):e53499. doi: 10.3791/53499.
This report aims to fully describe the experimental technique of using ellipsometry for cooling rate dependent Tg (CR-Tg) experiments. These measurements are simple high-throughput characterization experiments, which can determine the glass transition temperature (Tg), average dynamics, fragility and the expansion coefficient of the super-cooled liquid and glassy states for a variety of glassy materials. This technique allows for these parameters to be measured in a single experiment, while other methods must combine a variety of different techniques to investigate all of these properties. Measurements of dynamics close to Tg are particularly challenging. The advantage of cooling rate dependent Tg measurements over other methods which directly probe bulk and surface relaxation dynamics is that they are relatively quick and simple experiments, which do not utilize fluorophores or other complicated experimental techniques. Furthermore, this technique probes the average dynamics of technologically relevant thin films in temperature and relaxation time (τα) regimes relevant to the glass transition (τα > 100 sec). The limitation to using ellipsometry for cooling rate dependent Tg experiments is that it cannot probe relaxation times relevant to measurements of viscosity (τα << 1 sec). Other cooling rate dependent Tg measurement techniques, however, can extend the CR-Tg method to faster relaxation times. Furthermore, this technique can be used for any glassy system so long as the integrity of the film remains throughout the experiment.
本报告旨在全面描述使用椭偏仪进行与冷却速率相关的玻璃化转变温度(CR-Tg)实验的实验技术。这些测量是简单的高通量表征实验,可确定各种玻璃材料的玻璃化转变温度(Tg)、平均动力学、脆性以及过冷液体和玻璃态的膨胀系数。该技术允许在单个实验中测量这些参数,而其他方法必须结合多种不同技术来研究所有这些性质。测量接近Tg的动力学尤其具有挑战性。与直接探测体相和表面弛豫动力学的其他方法相比,与冷却速率相关的Tg测量的优势在于它们是相对快速且简单的实验,不使用荧光团或其他复杂的实验技术。此外,该技术在与玻璃化转变相关的温度和弛豫时间(τα)范围内探测技术相关薄膜的平均动力学(τα>100秒)。使用椭偏仪进行与冷却速率相关的Tg实验的局限性在于它无法探测与粘度测量相关的弛豫时间(τα<<1秒)。然而,其他与冷却速率相关的Tg测量技术可以将CR-Tg方法扩展到更快的弛豫时间。此外,只要薄膜在整个实验过程中保持完整性,该技术可用于任何玻璃体系。