Rolle Konrad, Butt Hans-Jürgen, Fytas George
Max-Planck-Institute for Polymer Research, Ackermannweg 10, 55128 Mainz, Germany.
ACS Photonics. 2021 Feb 17;8(2):531-539. doi: 10.1021/acsphotonics.0c01533. Epub 2020 Dec 28.
Glass transition temperatures are most commonly measured by differential scanning calorimetry, a method that has been extended to the flash scanning calorimetry (FSC) regime by reducing sample volumes. However, significant manual preparation effort can render FSC impractical for, e.g., local probing of spatially heterogeneous specimens. Another strategy can be to select a small volume by focusing down a laser beam, where Brillouin Light Scattering (BLS) is a proven method for confocal measurement. Here, we introduce Flash Brillouin Scattering, which extends BLS to fast scan rates, achieved by periodically heating the probed region with an infrared laser. For comparison with conventional BLS, we first characterize of pure glycerol, and show how rapid quenching produces a less packed glass with downshifted sound velocity. We then turn toward its aqueous solutions, which crystallize too fast for a nonflash approach, and demonstrate scan rates in excess of 10 K/s. These results are of interest not only because glycerol is a model system for hydrogen-bonded glass formers, but also because of its applications as a cryoprotectant for frozen biological samples. Light scattering studies of the latter, currently limited to cryo-Raman spectroscopy, are likely to be complemented by the technique introduced here.
玻璃化转变温度最常用差示扫描量热法来测量,该方法通过减小样品体积已扩展到快速扫描量热法(FSC)领域。然而,大量的手工制备工作会使FSC对于例如空间异质样品的局部探测变得不切实际。另一种策略可以是通过聚焦激光束来选择小体积区域,其中布里渊光散射(BLS)是一种经过验证的共焦测量方法。在此,我们引入快速布里渊散射,它通过用红外激光周期性加热探测区域将BLS扩展到快速扫描速率。为了与传统BLS进行比较,我们首先对纯甘油进行表征,并展示快速淬火如何产生一种堆积较松散、声速下移的玻璃态。然后我们转向其水溶液,对于非快速方法来说其结晶太快,我们展示了超过10 K/s的扫描速率。这些结果不仅因为甘油是氢键型玻璃形成体的模型体系而令人感兴趣,还因为其作为冷冻生物样品的冷冻保护剂的应用。目前仅限于低温拉曼光谱的后者的光散射研究,很可能会被这里介绍的技术所补充。