Hess Kai-Uwe, Schawe Jürgen E K, Wilding Martin, Purgstaller Bettina, Goetschl Katja E, Sturm Sebastian, Müller-Caspary Knut, Sturm Elena V, Schmahl Wolfgang, Griesshaber Erika, Bissbort Thilo, Weidendorfer Daniel, Dietzel Martin, Dingwell Donald B
Earth and Environmental Sciences, Ludwig-Maximilians-Universität München, Theresienstraße 41/III, 80333 München, Germany.
Mettler-Toledo GmbH, Heuwinkelstrasse 3, 8603, Nänikon, Switzerland.
Philos Trans A Math Phys Eng Sci. 2023 Oct 16;381(2258):20220356. doi: 10.1098/rsta.2022.0356. Epub 2023 Aug 28.
We report the first calorimetric observations of glass transition temperatures and crystallization rates of anhydrous, amorphous calcium-magnesium carbonate using fast scanning differential scanning calorimetry. Hydrous amorphous CaMgCO · 0.5HO (ACMC) solid was precipitated from a MgCl-NaHCO buffered solution, separated from the supernatant, and freeze-dried. An aliquot of the freeze-dried samples was additionally dried at 250°C for up to 6 h in a furnace and in a high-purity N atmosphere to produce anhydrous ACMC. The glass transition temperature of the anhydrous CaMgCO was determined by applying different heating rates (1000-6000 K s) and correcting for thermal lag to be 376°C and the relaxational heat capacity was determined to be p = 0.16 J/(g K). Additionally, the heating rate dependence of the temperature that is associated with the corrected crystallization peaks is used to determine the activation energy of crystallization to be 275 kJ mol. A high-resolution transmission electron microscopy study on the hydrous and anhydrous samples provided further constraints on their compositional and structural states. This article is part of the theme issue 'Exploring the length scales, timescales and chemistry of challenging materials (Part 1)'.
我们报告了使用快速扫描差示扫描量热法对无水无定形碳酸钙镁的玻璃化转变温度和结晶速率进行的首次量热观察。从MgCl-NaHCO缓冲溶液中沉淀出水合无定形CaMgCO·0.5HO(ACMC)固体,与上清液分离并冻干。将一部分冻干样品在炉中于250°C在高纯度N气氛中额外干燥长达6小时,以制备无水ACMC。通过应用不同的加热速率(1000-6000 K s)并校正热滞后,确定无水CaMgCO的玻璃化转变温度为376°C,松弛热容确定为p = 0.16 J/(g K)。此外,与校正后的结晶峰相关的温度的加热速率依赖性用于确定结晶活化能为275 kJ mol。对含水和无水样品的高分辨率透射电子显微镜研究进一步限制了它们的组成和结构状态。本文是主题为“探索具有挑战性材料的长度尺度、时间尺度和化学性质(第1部分)”的一部分。