Publication date: 10th April 2024
Modern MEMS-based transmission electron microscopy (TEM) holders enable precise specimen environment control, which is ideal for direct in-situ and in-operando observations, whether in real time or not. This talk presents two examples where MEMS-based holders are used primarily to control material processing and chemical reaction progress, enabling unique experiments assessing (1) solid-phase crystallization of a mixed ion-electron conducting (MIEC) amorphous complex oxide—a model amorphous low-temperature solid oxide fuel/electrolysis cell electrode, and (2) CaCO3 calcination—a model solid-vapor decomposition reaction and the critical step in calcium looping for CO2 capture and thermochemical energy storage.
Key aspects of MIEC amorphous complex oxide processing such as the evolution of structure/chemistry with temperature and the corresponding effect on electrical conductivity are detailed, and approaches to direct amorphous complex oxide processing towards desirable synthesis products based on these insights are discussed, applied to the amorphous La0.8Sr0.2MnO3-δ system [1]. To elucidate the CaCO3 calcination reaction, we applied correlated in-situ electron and synchrotron probes to directly observe CaCO3 calcination and report a new reaction mechanism involving heterogeneous nucleation of nanoporous CaO at CaCO3 grain boundaries followed by planar reaction front motion, in contrast to the widely accepted spherical shrinking core model [2].
[1] Jenna L. Wardini, George Harrington, Sangjun Kang, Dennis Kemp, Roger A. De Souza, Christian Kübel, William J. Bowman. (In revision).
[2] Jenny Martinez, Jenna L. Wardini, Xueli Zheng, Joann-Matthew Means, Huiming Guo, Pratik Dholabhai, Leora Dresselhaus-Marais, William J. Bowman. (2024) Advanced Materials Interfaces.
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