Electron NanoCrystallography of Metal-Organic Frameworks

The rapid progress in the production and application of nanomaterials highlights the critical importance of advanced characterization techniques adapted to their nanoscale dimensions. This thesis focuses on method development and application of 3D Electron Diffraction (3D-ED) [1] as an effective alternative to traditional X-ray diffraction (XRD) for the analysis of submicron-sized crystals [2, 3]. We begin by exploring the foundational principles of 3D-ED and the specific requirements necessary for the accurate acquisition and analysis of electron diffraction data. Following this, we detail the development and implementation of automated data acquisition protocols, which significantly improve the efficiency, precision, and reproducibility of structural characterizations. Expanding on these developments, the study focuses on the application of 3D-ED, to investigate a range of novel and unreported metal-organic frameworks (MOFs), demonstrating the versatility and robustness of 3D-ED techniques in resolving complex structural details, as validated by Rietveld refinements. This thesis illustrates how 3D-ED can serve as an indispensable tool for the structural characterization of nanomaterials, demonstrating its potential to significantly contribute to advancements in materials science.