Direct Synthesis of ZIF-8 on Transmission Electron Microscopy Grids Allows Structure Analysis and 3D Reconstruction

The first example of layer‐by‐layer growth of a metal–organic framework (MOF) directly on transmission electron microscopy (TEM) grids is described. ZIF‐8 is deposited on thin amorphous carbon films and subjected to a structure analysis by (scanning) TEM ((S)TEM). This method serves as a two‐in‐one synthesis and TEM sample‐preparation technique and allows straightforward analysis of ZIF‐8 crystallites. Artifacts resulting from sample preparation are completely avoided by this approach. The morphological properties, crystal structure, and the chemical composition of the material are investigated with high spatial resolution by a variety of methods of (analytical) electron microscopy. Furthermore, the incorporation of metallic nanoparticles in ZIF‐8 by integrating a corresponding step into the layer‐by‐layer deposition process is examined. The formation of ZIF‐8 crystals on the film proceeds as under the absence of nanoparticle‐forming synthesis steps. However, the nanoparticles rather cover the supporting amorphous carbon film than being incorporated in the ZIF‐8 material. This information cannot be obtained from standard characterization techniques but requires the application of analytical (S)TEM techniques.