Abstract

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.

Highlights

  • In our study, we focus on ZIF-8 that belongs to the widely studied class of zeolitic imidazolate frameworks (ZIFs) [5, 6]

  • Metal-organic frameworks (MOFs) consist of metal nodes that are connected by organic linkers

  • We focus on ZIF-8 that belongs to the widely studied class of zeolitic imidazolate frameworks (ZIFs) [5, 6]

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Summary

Introduction

We focus on ZIF-8 that belongs to the widely studied class of zeolitic imidazolate frameworks (ZIFs) [5, 6]. Due to a large number of usable metal nodes and linkers, MOFs have a designable topology, porosity, and functionality [1] that has lead to the synthesis of around 70.000 MOFs until 2017 [3]. Transmission electron microscopy (TEM) is a key technique for analyzing the structural and chemical properties of SURMOFs. For TEM sample preparation, the film must be detached from the substrate and transferred to an electron-transparent support. The preparation of SURMOF films for TEM studies is a substantial obstacle that has not yet been solved satisfactorily.

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