Bridging the gap in studying surface reactions, processes, and morphology and measuring at (catalytic) relevant conditions is crucial for our understanding of the working principles of porous crystalline materials. Scanning tunneling microscopy is limited because of the required conductivity of the sample, whereas atomic force microscopy (AFM) is often challenging in use owing to the physical mechanism underlying the technique. Herein, we report a tailor-made autoclave-inserted AFM, able to measure at ∼20 bar and ∼110 °C. First, we show the ability to obtain nanometer resolution on well-defined test samples at before-mentioned conditions. Second, to demonstrate the possibilities of analyzing morphological evolutions at elevated temperatures and pressures, we use this setup to measure the stability of a surface-anchored metal-organic framework (SURMOF) in-situ at pressures of 1-20 bar in the temperature range between 20 and 60 °C. It was found that the showcase HKUST-1 material has a good physical stability, as it is hardly damaged from exposure to pressures up to 20 bar. However, its thermal stability is weaker, as exposure to elevated T damaged the material by influencing the interaction between organic linker and metal cluster. In-situ measurements at elevated T also showed an increased mobility of the material when working at such conditions. Combining the strength of AFM at elevated T and p with ex-situ AFM and spectroscopic measurements on this MOF showcases an example of how porous materials can be studied at (industrially) relevant conditions using the autoclave-inserted AFM.
Keywords: atomic force microscopy; autoclave measurements; catalyst stability; metal-organic frameworks; scanning probe microscopy.
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