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The Dynamics of Active Metal Catalysts Revealed by In Situ Electron MicroscopyThe Dynamics of Active Metal Catalysts Revealed by In Situ Electron Microscopy The Dynamics of Active Metal Catalysts Revealed by In Situ Electron Microscopy

The Dynamics of Active Metal Catalysts Revealed by In Situ Electron Microscopy
Conventional high-resolution imaging by electron microscopy plays an important role in the structural and compositional analysis of catalysts. However, since the observations are generally performed under vacuum and close to room temperature, the obtained atomistic details concern an equilibrium state that is of limited value when the active state of a catalyst is in the focus of the investigation. Since the early attempts of Ruska in 1942 [1], in situ microscopy has demonstrated its potential and, with the recent availability of commercial tools and instruments, led to a shift of the focus from ultimate spatial resolution towards observation of relevant dynamics. During the last couple of years we have implemented commercially available sample holders for in situ studies of catalysts in their reactive state inside a transmission electron microscope. In order to relate local processes that occur on the nanometer scale with collective processes that involve fast movement of large numbers of atoms, we have adapted an environmental scanning electron microscope (ESEM) for the investigation of surface dynamics on active catalysts. Using these two instruments, we are now able to cover a pressure range from 10-4 to 103 mbar and a spatial resolution ranging from the mm to the sub-nm scale. Presently we are investigating metal catalyzed CVD growth of graphene [2,3], as well as structural dynamics during oscillatory red-ox reactions on metal catalysts. The observations are performed in real-time and under conditions in which the active state of the catalyst can be monitored. The latter is of upmost importance, since the key requirement is to observe relevant processes and dynamics that are related to catalytic function. The ability to directly image the active catalyst and associated morphological changes at high spatial resolution enables us to refine the interpretation of spatially averaged spectroscopic data that was obtained under otherwise similar reaction conditions, for example during near-ambient-pressure in situ XPS measurements [4]. It will be shown that the ability of observing the adaption of an active surface to changes in the chemical potential of the surrounding gas phase in real-time potentially offers new and direct ways of optimizing catalysts and applied reaction conditions. References[1] E. Ruska, Kolloid-Zeitschrift, 100 (1942) 212-219[2] Z.-J. Wang et al., ACS Nano, 9 (2015) 1506–1519[3] Z.-J. Wang et al., Nat. Commun. 7 (2016) DOI:10.1038/ncomms13256[4] R. Blume et al., PhysChemChemPhys, 16 (2014) 25989 [more]
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