A combined in operando approach for low-energy Scanning Transmission Electron Microscopy and Grazing Incident Small Angle X-ray Scattering

Probing the evolution of electronic, structural, and chemical properties of nanostructured materials under reaction conditions is a crucial issue to determine their structure-functionality relationships. A relevant example is represented by heterogeneous catalysts, whose properties change dramatically with respect to the environment. Much of effort has been made lately in designing new solutions and technologies, or modifying the existing ones for purpose of operando conditions analysis. The use of micro- or nanoreactors is a second approach, where ultrathin membranes can efficiently separate the high-pressure volume from the (ultra)high vacuum of the characterization chamber. Very recently, microreactor cells have been developed to integrate the capabilities of ensemble-averaging synchrotron techniques with local probe ones, as TEM to analyze the same catalytic process with different instruments. Despite the great power of this method, the extremely small probing size of TEMs restricts the application of a combined approach to a limited set of micro-focused synchrotron techniques. We propose here the development of a novel multifunctional microreactor for operando low voltage Scanning TEM in a SEM compatible with a broad range of synchrotron techniques. We successfully designed a device compatible with Grazing Incident Small Angle X-ray Scattering (GISAXS), demonstrating the feasibility of our approach by studying the shape and size evolution of PVP-capped Pd nanocrystals under oxidation/reaction conditions.