For nanoparticles active for chemical and energy transformations in static liquid environment, chemistries of surface or near-surface regions of these catalyst nanoparticles in liquid are crucial for fundamentally understanding their catalytic performances at a molecular level. Compared to catalysis at a solid-gas interface, there is very limited information on the surface of these catalyst nanoparticles under a working condition or during catalysis in liquid. Photoelectron spectroscopy is a surface-sensitive technique; however, it is challenging to study the surfaces of catalyst nanoparticles dispersed in static liquid because of the short inelastic mean free path of photoelectrons traveling in liquid. Here, we report a method for tracking the surface of nanoparticles dispersed in static liquid by employing graphene layers as an electron-transparent membrane to separate the static liquid containing a solvent, catalyst nanoparticles, and reactants from the high-vacuum environment of photoelectron spectrometers. The surfaces of Ag nanoparticles dispersed in static liquid sealed in such a graphene membrane liquid cell were successfully characterized using a photoelectron spectrometer equipped with a high vacuum energy analyzer. With this method, the surface of catalyst nanoparticles dispersed in liquid during catalysis at a relatively high temperature up to 150 °C can be tracked with photoelectron spectroscopy.
Studying surface of catalyst nanoparticles in a flowing liquid is important for understanding the underlying mechanism of a reaction performed in liquid. We report the design of a reaction cell system of Si3N4 window covering the flowing liquid with an electron-transmissible membrane. By using metal nanoparticles as a catalyst dispersed in a solvent, examination of the surface of catalyst nanoparticles in a flowing liquid was demonstrated by observation of Ag 3d photoemission feature when a liquid containing Ag nanoparticles was flowing through this system.
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