Ex SituTransmission Electron Microscopy: A Fixed-Bed Reactor Approach

Abstract

A fixed-bed reactor has been designed and constructed for ex situ transmission electron microscopy (TEM) studies of heterogeneous catalysts. Theex situfacility exposes a fully prepared TEM sample on a grid to actual process conditions (e.g., temperature, pressure, gas composition, etc.) by placing the grid at the exit section of a conventional fixed-bed reactor. A unique reactor design allows grid transfer into the electron microscope and back into the reactor again under a controlled (inert) environment, thus allowing time-resolved monitoring of catalyst morphology changes under realistic, well-controlled conditions. This facility stands completely independent of the TEM. Thus, no special TEM modifications are required and long-termex situstudies do not impact microscope utilization. The utility of the facility is demonstratedviathe oxidation of intermediate size (∼20–∼80 nm) supported copper particles.