title: Ex situ transmission 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. The ex situ facility 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-term ex situ studies do not impact microscope utilization. The utility of the facility is demonstrated via the oxidation of intermediate size ( approximately 20- approximately 80 nm) supported copper particles.
authors.affiliation: ExxonMobil Research and Engineering Company, 1545 Route 22 East, Annandale, NJ 08801-0998, USA. chris.e.kliewer@exxonmobil.com
authors.forename: Chris E
authors.initials: CE
authors.lastname: Kliewer
authors.forename: Gabor
authors.initials: G
authors.lastname: Kiss
authors.forename: Gregory J
authors.initials: GJ
authors.lastname: Demartin
mesh_terms: D003300:Copper / Q000737:chemistry; D004867:Equipment Design; D007221:Industry; D008854:Microscopy, Electron / Q000295:instrumentation / Q000379:methods*; D010084:Oxidation-Reduction; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
chemical_list: D003300:Copper