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Ex Situ Transmission Electron Microscopy: A Fixed-Bed Reactor Approach

Published online by Cambridge University Press:  09 December 2005

Chris E. Kliewer ,
Gabor Kiss  and
Gregory J. DeMartin
Chris E. Kliewer
Affiliation:
ExxonMobil Research and Engineering Company, 1545 Route 22 East, Annandale, NJ 08801-0998, USA
Gabor Kiss
Affiliation:
ExxonMobil Research and Engineering Company, 1545 Route 22 East, Annandale, NJ 08801-0998, USA
Gregory J. DeMartin
Affiliation:
ExxonMobil Research and Engineering Company, 1545 Route 22 East, Annandale, NJ 08801-0998, USA
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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 (∼20–∼80 nm) supported copper particles.

Keywords

ex situ transmission electron microscopyoxidation
Type
MATERIALS APPLICATIONS
Information
Microscopy and Microanalysis , Volume 12 , Issue 2 , April 2006 , pp. 135 - 144
Copyright
© 2006 Microscopy Society of America

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References

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