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Novel MEMS-Based Gas-Cell/Heating Specimen Holder Provides Advanced Imaging Capabilities for In Situ Reaction Studies

Published online by Cambridge University Press:  27 July 2012

Lawrence F. Allard ,
Steven H. Overbury ,
Wilbur C. Bigelow ,
Michael B. Katz ,
David P. Nackashi  and
John Damiano
Lawrence F. Allard*
Affiliation:
Physical Sciences Directorate, Oak Ridge National Laboratory, Oak Ridge, TN 37831, USA
Steven H. Overbury
Affiliation:
Physical Sciences Directorate, Oak Ridge National Laboratory, Oak Ridge, TN 37831, USA
Wilbur C. Bigelow
Affiliation:
Department of Materials Science & Engineering, University of Michigan, Ann Arbor, MI 48104, USA
Michael B. Katz
Affiliation:
Department of Materials Science & Engineering, University of Michigan, Ann Arbor, MI 48104, USA
David P. Nackashi
Affiliation:
Protochips Inc., 617 Hutton St., Suite 111, Raleigh, NC 27606, USA
John Damiano
Affiliation:
Protochips Inc., 617 Hutton St., Suite 111, Raleigh, NC 27606, USA
*
Corresponding author. E-mail: allardLFjr@ornl.gov
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Abstract

In prior research, specimen holders that employ a novel MEMS-based heating technology (AduroTM) provided by Protochips Inc. (Raleigh, NC, USA) have been shown to permit sub-Ångström imaging at elevated temperatures up to 1,000°C during in situ heating experiments in modern aberration-corrected electron microscopes. The Aduro heating devices permit precise control of temperature and have the unique feature of providing both heating and cooling rates of 106°C/s. In the present work, we describe the recent development of a new specimen holder that incorporates the Aduro heating device into a “closed-cell” configuration, designed to function within the narrow (2 mm) objective lens pole piece gap of an aberration-corrected JEOL 2200FS STEM/TEM, and capable of exposing specimens to gases at pressures up to 1 atm. We show the early results of tests of this specimen holder demonstrating imaging at elevated temperatures and at pressures up to a full atmosphere, while retaining the atomic resolution performance of the microscope in high-angle annular dark-field and bright-field imaging modes.

Keywords

in situgas reactiongas cellhigh-resolutionelectron microscopycatalystsMEMS
Type
Special Section: Aberration-Corrected Electron Microscopy
Information
Microscopy and Microanalysis , Volume 18 , Issue 4 , August 2012 , pp. 656 - 666
Copyright
Copyright © Microscopy Society of America 2012

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References

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