4.5 Article

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

Journal

MICROSCOPY AND MICROANALYSIS
Volume 18, Issue 4, Pages 656-666

Publisher

CAMBRIDGE UNIV PRESS
DOI: 10.1017/S1431927612001249

Keywords

in situ; gas reaction; gas cell; high-resolution; electron microscopy; catalysts; MEMS

Funding

  1. U.S. Department of Energy, Office of Energy Efficiency and Renewable Energy, Vehicle Technologies Program

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In prior research, specimen holders that employ a novel MEMS-based heating technology (Aduro (TM)) provided by Protochips Inc. (Raleigh, NC, USA) have been shown to permit sub-Angstrom imaging at elevated temperatures up to 1,000 degrees 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 10(6 degrees)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.

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