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

• Published in: Microscopy and microanalysis 2012-08, Vol.18 (4), p.656-666
• Main Authors: Allard, Lawrence F., Overbury, Steven H., Bigelow, Wilbur C., Katz, Michael B., Nackashi, David P., Damiano, John
• Format: Article
• Language: English
• Subjects: Design; Electrons; Geometry; Heating; High temperature; Laboratories; Microscopy; Silicon nitride; Spectrum analysis; Temperature; Temperature control
• ISSN: 1431-9276; 1435-8115
• DOI: 10.1017/S1431927612001249

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.