Microsc Microanal. 2012 Aug;18(4):656-66. doi: 10.1017/S1431927612001249. Epub 2012 Jul 27.

Novel MEMS-based gas-cell/heating specimen holder provides advanced imaging capabilities for in situ reaction studies.

Microscopy and microanalysis : the official journal of Microscopy Society of America, Microbeam Analysis Society, Microscopical Society of Canada

Lawrence F Allard, Steven H Overbury, Wilbur C Bigelow, Michael B Katz, David P Nackashi, John Damiano

PMID: 22835379 DOI: 10.1017/S1431927612001249

Abstract

In prior research, specimen holders that employ a novel MEMS-based heating technology (Aduro™) 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.

Publication Types

• Journal Article
• Research Support, U.S. Gov't, Non-P.H.S.