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Introducing and Controlling Water Vapor in Closed-Cell In Situ Electron Microscopy Gas Reactions

Published online by Cambridge University Press:  11 March 2020

Kinga A. Unocic ,
Franklin S. Walden ,
Nelson L. Marthe ,
Abhaya K. Datye ,
Wilbur C. Bigelow  and
Lawrence F. Allard
Kinga A. Unocic*
Affiliation:
Center for Nanophase Materials Sciences Division, Oak Ridge National Laboratory, 1 Bethel Valley Rd, Oak Ridge, TN37831, USA
Franklin S. Walden
Affiliation:
Protochips Inc., 3800 Gateway Centre Blvd, Suite 306, Morrisville, NC27560, USA
Nelson L. Marthe
Affiliation:
Protochips Inc., 3800 Gateway Centre Blvd, Suite 306, Morrisville, NC27560, USA
Abhaya K. Datye
Affiliation:
Chemical and Biological Engineering, University of New Mexico, MSC01 1120, Albuquerque, NM87131, USA
Wilbur C. Bigelow
Affiliation:
Department of Materials Science and Engineering, University of Michigan, Dow Bldg., Hayward Ave., Ann Arbor, MI48109, USA
Lawrence F. Allard
Affiliation:
Center for Nanophase Materials Sciences Division, Oak Ridge National Laboratory, 1 Bethel Valley Rd, Oak Ridge, TN37831, USA
*
*Author for correspondence: Kinga A. Unocic, E-mail: unocicka@ornl.gov
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Abstract

Protocols for conducting in situ transmission electron microscopy (TEM) reactions using an environmental TEM with dry gases have been well established. However, many important reactions that are relevant to catalysis or high-temperature oxidation occur at atmospheric pressure and are influenced by the presence of water vapor. These experiments necessitate using a closed-cell gas reaction TEM holder. We have developed protocols for introducing and controlling water vapor concentrations in experimental gases from 2% at a full atmosphere to 100% at ~17 Torr, while measuring the gas composition using a residual gas analyzer (RGA) on the return side of the in situ gas reactor holder. Initially, as a model system, cube-shaped MgO crystals were used to help develop the protocols for handling the water vapor injection process and confirming that we could successfully inject water vapor into the gas cell. The interaction of water vapor with MgO triggered surface morphological and chemical changes as a result of the formation of Mg(OH)2, later validated with mass spectra obtained with our RGA system with and without water vapor. Integrating an RGA with an in situ scanning/TEM closed-cell gas reaction system can thus provide critical measurements correlating gas composition with dynamic surface restructuring of materials during reactions.

Keywords

closed-cell gas reaction systemin situ STEMMgOresidual gas analyzerwater vapor
Type
Software and Instrumentation
Information
Microscopy and Microanalysis , Volume 26 , Issue 2 , April 2020 , pp. 229 - 239
Copyright
Copyright © Microscopy Society of America 2020

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