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Analysis of Catalytic Gas Products Using Electron Energy-Loss Spectroscopy and Residual Gas Analysis for Operando Transmission Electron Microscopy

Published online by Cambridge University Press:  12 May 2014

Benjamin K. Miller  and
Peter A. Crozier
Benjamin K. Miller
Affiliation:
School for Engineering of Matter, Transport and Energy, Arizona State University, Tempe, AZ 85287-6106, USA
Peter A. Crozier*
Affiliation:
School for Engineering of Matter, Transport and Energy, Arizona State University, Tempe, AZ 85287-6106, USA
*
*Corresponding author. crozier@asu.edu
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Abstract

Operando transmission electron microscopy (TEM) of catalytic reactions requires that the gas composition inside the TEM be known during the in situ reaction. Two techniques for measuring gas composition inside the environmental TEM are described and compared here. First, electron energy-loss spectroscopy, both in the low-loss and core-loss regions of the spectrum was utilized. The data were quantified using a linear combination of reference spectra from individual gasses to fit a mixture spectrum. Mass spectrometry using a residual gas analyzer was also used to quantify the gas inside the environmental cell. Both electron energy-loss spectroscopy and residual gas analysis were applied simultaneously to a known 50/50 mixture of CO and CO2, so the results from the two techniques could be compared and evaluated. An operando TEM experiment was performed using a Ru catalyst supported on silica spheres and loaded into the TEM on a specially developed porous pellet TEM sample. Both techniques were used to monitor the conversion of CO to CO2 over the catalyst, while simultaneous atomic resolution imaging of the catalyst was performed.

Keywords

operandoin situ TEMenvironmental TEM (ETEM)mass spectrometryEELScatalyst
Type
EDGE Special Issue
Information
Microscopy and Microanalysis , Volume 20 , Issue 3 , June 2014 , pp. 815 - 824
Copyright
© Microscopy Society of America 2014 

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