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Revealing Correlation of Valence State with Nanoporous Structure in Cobalt Catalyst Nanoparticles by In Situ Environmental TEM

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† Materials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, California 94720, United States,
‡ Center for Functional Nanomaterials, Brookhaven National Laboratory, Upton, New York 11973, United States
*Address correspondence to [email protected]
Cite this: ACS Nano 2012, 6, 5, 4241–4247
Publication Date (Web):April 11, 2012
https://doi.org/10.1021/nn3007652
Copyright © 2012 American Chemical Society
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    Simultaneously probing the electronic structure and morphology of materials at the nanometer or atomic scale while a chemical reaction proceeds is significant for understanding the underlying reaction mechanisms and optimizing a materials design. This is especially important in the study of nanoparticle catalysts, yet such experiments have rarely been achieved. Utilizing an environmental transmission electron microscope equipped with a differentially pumped gas cell, we are able to conduct nanoscopic imaging and electron energy loss spectroscopy in situ for cobalt catalysts under reaction conditions. Studies reveal quantitative correlation of the cobalt valence states with the particles’ nanoporous structures. The in situ experiments were performed on nanoporous cobalt particles coated with silica, while a 15 mTorr hydrogen environment was maintained at various temperatures (300–600 °C). When the nanoporous particles were reduced, the valence state changed from cobalt oxide to metallic cobalt and concurrent structural coarsening was observed. In situ mapping of the valence state and the corresponding nanoporous structures allows quantitative analysis necessary for understanding and improving the mass activity and lifetime of cobalt-based catalysts, for example, for Fischer–Tropsch synthesis that converts carbon monoxide and hydrogen into fuels, and uncovering the catalyst optimization mechanisms.

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