Behavior of Au Species in Au/Fe2O3 Catalysts Characterized by Novel In Situ Heating Techniques and Aberration-Corrected STEM Imaging

Allard, Lawrence F.; Flytzani-Stephanopoulos, Maria; Overbury, Steven H.

doi:10.1017/S1431927610013486

Behavior of Au Species in Au/Fe₂O₃ Catalysts Characterized by Novel In Situ Heating Techniques and Aberration-Corrected STEM Imaging

Journal Article · Tue Jun 01 04:00:00 EDT 2010 · Microscopy and Microanalysis

DOI:https://doi.org/10.1017/S1431927610013486· OSTI ID:1364256

Allard, Lawrence F. ^[1]; Flytzani-Stephanopoulos, Maria ^[2]; Overbury, Steven H. ^[1]

Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Tufts Univ., Medford, MA (United States). Dept. of Chemical and Biological Engineering

The recent advent of a novel design of in situ heating technology for electron microscopes has permitted unprecedented control of elevated temperature studies of catalytic materials, particularly when coupled with the sub- ngstr m imaging performance of a modern aberration-corrected scanning transmission electron microscope (STEM). In using micro-electro-mechanical-systems (MEMS)-based Aduro heating chips from Protochips, Inc. (Raleigh, NC, USA) it allows nearly instantaneous heating and cooling of catalyst powders, while avoiding the effects of temperature ramping as experienced with standard heating stages. The heating technology also provides stable operation limited only by the inherent drift in the microscope stage, thus allowing full image resolution to be achieved even at elevated temperatures. Our study details the use of both the high X-Y spatial resolution in both dark-field and simultaneous bright-field imaging, along with the high resolution in Z (depth sectioning) provided by the large probe incidence semiangle in the aberration-corrected instrument, to characterize the evolution of microstructure in a commercial Au/Fe₂O₃ water-gas shift catalyst during elevated temperature treatment. The phenomenon of Au diffusion to the surface of hematite support particles to form discrete crystalline Au nanoparticles in the 1-2 nm size range, after a prior leaching treatment to remove surface Au species has been characterized.

Research Organization:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States). High Temperature Materials Laboratory (HTML)

Sponsoring Organization:: USDOE Office of Energy Efficiency and Renewable Energy (EERE)

DOE Contract Number:: AC05-00OR22725

OSTI ID:: 1364256

Journal Information:: Microscopy and Microanalysis, Journal Name: Microscopy and Microanalysis Journal Issue: 04 Vol. 16; ISSN 1431-9276; ISSN applab

Publisher:: Microscopy Society of America (MSA)

Country of Publication:: United States

Language:: English

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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
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Behavior of Au Species in Au/Fe2O3 Catalysts Characterized by Novel In Situ Heating Techniques and Aberration-Corrected STEM Imaging

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Behavior of Au Species in Au/Fe₂O₃ Catalysts Characterized by Novel In Situ Heating Techniques and Aberration-Corrected STEM Imaging