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Title: The Role of Gas in Determining Image Quality and Resolution During In Situ Scanning Transmission Electron Microscopy Experiments

Abstract

As gas-solid heterogeneous catalytic reactions are molecular in nature, a full mechanistic understanding of the process requires atomic scale characterization under realistic operating conditions. While atomic resolution imaging has become a routine in modern high-vacuum (scanning) transmission electron microscopy ((S)TEM), both image quality and resolution nominally degrade when reaction gases are introduced. In this work, we systematically assess the effects of different gases at various pressures on the quality and resolution of images obtained at room temperature in the annular dark field STEM imaging mode using a differentially pumped (DP) gas cell. This imaging mode is largely free from inelastic scattering effects induced by the presence of gases and retains good imaging properties over a wide range of gas mass/pressures. We demonstrate the application of the ESTEM with atomic resolution images of a complex oxide alkane oxidation catalyst MoVNbTeOx (M1) immersed in light and heavy gas environments.

Authors:
ORCiD logo [1];  [2]
  1. Physical & Computational Science Directorate, Pacific Northwest National Laboratory, Richland WA 99352 USA
  2. Physical & Computational Science Directorate, Pacific Northwest National Laboratory, Richland WA 99352 USA; Department of Materials Science and Engineering, University of Washington, Seattle WA 98195 USA
Publication Date:
Research Org.:
Pacific Northwest National Laboratory (PNNL), Richland, WA (US), Environmental Molecular Sciences Laboratory (EMSL)
Sponsoring Org.:
USDOE
OSTI Identifier:
1406798
Report Number(s):
PNNL-SA-126401
Journal ID: ISSN 1867-3880; 48583
DOE Contract Number:  
AC05-76RL01830
Resource Type:
Journal Article
Journal Name:
ChemCatChem
Additional Journal Information:
Journal Volume: 9; Journal Issue: 18; Journal ID: ISSN 1867-3880
Publisher:
ChemPubSoc Europe
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; gas-solid reactions; environmental scanning; transmission electron microscopy; gas atmosphere; sample; SNR; Image resolution; Environmental Molecular Sciences Laboratory

Citation Formats

Zhu, Yuanyuan, and Browning, Nigel D. The Role of Gas in Determining Image Quality and Resolution During In Situ Scanning Transmission Electron Microscopy Experiments. United States: N. p., 2017. Web. doi:10.1002/cctc.201700474.
Zhu, Yuanyuan, & Browning, Nigel D. The Role of Gas in Determining Image Quality and Resolution During In Situ Scanning Transmission Electron Microscopy Experiments. United States. doi:10.1002/cctc.201700474.
Zhu, Yuanyuan, and Browning, Nigel D. Wed . "The Role of Gas in Determining Image Quality and Resolution During In Situ Scanning Transmission Electron Microscopy Experiments". United States. doi:10.1002/cctc.201700474.
@article{osti_1406798,
title = {The Role of Gas in Determining Image Quality and Resolution During In Situ Scanning Transmission Electron Microscopy Experiments},
author = {Zhu, Yuanyuan and Browning, Nigel D.},
abstractNote = {As gas-solid heterogeneous catalytic reactions are molecular in nature, a full mechanistic understanding of the process requires atomic scale characterization under realistic operating conditions. While atomic resolution imaging has become a routine in modern high-vacuum (scanning) transmission electron microscopy ((S)TEM), both image quality and resolution nominally degrade when reaction gases are introduced. In this work, we systematically assess the effects of different gases at various pressures on the quality and resolution of images obtained at room temperature in the annular dark field STEM imaging mode using a differentially pumped (DP) gas cell. This imaging mode is largely free from inelastic scattering effects induced by the presence of gases and retains good imaging properties over a wide range of gas mass/pressures. We demonstrate the application of the ESTEM with atomic resolution images of a complex oxide alkane oxidation catalyst MoVNbTeOx (M1) immersed in light and heavy gas environments.},
doi = {10.1002/cctc.201700474},
journal = {ChemCatChem},
issn = {1867-3880},
number = 18,
volume = 9,
place = {United States},
year = {2017},
month = {8}
}

Works referenced in this record:

Advances in atomic resolution in situ environmental transmission electron microscopy and 1Å aberration corrected in situ electron microscopy
journal, March 2009

  • Gai, Pratibha L.; Boyes, Edward D.
  • Microscopy Research and Technique, Vol. 72, Issue 3
  • DOI: 10.1002/jemt.20668

Atomic-resolution chemical analysis using a scanning transmission electron microscope
journal, November 1993

  • Browning, N. D.; Chisholm, M. F.; Pennycook, S. J.
  • Nature, Vol. 366, Issue 6451
  • DOI: 10.1038/366143a0

In situ and operando transmission electron microscopy of catalytic materials
journal, January 2015


The Merits of Static and Dynamic High-Resolution Electron Microscopy (HREM) for the Study of Solid Catalysts
journal, July 2010


Gas Reactor for Hot Stage Transmission Electron Microscopy
journal, September 1964

  • Gallegos, E. J.
  • Review of Scientific Instruments, Vol. 35, Issue 9
  • DOI: 10.1063/1.1718978

Electron Microscopic Observation of Specimens Under Controlled gas Pressure
journal, April 1962


In Situ TEM Study of Catalytic Nanoparticle Reactions in Atmospheric Pressure Gas Environment
journal, September 2013

  • Xin, Huolin L.; Niu, Kaiyang; Alsem, Daan Hein
  • Microscopy and Microanalysis, Vol. 19, Issue 6
  • DOI: 10.1017/S1431927613013433

On the role of the gas environment, electron-dose-rate, and sample on the image resolution in transmission electron microscopy
journal, May 2016

  • Ek, Martin; Jespersen, Sebastian P. F.; Damsgaard, Christian D.
  • Advanced Structural and Chemical Imaging, Vol. 2, Issue 1
  • DOI: 10.1186/s40679-016-0018-x

Atom-Resolved Imaging of Dynamic Shape Changes in Supported Copper Nanocrystals
journal, March 2002


Dynamical Observation and Detailed Description of Catalysts under Strong Metal–Support Interaction
journal, June 2016


Image resolution and sensitivity in an environmental transmission electron microscope
journal, November 2012


State of the art in atomic resolution off-axis electron holography
journal, May 2012


Simultaneous atomic-resolution electron ptychography and Z-contrast imaging of light and heavy elements in complex nanostructures
journal, August 2016

  • Yang, H.; Rutte, R. N.; Jones, L.
  • Nature Communications, Vol. 7, Issue 1
  • DOI: 10.1038/ncomms12532

Implementing an accurate and rapid sparse sampling approach for low-dose atomic resolution STEM imaging
journal, October 2016

  • Kovarik, L.; Stevens, A.; Liyu, A.
  • Applied Physics Letters, Vol. 109, Issue 16
  • DOI: 10.1063/1.4965720

Aberration corrected and monochromated environmental transmission electron microscopy: challenges and prospects for materials science
journal, November 2010


Quantitative Z-contrast imaging in the scanning transmission electron microscope with size-selected clusters
journal, August 2011


Visualizing Gas Molecules Interacting with Supported Nanoparticulate Catalysts at Reaction Conditions
journal, January 2012


High voltage electron microscopy of environmental reactions
journal, January 1973


Observing gas-catalyst dynamics at atomic resolution and single-atom sensitivity
journal, January 2015


Atomic-scale electron microscopy at ambient pressure
journal, August 2008


Visualisation of single atom dynamics and their role in nanocatalysts under controlled reaction environments
journal, January 2014


Interface lattice displacement measurement to 1pm by geometric phase analysis on aberration-corrected HAADF STEM images
journal, September 2013


An atomic oxygen environmental cell for a transmission electron microscope
journal, July 1990

  • Rodriguez, N. M.; Oh, S. G.; Downs, W. B.
  • Review of Scientific Instruments, Vol. 61, Issue 7
  • DOI: 10.1063/1.1141109

Environmental high resolution electron microscopy and applications to chemical science
journal, June 1997


Visualizing reacting single atoms in chemical reactions: Advancing the frontiers of materials research
journal, July 2015


Influence of total beam current on HRTEM image resolution in differentially pumped ETEM with nitrogen gas
journal, January 2013


High-resolution environmental transmission electron microscopy: modeling and experimental verification
journal, February 2013

  • Suzuki, Makoto; Yaguchi, Toshie; Zhang, Xiao Feng
  • Microscopy, Vol. 62, Issue 4
  • DOI: 10.1093/jmicro/dft001

Towards full-structure determination of bimetallic nanoparticles with an aberration-corrected electron microscope
journal, November 2010

  • Ortalan, Volkan; Uzun, Alper; Gates, Bruce C.
  • Nature Nanotechnology, Vol. 5, Issue 12
  • DOI: 10.1038/nnano.2010.234

Feature Adaptive Sampling for Scanning Electron Microscopy
journal, May 2016

  • Dahmen, Tim; Engstler, Michael; Pauly, Christoph
  • Scientific Reports, Vol. 6, Issue 1
  • DOI: 10.1038/srep25350

In situ synthesis and characterization of Ru promoted Co/Al2O3 Fischer–Tropsch catalysts
journal, July 2006


High Temperature Gas Reaction Specimen Chamber for an Electron Microscope
journal, August 1968

  • Hashimoto, Hatsujiro; Naiki, Toshio; Eto, Terukazu
  • Japanese Journal of Applied Physics, Vol. 7, Issue 8
  • DOI: 10.1143/JJAP.7.946