Coupling EELS/EFTEM Imaging with Environmental Fluid Cell Microscopy

Unocic, Raymond R; Baggetto, Loic; Veith, Gabriel M; Dudney, Nancy J; More, Karren Leslie

doi:10.1017/S1431927612007374

Title: Coupling EELS/EFTEM Imaging with Environmental Fluid Cell Microscopy

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Abstract

Insight into dynamically evolving electrochemical reactions and mechanisms encountered in electrical energy storage (EES) and conversion technologies (batteries, fuel cells, and supercapacitors), materials science (corrosion and oxidation), and materials synthesis (electrodeposition) remains limited due to the present lack of in situ high-resolution characterization methodologies. Electrochemical fluid cell microscopy is an emerging in-situ method that allows for the direct, real-time imaging of electrochemical processes within a fluid environment. This technique is facilitated by the use of MEMS-based biasing microchip platforms that serve the purpose of sealing the highly volatile electrolyte between two electron transparent SiNx membranes and interfacing electrodes to an external potentiostat for controlled nanoscale electrochemislly experiments [!]. In order to elucidate both stmctural and chemical changes during such in situ electrochemical experiments, it is impmtant to first improve upon the spatial resolution by utilizing energy-filtered transmission electron microscopy (EFTEM) (to minimize chromatic aben ation), then to detennine the chemical changes via electron energy loss spectroscopy (EELS). This presents a formidable challenge since the overall thickness through which electrons are scattered through the multiple layers of the cell can be on the order of hundreds of nanometers to microns, scattering through which has the deleterious effect of degrading image resolutionmore »« less

Authors:

Unocic, Raymond R ^[1]; Baggetto, Loic ^[1]; Veith, Gabriel M ^[1]; Dudney, Nancy J ^[1]; More, Karren Leslie ^[1]

ORNL

Publication Date:: Sun Jan 01 00:00:00 EST 2012

Research Org.:: Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

Sponsoring Org.:: USDOE

OSTI Identifier:: 1068753

DOE Contract Number:: DE-AC05-00OR22725

Resource Type:: Journal Article

Journal Name:: Microscopy and Microanalysis

Additional Journal Information:: Journal Volume: 18; Journal Issue: S2; Journal ID: ISSN 1431--9276

Country of Publication:: United States

Language:: English

Citation Formats


                    Unocic, Raymond R, Baggetto, Loic, Veith, Gabriel M, Dudney, Nancy J, and More, Karren Leslie. Coupling EELS/EFTEM Imaging with Environmental Fluid Cell Microscopy.  United States: N. p., 2012. 
        Web.  doi:10.1017/S1431927612007374.

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                    Unocic, Raymond R, Baggetto, Loic, Veith, Gabriel M, Dudney, Nancy J, & More, Karren Leslie. Coupling EELS/EFTEM Imaging with Environmental Fluid Cell Microscopy.  United States.  https://doi.org/10.1017/S1431927612007374

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                    Unocic, Raymond R, Baggetto, Loic, Veith, Gabriel M, Dudney, Nancy J, and More, Karren Leslie. 2012.  
        "Coupling EELS/EFTEM Imaging with Environmental Fluid Cell Microscopy".  United States.  https://doi.org/10.1017/S1431927612007374.

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@article{osti_1068753,

  title        = {Coupling EELS/EFTEM Imaging with Environmental Fluid Cell Microscopy},

  author       = {Unocic, Raymond R and Baggetto, Loic and Veith, Gabriel M and Dudney, Nancy J and More, Karren Leslie},

  abstractNote = {Insight into dynamically evolving electrochemical reactions and mechanisms encountered in electrical energy storage (EES) and conversion technologies (batteries, fuel cells, and supercapacitors), materials science (corrosion and oxidation), and materials synthesis (electrodeposition) remains limited due to the present lack of in situ high-resolution characterization methodologies. Electrochemical fluid cell microscopy is an emerging in-situ method that allows for the direct, real-time imaging of electrochemical processes within a fluid environment. This technique is facilitated by the use of MEMS-based biasing microchip platforms that serve the purpose of sealing the highly volatile electrolyte between two electron transparent SiNx membranes and interfacing electrodes to an external potentiostat for controlled nanoscale electrochemislly experiments [!]. In order to elucidate both stmctural and chemical changes during such in situ electrochemical experiments, it is impmtant to first improve upon the spatial resolution by utilizing energy-filtered transmission electron microscopy (EFTEM) (to minimize chromatic aben ation), then to detennine the chemical changes via electron energy loss spectroscopy (EELS). This presents a formidable challenge since the overall thickness through which electrons are scattered through the multiple layers of the cell can be on the order of hundreds of nanometers to microns, scattering through which has the deleterious effect of degrading image resolution and decreasing signal-to noise for spectroscopy [2].},

  doi          = {10.1017/S1431927612007374},

  url          = {https://www.osti.gov/biblio/1068753},
  journal      = {Microscopy and Microanalysis},

  issn         = {1431--9276},

  number       = S2,

  volume       = 18,

  place        = {United States},

  year         = {Sun Jan 01 00:00:00 EST 2012},

  month        = {Sun Jan 01 00:00:00 EST 2012}

}

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