Universal liquid sample device and process for high resolution transmission electron microscope imaging and multimodal analyses of liquid sample materials

Yu, Xiao-Ying; Kovarik, Libor; Arey, Bruce W.

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Title: Universal liquid sample device and process for high resolution transmission electron microscope imaging and multimodal analyses of liquid sample materials

Abstract

Liquid sample imaging devices and processes are disclosed for high resolution TEM imaging and multimodal analyses of liquid sample materials in situ under high vacuum that are compatible with standard type TEM chip membranes and TEM sample holders allowing TEM liquid sample imaging to be performed wherever a TEM instrument is accessible and at a substantially reduced cost compared to prior art systems and approaches.

Inventors:: Yu, Xiao-Ying; Kovarik, Libor; Arey, Bruce W.

Issue Date:: 2020-03-24

Research Org.:: Pacific Northwest National Laboratory (PNNL), Richland, WA (United States)

Sponsoring Org.:: USDOE

OSTI Identifier:: 1637801

Patent Number(s):: 10598609

Application Number:: 15/483,939

Assignee:: Battelle Memorial Institute (Richland, WA)

Patent Classifications (CPCs):: G - PHYSICS G01 - MEASURING G01N - INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES

H - ELECTRICITY H01 - BASIC ELECTRIC ELEMENTS H01J - ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS

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G - PHYSICS G01 - MEASURING G01N - INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
G01N23/02 - by transmitting the radiation through the material
G01N23/2204 - Specimen supports therefor

H - ELECTRICITY H01 - BASIC ELECTRIC ELEMENTS H01J - ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
H01J2237/2802 - Transmission microscopes
H01J37/16 - Vessels
H01J37/20 - Means for supporting or positioning the objects or the material
H01J37/26 - Electron or ion microscopes

Show less

DOE Contract Number:: AC05-76RL01830

Resource Type:: Patent

Resource Relation:: Patent File Date: 04/10/2017

Country of Publication:: United States

Language:: English

Subject:: 36 MATERIALS SCIENCE; 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

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                    Yu, Xiao-Ying, Kovarik, Libor, and Arey, Bruce W. Universal liquid sample device and process for high resolution transmission electron microscope imaging and multimodal analyses of liquid sample materials.  United States: N. p., 2020. 
        Web.

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                    Yu, Xiao-Ying, Kovarik, Libor, & Arey, Bruce W. Universal liquid sample device and process for high resolution transmission electron microscope imaging and multimodal analyses of liquid sample materials.  United States.

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                    Yu, Xiao-Ying, Kovarik, Libor, and Arey, Bruce W. Tue .  
        "Universal liquid sample device and process for high resolution transmission electron microscope imaging and multimodal analyses of liquid sample materials".  United States.  https://www.osti.gov/servlets/purl/1637801.

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@article{osti_1637801,

  title        = {Universal liquid sample device and process for high resolution transmission electron microscope imaging and multimodal analyses of liquid sample materials},

  author       = {Yu, Xiao-Ying and Kovarik, Libor and Arey, Bruce W.},

  abstractNote = {Liquid sample imaging devices and processes are disclosed for high resolution TEM imaging and multimodal analyses of liquid sample materials in situ under high vacuum that are compatible with standard type TEM chip membranes and TEM sample holders allowing TEM liquid sample imaging to be performed wherever a TEM instrument is accessible and at a substantially reduced cost compared to prior art systems and approaches.},

  doi          = {},

  journal      = {},
number       = ,

  volume       = ,

  place        = {United States},

  year         = {2020},

  month        = {3}

}

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Patent Reed, Bryan W.; DeHope, William J.; Huete, Glenn; ...

An electron microscope is disclosed which has a laser-driven photocathode and an arbitrary waveform generator (AWG) laser system ("laser"). The laser produces a train of temporally-shaped laser pulses of a predefined pulse duration and waveform, and directs the laser pulses to the laser-driven photocathode to produce a train of electron pulses. An image sensor is used along with a deflector subsystem. The deflector subsystem is arranged downstream of the target but upstream of the image sensor, and has two pairs of plates arranged perpendicular to one another. A control system controls the laser and a plurality of switching components synchronizedmore » « less
Full Text Available
High-speed multi-frame dynamic transmission electron microscope image acquisition system with arbitrary timing

Patent Reed, Bryan W.; DeHope, William J.; Huete, Glenn; ...

An electron microscope is disclosed which has a laser-driven photocathode and an arbitrary waveform generator (AWG) laser system ("laser"). The laser produces a train of temporally-shaped laser pulses each being of a programmable pulse duration, and directs the laser pulses to the laser-driven photocathode to produce a train of electron pulses. An image sensor is used along with a deflector subsystem. The deflector subsystem is arranged downstream of the target but upstream of the image sensor, and has a plurality of plates. A control system having a digital sequencer controls the laser and a plurality of switching components, synchronized withmore » « less
Full Text Available
High-speed multiframe dynamic transmission electron microscope image acquisition system with arbitrary timing

Patent Reed, Bryan W.; Dehope, William J; Huete, Glenn; ...

An electron microscope is disclosed which has a laser-driven photocathode and an arbitrary waveform generator (AWG) laser system ("laser"). The laser produces a train of temporally-shaped laser pulses of a predefined pulse duration and waveform, and directs the laser pulses to the laser-driven photocathode to produce a train of electron pulses. An image sensor is used along with a deflector subsystem. The deflector subsystem is arranged downstream of the target but upstream of the image sensor, and has two pairs of plates arranged perpendicular to one another. A control system controls the laser and a plurality of switching components synchronizedmore » « less
Full Text Available

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Title: Universal liquid sample device and process for high resolution transmission electron microscope imaging and multimodal analyses of liquid sample materials

Abstract

Citation Formats

Positioning and electrophysiological characterization of individual cells and reconstituted membrane systems on microstructured carriers patent, July 2004

Cyclic voltammetry at gold single-crystal surfaces. Part 2. Behaviour of high-index faces journal, May 1996

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Interfacial structure of iodine electrodeposited on Au(111): studies by LEED and in situ STM journal, July 1995

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Measurement of three-dimensional microstructure in a LiCoO2 positive electrode journal, April 2011

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In situ x-ray-diffraction and -reflectivity studies of the Au(111)/electrolyte interface: Reconstruction and anion adsorption journal, October 1992

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Multiaperture sample positioning and analysis system patent, April 2007

Retainer made of synthetic resin for use in ball bearing and ball bearing patent, May 2015

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In situ x-ray standing-wave analysis of electrodeposited Cu monolayers on GaAs(001) journal, October 1998

Iodide adsorption at the Au(111) electrode surface journal, June 1999

Sample Holder, Method for Observation and Inspection, and Apparatus for Observation and Inspection patent-application, July 2009

Method for Operating a Battery patent-application, June 2012

Simultaneous determination of both the calibration constant in an electrochemical quartz crystal microbalance and the active surface area of a polycrystalline gold electrode journal, January 2000

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In situ X-ray diffraction and X-ray absorption studies of high-rate lithium-ion batteries journal, January 2001

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Systems and methods for analyzing liquids under vacuum patent, October 2013

Imaging liquids using microfluidic cells journal, May 2013

X-Ray Structural Analysis of Semiconductor-Electrolyte Interfaces conference, August 2003

Cell for Simultaneous Synchrotron Radiation X-ray and Electrochemical Corrosion Measurements on Cultural Heritage Metals and Other Materials journal, May 2006

In situ scanning tunneling microscopy of underpotential and bulk deposition of silver on gold (111) journal, July 1995

A novel thick-layer electrochemical cell for in situ x-ray diffraction journal, February 1998

Electron microscope sample holder for forming a gas or liquid cell with two semiconductor devices patent, April 2016

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Molecular level studies of solid-gas and solid-liquid interfaces journal, July 1995

Transmission-Geometry Electrochemical Cell for In-Situ Scattering and Spectroscopy Investigations patent-application, April 2014

Device and Method for the Examination of Samples in a Non-Vacuum Environment Using a Scanning Electron Microscope patent-application, March 2004

Microbioreactor for Continuous Cell Culture patent-application, September 2006

Method of use of reusable sample holding device permitting ready loading of very small wet samples patent, January 2012

Development of an Automated Digestion and Droplet Deposition Microfluidic Chip for MALDI-TOF MS journal, July 2008

Sensitivity of Electrochemical Adlayer Structure to the Metal Crystallographic Orientation: Potential-Dependent Iodide Adsorption on Au(100) in Comparison with Other Low-Index Surfaces journal, August 1994

Advances in sealed liquid cells for in-situ TEM electrochemial investigation of lithium-ion battery journal, January 2015

Atomic Level Characterization of the Iodine-Modified Au(111) Electrode Surface in Perchloric Acid Solution by in-Situ STM and ex-Situ LEED journal, November 1995

Specimen Box for Electron Microscope Capable of Observing General Specimen and Live Cell patent-application, June 2007

Optical Measuring Instrument, and Wavelength Calibration Method and Optical Measuring Method for Light Detector patent-application, December 2009

Flow Cells for Electron Microscope Imaging with Multiple Flow Streams patent-application, November 2012

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Relating the in-situ, ex-situ, and non-situ environments in surface electrochemistry journal, July 1995

Structure of Electrochemically Deposited Iodine Adlayer on Au(111) Studied by Ultrahigh-Vacuum Instrumentation and in Situ STM journal, May 1995

Electrochemical Quartz Crystal Microbalance Study of Halide Adsorption and Concomitant Change of Surface Excess of Water on Highly Ordered Au(111) journal, June 1997

Optical Characterisation Methods and Systems patent-application, December 2009

Inspection method and reagent solution patent, March 2011

Determination of the surface area of gold electrodes by iodine chemisorption journal, September 1987

In situ X-ray analysis under controlled potential conditions: An innovative setup and its application to the investigation of ultrathin films electrodeposited on Ag(111) journal, July 2006

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A Rotating Ball Inlet for On-Line MALDI Mass Spectrometry journal, January 2000

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An Electrochemical Cell for Operando Study of Lithium Batteries Using Synchrotron Radiation journal, January 2010

Structure and electrocompression of electrodeposited iodine monolayers on gold (111) journal, January 1994

Chemistry and physics of the ‘‘liquid’’/solid interface: A surface science perspective journal, July 1993

Method of Use of Reusable Sample Holding Device Permitting Ready Loading of Very Small Wet Samples patent-application, January 2012

A study of iodine adlayers on polycrystalline gold electrodes by in situ electrochemical Rutherford backscattering (ECRBS) journal, February 2009

Positioning and electrophysiological characterization of individual cells and reconstituted membrane systems on microstructured carriers
patent, July 2004

Cyclic voltammetry at gold single-crystal surfaces. Part 2. Behaviour of high-index faces
journal, May 1996

Concepts, instruments, and model systems that enabled the rapid evolution of surface science
journal, June 2009

Charged Particle Beam Device and Filter Member
patent-application, March 2016

Surface analysis spectroscopy apparatus
patent, August 1989

Reusable sample holding device permitting ready loading of very small wet samples
patent, November 2011

Probing electrode surface chemical composition with core and valence band photoemission and an anaerobic cell
journal, March 1998

Surface Sensitivity in Cluster-Ion-Induced Sputtering
journal, June 2006

Microfluidic electrochemical device and process for chemical imaging and electrochemical analysis at the electrode-liquid interface in-situ
patent, March 2016

Interfacial structure of iodine electrodeposited on Au(111): studies by LEED and in situ STM
journal, July 1995

Making a hybrid microfluidic platform compatible for in situ imaging by vacuum-based techniques
journal, November 2011

Measurement of three-dimensional microstructure in a LiCoO2 positive electrode
journal, April 2011

Sample positioning and analysis system
patent, June 2008

Impact of surface chemistry
journal, September 2010

Reflection-mode x-ray powder diffraction cell for in situ studies of electrochemical reactions
journal, May 2004

Apparatus and Method for Non-Contact Microfluidic Sample Manipulation
patent-application, November 2007

On-Line MALDI-TOF MS Using a Continuous Vacuum Deposition Interface
journal, December 1998

In situ x-ray-diffraction and -reflectivity studies of the Au(111)/electrolyte interface: Reconstruction and anion adsorption
journal, October 1992

Identification of Endothelial Proteins by MALDI-MS Using a Compact Disc Microfluidic System
journal, May 2004

Multiaperture sample positioning and analysis system
patent, April 2007

Retainer made of synthetic resin for use in ball bearing and ball bearing
patent, May 2015

Poly(dimethylsiloxane) as a Material for Fabricating Microfluidic Devices
journal, April 2002

In situ x-ray standing-wave analysis of electrodeposited Cu monolayers on GaAs(001)
journal, October 1998

Iodide adsorption at the Au(111) electrode surface
journal, June 1999

Sample Holder, Method for Observation and Inspection, and Apparatus for Observation and Inspection
patent-application, July 2009

Method for Operating a Battery
patent-application, June 2012

Simultaneous determination of both the calibration constant in an electrochemical quartz crystal microbalance and the active surface area of a polycrystalline gold electrode
journal, January 2000

Oxford style sample cup
patent, March 2017

In situ X-ray diffraction and X-ray absorption studies of high-rate lithium-ion batteries
journal, January 2001

Analytical chip, analytical-chip unit, and analysis apparatus
patent, April 2007

On-line single droplet deposition for MALDI mass spectrometry
journal, October 2004

Systems and methods for analyzing liquids under vacuum
patent, October 2013

Imaging liquids using microfluidic cells
journal, May 2013

X-Ray Structural Analysis of Semiconductor-Electrolyte Interfaces
conference, August 2003

Cell for Simultaneous Synchrotron Radiation X-ray and Electrochemical Corrosion Measurements on Cultural Heritage Metals and Other Materials
journal, May 2006

In situ scanning tunneling microscopy of underpotential and bulk deposition of silver on gold (111)
journal, July 1995

A novel thick-layer electrochemical cell for in situ x-ray diffraction
journal, February 1998

Electron microscope sample holder for forming a gas or liquid cell with two semiconductor devices
patent, April 2016

Manufacturing Method of Chemical Battery Electrode and Battery
patent-application, October 2005

Introductory lecture. Studies of the liquid/solid interface by scanning tunnelling microscopy and scanning electrochemical microscopy
journal, January 1992

Performance of a microfluidic device for in situ ToF-SIMS analysis of selected organic molecules at aqueous surfaces
journal, January 2013

In situ SEM and ToF-SIMS analysis of IgG conjugated gold nanoparticles at aqueous surfaces : In situ SEM and ToF-SIMS analysis of aqueous Au nanoparticles
journal, March 2013

Electrophoresis Separation in Open Microchannels. A Method for Coupling Electrophoresis with MALDI-MS
journal, May 2001

Molecular level studies of solid-gas and solid-liquid interfaces
journal, July 1995

Transmission-Geometry Electrochemical Cell for In-Situ Scattering and Spectroscopy Investigations
patent-application, April 2014

Device and Method for the Examination of Samples in a Non-Vacuum Environment Using a Scanning Electron Microscope
patent-application, March 2004

Microbioreactor for Continuous Cell Culture
patent-application, September 2006

Method of use of reusable sample holding device permitting ready loading of very small wet samples
patent, January 2012

Development of an Automated Digestion and Droplet Deposition Microfluidic Chip for MALDI-TOF MS
journal, July 2008

Sensitivity of Electrochemical Adlayer Structure to the Metal Crystallographic Orientation: Potential-Dependent Iodide Adsorption on Au(100) in Comparison with Other Low-Index Surfaces
journal, August 1994

Advances in sealed liquid cells for in-situ TEM electrochemial investigation of lithium-ion battery
journal, January 2015

Atomic Level Characterization of the Iodine-Modified Au(111) Electrode Surface in Perchloric Acid Solution by in-Situ STM and ex-Situ LEED
journal, November 1995

Specimen Box for Electron Microscope Capable of Observing General Specimen and Live Cell
patent-application, June 2007

Optical Measuring Instrument, and Wavelength Calibration Method and Optical Measuring Method for Light Detector
patent-application, December 2009

Flow Cells for Electron Microscope Imaging with Multiple Flow Streams
patent-application, November 2012

Cyclic voltammetry at gold single-crystal surfaces. Part 1. Behaviour at low-index faces
journal, May 1996

Relating the in-situ, ex-situ, and non-situ environments in surface electrochemistry
journal, July 1995

Structure of Electrochemically Deposited Iodine Adlayer on Au(111) Studied by Ultrahigh-Vacuum Instrumentation and in Situ STM
journal, May 1995

Electrochemical Quartz Crystal Microbalance Study of Halide Adsorption and Concomitant Change of Surface Excess of Water on Highly Ordered Au(111)
journal, June 1997

Optical Characterisation Methods and Systems
patent-application, December 2009

Inspection method and reagent solution
patent, March 2011

Determination of the surface area of gold electrodes by iodine chemisorption
journal, September 1987

In situ X-ray analysis under controlled potential conditions: An innovative setup and its application to the investigation of ultrathin films electrodeposited on Ag(111)
journal, July 2006

Probing liquid surfaces under vacuum using SEM and ToF-SIMS
journal, January 2011

Multiaperture sample positioning and analysis system
patent, July 2007

Micro-Fluidic Test Apparatus and Method
patent-application, March 2008

Patterned Cell Network Substrate Interface and Methods and Uses Thereof
patent-application, October 2007

In situ scanning tunneling microscopy in electrolyte solutions
journal, July 1998

Systems and Methods for Analyzing Liquids under Vacuum
patent-application, September 2012

In situ molecular imaging of a hydrated biofilm in a microfluidic reactor by ToF-SIMS
journal, January 2014

A Rotating Ball Inlet for On-Line MALDI Mass Spectrometry
journal, January 2000

Liquid sample introduction for matrix-assisted laser desorption ionization
journal, September 1993

An Electrochemical Cell for Operando Study of Lithium Batteries Using Synchrotron Radiation
journal, January 2010

Structure and electrocompression of electrodeposited iodine monolayers on gold (111)
journal, January 1994

Chemistry and physics of the ‘‘liquid’’/solid interface: A surface science perspective
journal, July 1993

Method of Use of Reusable Sample Holding Device Permitting Ready Loading of Very Small Wet Samples
patent-application, January 2012

A study of iodine adlayers on polycrystalline gold electrodes by in situ electrochemical Rutherford backscattering (ECRBS)
journal, February 2009

Testing Apparatus Using Charged Particles and Device Manufacturing Method Using the Testing Apparatus
patent-application, March 2005

Reusable Sample Holding Device Permitting Ready Loading of Very Small Wet Samples
patent-application, August 2010