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Title: Cryogenic Specimens for Nanoscale Characterization of Solid-Liquid Interfaces

Abstract

New cryogenic characterization techniques for exploring the nanoscale structure and chemistry of intact solid-liquid interfaces have recently been developed. These techniques provide a high-resolution picture of buried interfaces from large samples or devices that cannot be obtained by other means. The advancement was enabled by the development of instrumentation for cryogenic focused ion beam lift-out, which allows extraction and preparation of intact electron-transparent solid-liquid interfaces from large samples for characterization by cryogenic scanning transmission electron microscopy or atom probe tomography. Future implementation of these techniques will complement current strides in imaging of materials in fluid environments by in-situ liquid phase electron microscopy, providing a more complete understanding of the morphology, surface chemistry, and dynamic processes that occur at solid-liquid interfaces.

Authors:
 [1];  [2];  [3];  [4]; ORCiD logo [5]
  1. Oak Ridge National Laboratory
  2. INM Leibniz Inst New Mat, Saarbrucken, Germany
  3. University of Oregon
  4. Sandia National Laboratory
  5. BATTELLE (PACIFIC NW LAB)
Publication Date:
Research Org.:
Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1580515
Report Number(s):
PNNL-SA-148424
DOE Contract Number:  
AC05-76RL01830
Resource Type:
Journal Article
Journal Name:
MRS Bulletin
Additional Journal Information:
Journal Volume: 44; Journal Issue: 12
Country of Publication:
United States
Language:
English
Subject:
focused ion beam (FIB), scanning transmission electron microscopy (STEM), atom probe tomography, fluid, solid liquid interfaces

Citation Formats

Zachman, Michael, De Jonge, Niels, Fischer, Robert, Jungjohann, Katherine L., and Perea, Daniel E. Cryogenic Specimens for Nanoscale Characterization of Solid-Liquid Interfaces. United States: N. p., 2019. Web. doi:10.1557/mrs.2019.289.
Zachman, Michael, De Jonge, Niels, Fischer, Robert, Jungjohann, Katherine L., & Perea, Daniel E. Cryogenic Specimens for Nanoscale Characterization of Solid-Liquid Interfaces. United States. doi:10.1557/mrs.2019.289.
Zachman, Michael, De Jonge, Niels, Fischer, Robert, Jungjohann, Katherine L., and Perea, Daniel E. Mon . "Cryogenic Specimens for Nanoscale Characterization of Solid-Liquid Interfaces". United States. doi:10.1557/mrs.2019.289.
@article{osti_1580515,
title = {Cryogenic Specimens for Nanoscale Characterization of Solid-Liquid Interfaces},
author = {Zachman, Michael and De Jonge, Niels and Fischer, Robert and Jungjohann, Katherine L. and Perea, Daniel E.},
abstractNote = {New cryogenic characterization techniques for exploring the nanoscale structure and chemistry of intact solid-liquid interfaces have recently been developed. These techniques provide a high-resolution picture of buried interfaces from large samples or devices that cannot be obtained by other means. The advancement was enabled by the development of instrumentation for cryogenic focused ion beam lift-out, which allows extraction and preparation of intact electron-transparent solid-liquid interfaces from large samples for characterization by cryogenic scanning transmission electron microscopy or atom probe tomography. Future implementation of these techniques will complement current strides in imaging of materials in fluid environments by in-situ liquid phase electron microscopy, providing a more complete understanding of the morphology, surface chemistry, and dynamic processes that occur at solid-liquid interfaces.},
doi = {10.1557/mrs.2019.289},
journal = {MRS Bulletin},
number = 12,
volume = 44,
place = {United States},
year = {2019},
month = {12}
}

Works referenced in this record:

Liquid-phase electron microscopy of molecular drug response in breast cancer cells reveals irresponsive cell subpopulations related to lack of HER2 homodimers
journal, November 2017

  • Peckys, Diana B.; Korf, Ulrike; Wiemann, Stefan
  • Molecular Biology of the Cell, Vol. 28, Issue 23
  • DOI: 10.1091/mbc.e17-06-0381

Calcium carbonate nucleation driven by ion binding in a biomimetic matrix revealed by in situ electron microscopy
journal, January 2015

  • Smeets, Paul J. M.; Cho, Kang Rae; Kempen, Ralph G. E.
  • Nature Materials, Vol. 14, Issue 4
  • DOI: 10.1038/nmat4193

Controlled Growth of Nanoparticles from Solution with In Situ Liquid Transmission Electron Microscopy
journal, July 2011

  • Evans, James E.; Jungjohann, Katherine L.; Browning, Nigel D.
  • Nano Letters, Vol. 11, Issue 7
  • DOI: 10.1021/nl201166k

Exploring the Formation of Symmetric Gold Nanostars by Liquid-Cell Transmission Electron Microscopy
journal, June 2017


Experimental procedures to mitigate electron beam induced artifacts during in situ fluid imaging of nanomaterials
journal, April 2013


Electron–Water Interactions and Implications for Liquid Cell Electron Microscopy
journal, September 2014

  • Schneider, Nicholas M.; Norton, Michael M.; Mendel, Brian J.
  • The Journal of Physical Chemistry C, Vol. 118, Issue 38
  • DOI: 10.1021/jp507400n

Imaging Protein Structure in Water at 2.7 nm Resolution by Transmission Electron Microscopy
journal, February 2012


Reduced Radiation Damage in Transmission Electron Microscopy of Proteins in Graphene Liquid Cells
journal, November 2018


Direct Detection Electron Energy-Loss Spectroscopy: A Method to Push the Limits of Resolution and Sensitivity
journal, August 2017


Electron microscopy of specimens in liquid
journal, October 2011

  • de Jonge, Niels; Ross, Frances M.
  • Nature Nanotechnology, Vol. 6, Issue 11, p. 695-704
  • DOI: 10.1038/nnano.2011.161

Enhanced Sensitivity of Atomic-Resolution Spectroscopic Imaging by Direct Electron Detection
journal, July 2017


Visualizing the interfacial evolution from charge compensation to metallic screening across the manganite metal–insulator transition
journal, March 2014

  • Mundy, Julia A.; Hikita, Yasuyuki; Hidaka, Takeaki
  • Nature Communications, Vol. 5, Issue 1
  • DOI: 10.1038/ncomms4464

Structure and bonding at the atomic scale by scanning transmission electron microscopy
journal, April 2009


Three-dimensional nanoscale characterisation of materials by atom probe tomography
journal, November 2016


In situ site-specific specimen preparation for atom probe tomography
journal, February 2007


Heterogeneous Two-Phase Pillars in Epitaxial NiFe 2 O 4 -LaFeO 3 Nanocomposites
journal, July 2017

  • Comes, Ryan B.; Perea, Daniel E.; Spurgeon, Steven R.
  • Advanced Materials Interfaces, Vol. 4, Issue 16
  • DOI: 10.1002/admi.201700396

Practical Aspects of Electrochemical Corrosion Measurements During In Situ Analytical Transmission Electron Microscopy (TEM) of Austenitic Stainless Steel in Aqueous Media
journal, August 2017

  • Schilling, Sibylle; Janssen, Arne; Zaluzec, Nestor J.
  • Microscopy and Microanalysis, Vol. 23, Issue 4
  • DOI: 10.1017/S1431927617012314

Dynamic microscopy of nanoscale cluster growth at the solid–liquid interface
journal, July 2003

  • Williamson, M. J.; Tromp, R. M.; Vereecken, P. M.
  • Nature Materials, Vol. 2, Issue 8
  • DOI: 10.1038/nmat944

A b i n i t i o calculations on the lithium fluoride–ethylene complex
journal, December 1977

  • Szczȩśniak, Mal/gorzata M.; Ratajczak, Henryk
  • The Journal of Chemical Physics, Vol. 67, Issue 11
  • DOI: 10.1063/1.434654

Observation and Quantification of Nanoscale Processes in Lithium Batteries by Operando Electrochemical (S)TEM
journal, February 2015


Studying localized corrosion using liquid cell transmission electron microscopy
journal, January 2015

  • Chee, See Wee; Pratt, Sarah H.; Hattar, Khalid
  • Chemical Communications, Vol. 51, Issue 1
  • DOI: 10.1039/C4CC06443G

A focused ion beam milling and lift-out approach for site-specific preparation of frozen-hydrated lamellas from multicellular organisms
journal, November 2015

  • Mahamid, Julia; Schampers, Ruud; Persoon, Hans
  • Journal of Structural Biology, Vol. 192, Issue 2
  • DOI: 10.1016/j.jsb.2015.07.012

Integrated Circuits Comprising Patterned Functional Liquids
journal, July 2018

  • Prasad, Bhagwati; Pfanzelt, Georg; Fillis-Tsirakis, Evangelos
  • Advanced Materials, Vol. 30, Issue 35
  • DOI: 10.1002/adma.201802598

Designer interphases for the lithium-oxygen electrochemical cell
journal, April 2017

  • Choudhury, Snehashis; Wan, Charles Tai-Chieh; Al Sadat, Wajdi I.
  • Science Advances, Vol. 3, Issue 4
  • DOI: 10.1126/sciadv.1602809

Cryomicrotomy applied to the preparation of frozen hydrated muscle tissue for transmission electron microscopy
journal, March 1977


Strategies for Preparing Graphene Liquid Cells for Transmission Electron Microscopy
journal, May 2018


Vitrification of pure Water for Electron Microscopy
journal, December 1981


Cryo-Electron Microscopy of Vitrified Water
journal, September 1984


Localized corrosion of low-carbon steel at the nanoscale
journal, April 2019

  • Hayden, Steven C.; Chisholm, Claire; Grudt, Rachael O.
  • npj Materials Degradation, Vol. 3, Issue 1
  • DOI: 10.1038/s41529-019-0078-1

Focused-ion-beam thinning of frozen-hydrated biological specimens for cryo-electron microscopy
journal, February 2007

  • Marko, Michael; Hsieh, Chyongere; Schalek, Richard
  • Nature Methods, Vol. 4, Issue 3
  • DOI: 10.1038/nmeth1014

The making of frozen-hydrated, vitreous lamellas from cells for cryo-electron microscopy
journal, November 2010

  • Hayles, Michael F.; Matthijs de Winter, D. A.; Schneijdenberg, Chris T. W. M.
  • Journal of Structural Biology, Vol. 172, Issue 2
  • DOI: 10.1016/j.jsb.2010.07.004

Cryo-STEM mapping of solid–liquid interfaces and dendrites in lithium-metal batteries
journal, August 2018


Electron ptychography of 2D materials to deep sub-ångström resolution
journal, July 2018


On the current role of atom probe tomography in materials characterization and materials science
journal, October 2013

  • Marquis, Emmanuelle A.; Bachhav, Mukesh; Chen, Yimeng
  • Current Opinion in Solid State and Materials Science, Vol. 17, Issue 5
  • DOI: 10.1016/j.cossms.2013.09.003

Site-specific 3D imaging of cells and tissues with a dual beam microscope
journal, July 2006

  • Heymann, Jurgen A. W.; Hayles, Mike; Gestmann, Ingo
  • Journal of Structural Biology, Vol. 155, Issue 1
  • DOI: 10.1016/j.jsb.2006.03.006

Local variations of HER2 dimerization in breast cancer cells discovered by correlative fluorescence and liquid electron microscopy
journal, July 2015

  • Peckys, Diana B.; Korf, Ulrike; de Jonge, Niels
  • Science Advances, Vol. 1, Issue 6
  • DOI: 10.1126/sciadv.1500165

Early-stage NiCrMo oxidation revealed by cryo-transmission electron microscopy
journal, May 2019


Making the practically impossible “Merely difficult”-Cryogenic FIB lift-out for “Damage free” soft matter imaging: FAST AND EFFICIENT CRYO LIFT-OUT AND TRANSFER TO TEM
journal, February 2016

  • Parmenter, Christopher D. J.; Fay, Michael W.; Hartfield, Cheryl
  • Microscopy Research and Technique, Vol. 79, Issue 4
  • DOI: 10.1002/jemt.22630

Probing bonding and electronic structure at atomic resolution with spectroscopic imaging
journal, January 2012


Observation of Single Colloidal Platinum Nanocrystal Growth Trajectories
journal, June 2009


High-Resolution EM of Colloidal Nanocrystal Growth Using Graphene Liquid Cells
journal, April 2012


Imaging the polymerization of multivalent nanoparticles in solution
journal, October 2017


Site-Specific Preparation of Intact Solid–Liquid Interfaces by Label-Free In Situ Localization and Cryo-Focused Ion Beam Lift-Out
journal, November 2016

  • Zachman, Michael J.; Asenath-Smith, Emily; Estroff, Lara A.
  • Microscopy and Microanalysis, Vol. 22, Issue 6
  • DOI: 10.1017/S1431927616011892

Electron microscopy of whole cells in liquid with nanometer resolution
journal, January 2009

  • Jonge, N. d.; Peckys, D. B.; Kremers, G. J.
  • Proceedings of the National Academy of Sciences, Vol. 106, Issue 7
  • DOI: 10.1073/pnas.0809567106

Lithium Self-Discharge and Its Prevention: Direct Visualization through In Situ Electrochemical Scanning Transmission Electron Microscopy
journal, September 2017

  • Harrison, Katharine L.; Zavadil, Kevin R.; Hahn, Nathan T.
  • ACS Nano, Vol. 11, Issue 11
  • DOI: 10.1021/acsnano.7b05513

Resolution and aberration correction in liquid cell transmission electron microscopy
journal, December 2018

  • de Jonge, Niels; Houben, Lothar; Dunin-Borkowski, Rafal E.
  • Nature Reviews Materials, Vol. 4, Issue 1
  • DOI: 10.1038/s41578-018-0071-2

Origin of H 2 Evolution in LIBs: H 2 O Reduction vs. Electrolyte Oxidation
journal, January 2016

  • Metzger, Michael; Strehle, Benjamin; Solchenbach, Sophie
  • Journal of The Electrochemical Society, Vol. 163, Issue 5
  • DOI: 10.1149/2.1151605jes

Beitrag zur �bermikroskopischen Abbildung bei h�heren Drucken
journal, August 1942


Transmission electron microscopy of specimens and processes in liquids
journal, October 2016

  • Ross, Frances M.; Wang, Chongmin; de Jonge, Niels
  • MRS Bulletin, Vol. 41, Issue 10
  • DOI: 10.1557/mrs.2016.212

Electron microscopy of frozen water and aqueous solutions
journal, December 1982


Electron microscopy of frozen hydrated sections of vitreous ice and vitrified biological samples
journal, July 1983


Low-Dose Aberration-Free Imaging of Li-Rich Cathode Materials at Various States of Charge Using Electron Ptychography
journal, September 2018


Lithium Electrodeposition Dynamics in Aprotic Electrolyte Observed in Situ via Transmission Electron Microscopy
journal, February 2015

  • Leenheer, Andrew J.; Jungjohann, Katherine L.; Zavadil, Kevin R.
  • ACS Nano, Vol. 9, Issue 4
  • DOI: 10.1021/acsnano.5b00876

Phase Boundary Propagation in Li-Alloying Battery Electrodes Revealed by Liquid-Cell Transmission Electron Microscopy
journal, May 2016

  • Leenheer, Andrew J.; Jungjohann, Katherine L.; Zavadil, Kevin R.
  • ACS Nano, Vol. 10, Issue 6
  • DOI: 10.1021/acsnano.6b02200

A site-specific focused-ion-beam lift-out method for cryo Transmission Electron Microscopy
journal, December 2012

  • Rubino, Stefano; Akhtar, Sultan; Melin, Petter
  • Journal of Structural Biology, Vol. 180, Issue 3
  • DOI: 10.1016/j.jsb.2012.08.012

A method for site-specific and cryogenic specimen fabrication of liquid/solid interfaces for atom probe tomography
journal, November 2018