Graphene Microcapsule Arrays for Combinatorial Electron Microscopy and Spectroscopy in Liquids

Yulaev, Alexander; Guo, Hongxuan; Strelcov, Evgheni; Chen, Lei; Vlassiouk, Ivan; Kolmakov, Andrei

doi:10.1021/acsami.7b02824

Title: Graphene Microcapsule Arrays for Combinatorial Electron Microscopy and Spectroscopy in Liquids

Journal Article · Thu Apr 27 00:00:00 EDT 2017 · ACS Applied Materials and Interfaces

DOI:https://doi.org/10.1021/acsami.7b02824· OSTI ID:1399453

Yulaev, Alexander ^[1]; Guo, Hongxuan ^[2]; Strelcov, Evgheni ^[3]; Chen, Lei ^[4];

^[5];

^[4]

National Inst. of Standards and Technology (NIST), Gaithersburg, MD (United States). Center for Nanoscale Science and Technology; Univ. of Maryland, College Park, MD (United States). Dept. of Materials Science and Engineering; Univ. of Maryland, College Park, MD (United States). Maryland NanoCenter
National Inst. of Standards and Technology (NIST), Gaithersburg, MD (United States). Center for Nanoscale Science and Technology; Univ. of Maryland, College Park, MD (United States). Maryland NanoCenter
National Inst. of Standards and Technology (NIST), Gaithersburg, MD (United States). Center for Nanoscale Science and Technology; Univ. of Maryland, College Park, MD (United States). Maryland NanoCenter
National Inst. of Standards and Technology (NIST), Gaithersburg, MD (United States). Center for Nanoscale Science and Technology
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

Atomic-scale thickness, molecular impermeability, low atomic number, and mechanical strength make graphene an ideal electron-transparent membrane for material characterization in liquids and gases with scanning electron microscopy and spectroscopy. Here in this paper, we present a novel sample platform made of an array of thousands of identical isolated graphene-capped microchannels with high aspect ratio. A combination of a global wide field of view with high resolution local imaging of the array allows for high throughput in situ studies as well as for combinatorial screening of solutions, liquid interfaces, and immersed samples. We demonstrate the capabilities of this platform by studying a pure water sample in comparison with alkali halide solutions, a model electrochemical plating process, and beam-induced crystal growth in liquid electrolyte. Spectroscopic characterization of liquid interfaces and immersed objects with Auger and X-ray fluorescence analysis through the graphene membrane are also demonstrated.

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

Sponsoring Organization:: USDOE

Grant/Contract Number:: AC05-00OR22725

OSTI ID:: 1399453

Journal Information:: ACS Applied Materials and Interfaces, Vol. 9, Issue 31; ISSN 1944-8244

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 22 works

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References (43)

Electron microscopy of specimens in liquid de Jonge, Niels; Ross, Frances M. Nature Nanotechnology, Vol. 6, Issue 11, p. 695-704 https://doi.org/10.1038/nnano.2011.161	journal	October 2011
The Nanoaquarium: A Platform for In Situ Transmission Electron Microscopy in Liquid Media Grogan, Joseph M.; Bau, Haim H. Journal of Microelectromechanical Systems, Vol. 19, Issue 4 https://doi.org/10.1109/JMEMS.2010.2051321	journal	August 2010
Monolithic Chip System with a Microfluidic Channel for In Situ Electron Microscopy of Liquids Jensen, Eric; Burrows, Andrew; Mølhave, Kristian Microscopy and Microanalysis, Vol. 20, Issue 2 https://doi.org/10.1017/S1431927614000300	journal	April 2014
High-Resolution Imaging and Spectroscopy at High Pressure: A Novel Liquid Cell for the Transmission Electron Microscope Tanase, Mihaela; Winterstein, Jonathan; Sharma, Renu Microscopy and Microanalysis, Vol. 21, Issue 6 https://doi.org/10.1017/S1431927615015482	journal	December 2015
An apparatus for imaging liquids, cells, and other wet samples in the scanning electron microscopy Thiberge, S.; Zik, O.; Moses, E. Review of Scientific Instruments, Vol. 75, Issue 7 https://doi.org/10.1063/1.1763262	journal	July 2004
The Atmospheric Scanning Electron Microscope with open sample space observes dynamic phenomena in liquid or gas Suga, Mitsuo; Nishiyama, Hidetoshi; Konyuba, Yuji Ultramicroscopy, Vol. 111, Issue 12 https://doi.org/10.1016/j.ultramic.2011.08.001	journal	December 2011
In-situ SEM microchip setup for electrochemical experiments with water based solutions Jensen, E.; Købler, C.; Jensen, P. S. Ultramicroscopy, Vol. 129 https://doi.org/10.1016/j.ultramic.2013.03.002	journal	June 2013
Design and Application of Variable Temperature Setup for Scanning Electron Microscopy in Gases and Liquids at Ambient Conditions Al-Asadi, Ahmed S.; Zhang, Jie; Li, Jianbo Microscopy and Microanalysis, Vol. 21, Issue 3 https://doi.org/10.1017/S1431927615000732	journal	June 2015
Electron Microscopy of Living Cells During in Situ Fluorescence Microscopy Liv, Nalan; van Oosten Slingeland, Daan S. B.; Baudoin, Jean-Pierre ACS Nano, Vol. 10, Issue 1 https://doi.org/10.1021/acsnano.5b03970	journal	December 2015
Calculations of electron inelastic mean free paths. IX. Data for 41 elemental solids over the 50 eV to 30 keV range Tanuma, S.; Powell, C. J.; Penn, D. R. Surface and Interface Analysis, Vol. 43, Issue 3 https://doi.org/10.1002/sia.3522	journal	February 2011
Photoelectron spectroscopy of wet and gaseous samples through graphene membranes Kraus, Jürgen; Reichelt, Robert; Günther, Sebastian Nanoscale, Vol. 6, Issue 23 https://doi.org/10.1039/C4NR03561E	journal	January 2014
Electron transparent graphene windows for environmental scanning electron microscopy in liquids and dense gases Stoll, Joshua D.; Kolmakov, Andrei Nanotechnology, Vol. 23, Issue 50 https://doi.org/10.1088/0957-4484/23/50/505704	journal	November 2012
High-Resolution EM of Colloidal Nanocrystal Growth Using Graphene Liquid Cells Yuk, Jong Min; Park, Jungwon; Ercius, Peter Science, Vol. 336, Issue 6077 https://doi.org/10.1126/science.1217654	journal	April 2012
High-Resolution Electron Microscopy and Spectroscopy of Ferritin in Biocompatible Graphene Liquid Cells and Graphene Sandwiches Wang, Canhui; Qiao, Qiao; Shokuhfar, Tolou Advanced Materials, Vol. 26, Issue 21 https://doi.org/10.1002/adma.201306069	journal	February 2014
Electron Microscopy in Air: Transparent Atomic Membranes and Imaging Modes Han, Yimo; Nguyen, Kayla; Ogawa, Yui Microscopy and Microanalysis, Vol. 21, Issue S3 https://doi.org/10.1017/S1431927615006340	journal	August 2015
Impermeable Atomic Membranes from Graphene Sheets Bunch, J. Scott; Verbridge, Scott S.; Alden, Jonathan S. Nano Letters, Vol. 8, Issue 8 https://doi.org/10.1021/nl801457b	journal	August 2008
Graphene Membranes for Atmospheric Pressure Photoelectron Spectroscopy Weatherup, Robert S.; Eren, Baran; Hao, Yibo The Journal of Physical Chemistry Letters, Vol. 7, Issue 9 https://doi.org/10.1021/acs.jpclett.6b00640	journal	April 2016
Photoelectron Spectroscopy at the Graphene-Liquid Interface Reveals the Electronic Structure of an Electrodeposited Cobalt/Graphene Electrocatalyst Velasco-Velez, Juan J.; Pfeifer, Verena; Hävecker, Michael Angewandte Chemie International Edition, Vol. 54, Issue 48 https://doi.org/10.1002/anie.201506044	journal	October 2015
Transfer of CVD-Grown Monolayer Graphene onto Arbitrary Substrates Suk, Ji Won; Kitt, Alexander; Magnuson, Carl W. ACS Nano, Vol. 5, Issue 9 https://doi.org/10.1021/nn201207c	journal	August 2011
Three-dimensional electron microscopy simulation with the CASINO Monte Carlo software Demers, Hendrix; Poirier-Demers, Nicolas; Couture, Alexandre Réal Scanning, Vol. 33, Issue 3 https://doi.org/10.1002/sca.20262	journal	May 2011
Scanning Electron Microscopy and X-ray Microanalysis Goldstein, Joseph I.; Newbury, Dale E.; Echlin, Patrick https://doi.org/10.1007/978-1-4615-0215-9	book	January 2003
Nanofiltration across Defect-Sealed Nanoporous Monolayer Graphene O’Hern, Sean C.; Jang, Doojoon; Bose, Suman Nano Letters, Vol. 15, Issue 5 https://doi.org/10.1021/acs.nanolett.5b00456	journal	April 2015
Implications of Permeation through Intrinsic Defects in Graphene on the Design of Defect-Tolerant Membranes for Gas Separation Boutilier, Michael S. H.; Sun, Chengzhen; O’Hern, Sean C. ACS Nano, Vol. 8, Issue 1, p. 841-849 https://doi.org/10.1021/nn405537u	journal	December 2013
Selective Molecular Transport through Intrinsic Defects in a Single Layer of CVD Graphene O’Hern, Sean C.; Stewart, Cameron A.; Boutilier, Michael S. H. ACS Nano, Vol. 6, Issue 11, p. 10130-10138 https://doi.org/10.1021/nn303869m	journal	October 2012
Hydrogen bonding in liquid water probed by resonant Auger-electron spectroscopy Winter, Bernd; Hergenhahn, Uwe; Faubel, Manfred The Journal of Chemical Physics, Vol. 127, Issue 9 https://doi.org/10.1063/1.2770457	journal	September 2007
Soft X-ray microscopes and their biological applications Kirz, Janos; Jacobsen, Chris; Howells, Malcolm Quarterly Reviews of Biophysics, Vol. 28, Issue 1 https://doi.org/10.1017/S0033583500003139	journal	February 1995
Relaxation Processes in Aqueous Systems upon X-ray Ionization: Entanglement of Electronic and Nuclear Dynamics Slavíček, Petr; Kryzhevoi, Nikolai V.; Aziz, Emad F. The Journal of Physical Chemistry Letters, Vol. 7, Issue 2 https://doi.org/10.1021/acs.jpclett.5b02665	journal	January 2016
Ultrafast energy transfer between water molecules Jahnke, T.; Sann, H.; Havermeier, T. Nature Physics, Vol. 6, Issue 2 https://doi.org/10.1038/nphys1498	journal	January 2010
Enabling Photoemission Electron Microscopy in Liquids via Graphene-Capped Microchannel Arrays Guo, Hongxuan; Strelcov, Evgheni; Yulaev, Alexander Nano Letters, Vol. 17, Issue 2 https://doi.org/10.1021/acs.nanolett.6b04460	journal	January 2017
Sensitivity Enhancement for Quantitative Electrochemical Determination of a Trace Amount of Accelerator in Copper Plating Solutions Chiu, Yong-Da; Dow, Wei-Ping; Huang, Su-Mei Journal of The Electrochemical Society, Vol. 158, Issue 5 https://doi.org/10.1149/1.3560479	journal	January 2011
Accelerator Screening by Cyclic Voltammetry for Microvia Filling by Copper Electroplating Chiu, Yong-Da; Dow, Wei-Ping Journal of The Electrochemical Society, Vol. 160, Issue 12 https://doi.org/10.1149/2.006312jes	journal	January 2013
Scanning Electron Microscopy for in Situ Monitoring of Semiconductor−Liquid Interfacial Processes: Electron Assisted Reduction of Ag Ions from Aqueous Solution on the Surface of TiO ₂ Rutile Nanowire Kolmakova, Natalia; Kolmakov, Andrei The Journal of Physical Chemistry C, Vol. 114, Issue 40 https://doi.org/10.1021/jp1044546	journal	July 2010
Electron-Beam-Induced Deposition of Platinum from a Liquid Precursor Donev, Eugenii U.; Hastings, J. Todd Nano Letters, Vol. 9, Issue 7 https://doi.org/10.1021/nl9012216	journal	July 2009
Control of Electron Beam-Induced Au Nanocrystal Growth Kinetics through Solution Chemistry Park, Jeung Hun; Schneider, Nicholas M.; Grogan, Joseph M. Nano Letters, Vol. 15, Issue 8 https://doi.org/10.1021/acs.nanolett.5b01677	journal	July 2015
Direct-write liquid phase transformations with a scanning transmission electron microscope Unocic, Raymond R.; Lupini, Andrew R.; Borisevich, Albina Y. Nanoscale, Vol. 8, Issue 34 https://doi.org/10.1039/C6NR04994J	journal	January 2016
Challenges associated with in-situ TEM in environmental systems: The case of silver in aqueous solutions Noh, Kyong Wook; Liu, Yin; Sun, Li Ultramicroscopy, Vol. 116 https://doi.org/10.1016/j.ultramic.2012.03.012	journal	May 2012
Real-Time Observation of Water-Soluble Mineral Precipitation in Aqueous Solution by In Situ High-Resolution Electron Microscopy Yuk, Jong Min; Zhou, Qin; Chang, Jiyoung ACS Nano, Vol. 10, Issue 1 https://doi.org/10.1021/acsnano.5b04064	journal	December 2015
Estimation of Setchenow constants for nonpolar gases in aqueous solutions of common salts at moderate temperatures Pawlikowski, Ellen M.; Prausnitz, John M. Industrial & Engineering Chemistry Fundamentals, Vol. 22, Issue 1 https://doi.org/10.1021/i100009a015	journal	February 1983
Electron–Water Interactions and Implications for Liquid Cell Electron Microscopy Schneider, Nicholas M.; Norton, Michael M.; Mendel, Brian J. The Journal of Physical Chemistry C, Vol. 118, Issue 38 https://doi.org/10.1021/jp507400n	journal	September 2014
Quantitative Description of Crystal Nucleation and Growth from in Situ Liquid Scanning Transmission Electron Microscopy Ievlev, Anton V.; Jesse, Stephen; Cochell, Thomas J. ACS Nano, Vol. 9, Issue 12 https://doi.org/10.1021/acsnano.5b03720	journal	October 2015
Graphene nanobubbles on TiO ₂ for in-operando electron spectroscopy of liquid-phase chemistry Nappini, S.; Matruglio, A.; Naumenko, D. Nanoscale, Vol. 9, Issue 13 https://doi.org/10.1039/C6NR09061C	journal	January 2017
Role of Hydrogen in Chemical Vapor Deposition Growth of Large Single-Crystal Graphene Vlassiouk, Ivan; Regmi, Murari; Fulvio, Pasquale ACS Nano, Vol. 5, Issue 7, p. 6069-6076 https://doi.org/10.1021/nn201978y	journal	July 2011
Large-Area Synthesis of High-Quality and Uniform Graphene Films on Copper Foils Li, X.; Cai, W.; An, J. Science, Vol. 324, Issue 5932, p. 1312-1314 https://doi.org/10.1126/science.1171245	journal	May 2009

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State-of-the-Art and Future Prospects for Atomically Thin Membranes from 2D Materials Prozorovska, Liudmyla; Kidambi, Piran R. Advanced Materials, Vol. 30, Issue 52 https://doi.org/10.1002/adma.201801179	journal	August 2018

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Title: Graphene Microcapsule Arrays for Combinatorial Electron Microscopy and Spectroscopy in Liquids

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