Photoelectron spectroscopy of wet and gaseous samples through graphene membranes

Kraus, Jürgen; Reichelt, Robert; Günther, Sebastian; Gregoratti, Luca; Amati, Matteo; Kiskinova, Maya; Yulaev, Alexander; Vlassiouk, Ivan V.; Kolmakov, Andrei

doi:10.1039/C4NR03561E

Title: Photoelectron spectroscopy of wet and gaseous samples through graphene membranes

Journal Article · Mon Sep 22 00:00:00 EDT 2014 · Nanoscale

DOI:https://doi.org/10.1039/C4NR03561E· OSTI ID:1214459

Kraus, Jürgen ^[1]; Reichelt, Robert ^[1]; Günther, Sebastian ^[1]; Gregoratti, Luca ^[2]; Amati, Matteo ^[2]; Kiskinova, Maya ^[2]; Yulaev, Alexander ^[3]; Vlassiouk, Ivan V. ^[4]; Kolmakov, Andrei ^[5]

Technische Univ. München (Germany)
Elettra - Sincrotrone Trieste (Italy)
Univ. of Maryland, College Park, MD (United States); National Inst. of Standards and Technology (NIST), Gaithersburg, MD (United States). Center for Nanoscale Sciencee and Technology
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
National Inst. of Standards and Technology (NIST), Gaithersburg, MD (United States). Center for Nanoscale Sciencee and Technology

Photoelectron spectroscopy (PES) and microscopy are highly important for exploring morphologically and chemically complex liquid–gas, solid–liquid and solid–gas interfaces under realistic conditions, but the very small electron mean free path inside dense media imposes serious experimental challenges. Currently, near ambient pressure PES is conducted using dexterously designed electron energy analyzers coupled with differentially pumped electron lenses which make it possible to conduct PES measurements at a few hPa. This report proposes an alternative ambient pressure approach that can be applied to a broad class of samples and be implemented in conventional PES instruments. It uses ultrathin electron transparent but molecular impermeable membranes to isolate the high pressure sample environment from the high vacuum PES detection system. We show that the separating graphene membrane windows are both mechanically robust and sufficiently transparent for electrons in a wide energy range to allow soft X-ray PES of liquid and gaseous water. The performed proof-of-principle experiments confirm the possibility to probe vacuum-incompatible toxic or reactive samples placed inside such hermetic, gas flow or fluidic environmental cells.

View Accepted Manuscript (DOE)

Cite

Export

Save

Research Organization:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Sciences (CNMS)

Sponsoring Organization:: USDOE

Grant/Contract Number:: AC05-00OR22725

OSTI ID:: 1214459

Journal Information:: Nanoscale, Vol. 6, Issue 23; ISSN 2040-3364

Publisher:: Royal Society of ChemistryCopyright Statement

Country of Publication:: United States

Language:: English

Citation Metrics:

Cited by: 61 works

Citation information provided by
Web of Science

References (58)

The evolution of model catalytic systems; studies of structure, bonding and dynamics from single crystal metal surfaces to nanoparticles, and from low pressure (<10 ⁻³ Torr) to high pressure (>10 ⁻³ Torr) to liquid interfaces Somorjai, Gabor A.; York, Roger L.; Butcher, Derek Phys. Chem. Chem. Phys., Vol. 9, Issue 27 https://doi.org/10.1039/B618805B	journal	January 2007
Measuring fundamental properties in operating solid oxide electrochemical cells by using in situ X-ray photoelectron spectroscopy Zhang, Chunjuan; Grass, Michael E.; McDaniel, Anthony H. Nature Materials, Vol. 9, Issue 11 https://doi.org/10.1038/nmat2851	journal	September 2010
Electron Spectroscopy of Aqueous Solution Interfaces Reveals Surface Enhancement of Halides Ghosal, S. Science, Vol. 307, Issue 5709 https://doi.org/10.1126/science.1106525	journal	January 2005
ESCA applied to liquids Siegbahn, Hans; Siegbahn, Kai Journal of Electron Spectroscopy and Related Phenomena, Vol. 2, Issue 3 https://doi.org/10.1016/0368-2048(73)80023-4	journal	January 1973
ESCA applied to liquids. II. Valence and core electron spectra of formamide Siegbarn, H.; Asplund, L.; Kelfve, P. Journal of Electron Spectroscopy and Related Phenomena, Vol. 5, Issue 1 https://doi.org/10.1016/0368-2048(74)85065-6	journal	January 1974
Photoemission from Liquid Aqueous Solutions Winter, Bernd; Faubel, Manfred Chemical Reviews, Vol. 106, Issue 4 https://doi.org/10.1021/cr040381p	journal	April 2006
In situ photoelectron spectroscopy at the liquid/nanoparticle interface Brown, Matthew A.; Jordan, Inga; Beloqui Redondo, Amaia Surface Science, Vol. 610 https://doi.org/10.1016/j.susc.2013.01.012	journal	April 2013
A combined droplet train and ambient pressure photoemission spectrometer for the investigation of liquid/vapor interfaces Starr, David E.; Wong, Ed K.; Worsnop, Douglas R. Physical Chemistry Chemical Physics, Vol. 10, Issue 21 https://doi.org/10.1039/b800717a	journal	January 2008
Electron spectroscopy for chemical analysis of liquids and solutions Siegbahn, Hans The Journal of Physical Chemistry, Vol. 89, Issue 6 https://doi.org/10.1021/j100252a005	journal	March 1985
A “high-pressure” electron spectrometer for surface studies Joyner, Richard W.; Roberts, M. Wyn; Yates, Kenneth Surface Science, Vol. 87, Issue 2 https://doi.org/10.1016/0039-6028(79)90544-2	journal	August 1979
In situ X-ray photoelectron spectroscopy of surfaces at pressures up to 1 mbar Ruppender, H. J.; Grunze, M.; Kong, C. W. Surface and Interface Analysis, Vol. 15, Issue 4 https://doi.org/10.1002/sia.740150403	journal	April 1990
A differentially pumped electrostatic lens system for photoemission studies in the millibar range Ogletree, D. Frank; Bluhm, Hendrik; Lebedev, Gennadi Review of Scientific Instruments, Vol. 73, Issue 11 https://doi.org/10.1063/1.1512336	journal	November 2002
Ambient pressure photoelectron spectroscopy: A new tool for surface science and nanotechnology Salmeron, M.; Schlogl, R. Surface Science Reports, Vol. 63, Issue 4 https://doi.org/10.1016/j.surfrep.2008.01.001	journal	April 2008
Investigation of solid/vapor interfaces using ambient pressure X-ray photoelectron spectroscopy Starr, D. E.; Liu, Z.; Hävecker, M. Chemical Society Reviews, Vol. 42, Issue 13 https://doi.org/10.1039/c3cs60057b	journal	January 2013
Operando Studies of Catalyst Surfaces during Catalysis and under Reaction Conditions: Ambient Pressure X-Ray Photoelectron Spectroscopy with a Flow-Cell Reactor Tao, Franklin Feng ChemCatChem, Vol. 4, Issue 5 https://doi.org/10.1002/cctc.201200002	journal	April 2012
Near ambient pressure XPS with a conventional X-ray source: NAP XPS with a conventional X-ray source Jürgensen, A.; Esser, N.; Hergenröder, R. Surface and Interface Analysis, Vol. 44, Issue 8 https://doi.org/10.1002/sia.4826	journal	January 2012
Design and Performance Aspects of a Custom-Built Ambient Pressure Photoelectron Spectrometer toward Bridging the Pressure Gap: Oxidation of Cu, Ag, and Au Surfaces at 1 mbar O ₂ Pressure Roy, Kanak; Vinod, C. P.; Gopinath, Chinnakonda S. The Journal of Physical Chemistry C, Vol. 117, Issue 9 https://doi.org/10.1021/jp312706s	journal	February 2013
The new ambient-pressure X-ray photoelectron spectroscopy instrument at MAX-lab Schnadt, Joachim; Knudsen, Jan; Andersen, Jesper N. Journal of Synchrotron Radiation, Vol. 19, Issue 5 https://doi.org/10.1107/S0909049512032700	journal	August 2012
Photoelectron spectroscopy under ambient pressure and temperature conditions Frank Ogletree, D.; Bluhm, Hendrik; Hebenstreit, Eleonore D. Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment, Vol. 601, Issue 1-2 https://doi.org/10.1016/j.nima.2008.12.155	journal	March 2009
Practical expressions for the mean escape depth, the information depth, and the effective attenuation length in Auger-electron spectroscopy and x-ray photoelectron spectroscopy Jablonski, A.; Powell, C. J. Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, Vol. 27, Issue 2 https://doi.org/10.1116/1.3071947	journal	March 2009
Photoelectron emission microscopy of ultrathin oxide covered devices Ballarotto, V. W.; Breban, M.; Siegrist, K. Journal of Vacuum Science & Technology B: Microelectronics and Nanometer Structures, Vol. 20, Issue 6 https://doi.org/10.1116/1.1525007	journal	January 2002
Hard X-ray Photoelectron Emission Microscopy as Tool for Studying Buried Layers Wakita, Takanori; Taniuchi, Toshiyuki; Ono, Kanta Japanese Journal of Applied Physics, Vol. 45, Issue 3A https://doi.org/10.1143/JJAP.45.1886	journal	March 2006
Hard X-ray photoemission spectroscopy Kobayashi, Keisuke Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment, Vol. 601, Issue 1-2 https://doi.org/10.1016/j.nima.2008.12.188	journal	March 2009
In situ x-ray photoelectron spectroscopy for electrochemical reactions in ordinary solvents Masuda, Takuya; Yoshikawa, Hideki; Noguchi, Hidenori Applied Physics Letters, Vol. 103, Issue 11 https://doi.org/10.1063/1.4821180	journal	September 2013
A Closed Cell for Electron Microscopy Abrams, I. M.; McBain, J. W. Journal of Applied Physics, Vol. 15, Issue 8 https://doi.org/10.1063/1.1707475	journal	August 1944
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
Two-dimensional atomic crystals Novoselov, K. S.; Jiang, D.; Schedin, F. Proceedings of the National Academy of Sciences, Vol. 102, Issue 30, p. 10451-10453 https://doi.org/10.1073/pnas.0502848102	journal	July 2005
Chemical methods for the production of graphenes Park, Sungjin; Ruoff, Rodney S. Nature Nanotechnology, Vol. 4, Issue 4, p. 217-224 https://doi.org/10.1038/nnano.2009.58	journal	March 2009
Low-energy electron point projection microscopy of suspended graphene, the ultimate ‘microscope slide’ Mutus, J. Y.; Livadaru, L.; Robinson, J. T. New Journal of Physics, Vol. 13, Issue 6 https://doi.org/10.1088/1367-2630/13/6/063011	journal	June 2011
Graphene oxide windows for in situ environmental cell photoelectron spectroscopy Kolmakov, Andrei; Dikin, Dmitriy A.; Cote, Laura J. Nature Nanotechnology, Vol. 6, Issue 10 https://doi.org/10.1038/nnano.2011.130	journal	August 2011
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
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
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
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
Electron effective attenuation lengths for applications in Auger electron spectroscopy and x-ray photoelectron spectroscopy Powell, C. J.; Jablonski, A. Surface and Interface Analysis, Vol. 33, Issue 3 https://doi.org/10.1002/sia.1204	journal	January 2002
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
Synchrotron-based photoelectron microscopy Barinov, Alexei; Dudin, Pavel; Gregoratti, Luca Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment, Vol. 601, Issue 1-2 https://doi.org/10.1016/j.nima.2008.12.157	journal	March 2009
Atomic-Scale Characterization of Graphene Grown on Copper (100) Single Crystals Rasool, Haider I.; Song, Emil B.; Mecklenburg, Matthew Journal of the American Chemical Society, Vol. 133, Issue 32 https://doi.org/10.1021/ja200245p	journal	August 2011
Atomic-Scale Investigation of Graphene Grown on Cu Foil and the Effects of Thermal Annealing Cho, Jongweon; Gao, Li; Tian, Jifa ACS Nano, Vol. 5, Issue 5 https://doi.org/10.1021/nn103338g	journal	April 2011
Epitaxial Graphene on Cu(111) Gao, Li; Guest, Jeffrey R.; Guisinger, Nathan P. Nano Letters, Vol. 10, Issue 9 https://doi.org/10.1021/nl1016706	journal	September 2010
Towards the perfect graphene membrane? – Improvement and limits during formation of high quality graphene grown on Cu-foils Kraus, Jürgen; Böcklein, Sebastian; Reichelt, Robert Carbon, Vol. 64 https://doi.org/10.1016/j.carbon.2013.07.090	journal	November 2013
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
Auger Electron Spectroscopy: A Rational Method for Determining Thickness of Graphene Films Xu, Mingsheng; Fujita, Daisuke; Gao, Jianhua ACS Nano, Vol. 4, Issue 5 https://doi.org/10.1021/nn100276w	journal	March 2010
Morphology and electronic structure of gold clusters on graphite: Scanning-tunneling techniques and photoemission Hövel, Heinz; Barke, Ingo Progress in Surface Science, Vol. 81, Issue 2-3 https://doi.org/10.1016/j.progsurf.2006.01.002	journal	January 2006
XPS study on the evaporation of gold submonolayers on carbon surfaces Büttner, Michael; Oelhafen, Peter Surface Science, Vol. 600, Issue 5 https://doi.org/10.1016/j.susc.2006.01.020	journal	March 2006
The Nature of Water Nucleation Sites on TiO ₂ (110) Surfaces Revealed by Ambient Pressure X-ray Photoelectron Spectroscopy Ketteler, Guido; Yamamoto, Susumu; Bluhm, Hendrik The Journal of Physical Chemistry C, Vol. 111, Issue 23 https://doi.org/10.1021/jp068606i	journal	June 2007
Chemistry in solution: recent techniques and applications using soft X-ray spectroscopy Lange, Kathrin M.; Kothe, Alexander; Aziz, Emad F. Physical Chemistry Chemical Physics, Vol. 14, Issue 16 https://doi.org/10.1039/c2cp24028a	journal	January 2012
Observation of Graphene Bubbles and Effective Mass Transport under Graphene Films Stolyarova, E.; Stolyarov, D.; Bolotin, K. Nano Letters, Vol. 9, Issue 1 https://doi.org/10.1021/nl803087x	journal	January 2009
Graphene Visualizes the First Water Adlayers on Mica at Ambient Conditions Xu, K.; Cao, P.; Heath, J. R. Science, Vol. 329, Issue 5996 https://doi.org/10.1126/science.1192907	journal	September 2010
Bubble and Pattern Formation in Liquid Induced by an Electron Beam Grogan, Joseph M.; Schneider, Nicholas M.; Ross, Frances M. Nano Letters, Vol. 14, Issue 1 https://doi.org/10.1021/nl404169a	journal	December 2013
Radiation damage of water in environmental scanning electron microscopy Royall, C. P.; Thiel, B. L.; Donald, A. M. Journal of Microscopy, Vol. 204, Issue 3 https://doi.org/10.1046/j.1365-2818.2001.00948.x	journal	December 2001
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
Cryo-electron energy loss spectroscopy: observations on vitrified hydrated specimens and radiation damage Leapman, Richard D.; Sun, Songquan Ultramicroscopy, Vol. 59, Issue 1-4 https://doi.org/10.1016/0304-3991(95)00019-W	journal	July 1995
Ultrathin Oxide Films by Atomic Layer Deposition on Graphene Wang, Luda; Travis, Jonathan J.; Cavanagh, Andrew S. Nano Letters, Vol. 12, Issue 7 https://doi.org/10.1021/nl3014956	journal	June 2012
Two-Dimensional Crystals: Beyond Graphene Neto, A. H. Castro; Novoselov, K. Materials Express, Vol. 1, Issue 1 https://doi.org/10.1166/mex.2011.1002	journal	March 2011
Probing Liquid/Solid Interfaces at the Molecular Level Zaera, Francisco Chemical Reviews, Vol. 112, Issue 5 https://doi.org/10.1021/cr2002068	journal	January 2012
Transfer of Large-Area Graphene Films for High-Performance Transparent Conductive Electrodes Li, Xuesong; Zhu, Yanwu; Cai, Weiwei Nano Letters, Vol. 9, Issue 12 https://doi.org/10.1021/nl902623y	journal	December 2009
Scanning Photoelectron Microscopy: a Powerful Technique for Probing Micro and Nano-Structures Abyaneh, Majid Kazemian; Gregoratti, Luca; Amati, Matteo e-Journal of Surface Science and Nanotechnology, Vol. 9 https://doi.org/10.1380/ejssnt.2011.158	journal	January 2011

Similar Records

Graphene-enabled electron microscopy and correlated super-resolution microscopy of wet cells

Journal Article · Thu Jun 11 00:00:00 EDT 2015 · Nature Communications · OSTI ID:1214459

Wojcik, Michal; Hauser, Margaret; Li, Wan; +2 more

Closing the pressure gap in x-ray photoelectron spectroscopy by membrane hydrogenation

Journal Article · Fri May 15 00:00:00 EDT 2015 · Review of Scientific Instruments · OSTI ID:1214459

Delmelle, Renaud; Borgschulte, Andreas; Probst, Benjamin; +3 more

Fabrication of Core–Shell Nanotube Array for Artificial Photosynthesis Featuring an Ultrathin Composite Separation Membrane

Journal Article · Tue Jan 02 00:00:00 EST 2018 · ACS Nano · OSTI ID:1214459

Edri, Eran; Aloni, Shaul; Frei, Heinz

Related Subjects

71 CLASSICAL AND QUANTUM MECHANICS
GENERAL PHYSICS

Title: Photoelectron spectroscopy of wet and gaseous samples through graphene membranes

Citation Formats

References (58)

Similar Records

Related Subjects