Polarized X-ray Absorption Spectroscopy Observation of Electronic and Structural Changes of Chemical Vapor Deposition Graphene in Contact with Water

Velasco-Vélez, Juan-Jesús; Wu, Chenghao; Wang, Boyao; Sun, Yu; Zhang, Yuegang; Guo, Jinghua; Salmerón, Miquel

doi:10.1021/jp507405z

Cited by 27 publications

(22 citation statements)

References 18 publications

(30 reference statements)

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“…Until now, mostly Infrared (IR), Raman and sum frequency generation (SFG) spectroscopies [116][117][118] X-ray absorption spectroscopy (XAS) in particular is an element-specific technique that can provide information on the electronic and geometric structure of molecules, and for that reason it has been extensively used to investigate the electronic structure of water using the oxygen K-edge [122][123][124]. Most investigations are typically performed collecting the photons generated by the decay of the core holes created by absorption of the X-rays, a method called fluorescence yield XAS (FY-XAS) [125][126][127][128][129]. Because of the micrometer penetration range of soft X-rays in condensed matter, the FY-XAS mode is essentially a bulk-sensitive technique.…”

Section: -The Liquid Water-solid Interfacementioning

confidence: 99%

Water at surfaces and interfaces: From molecules to ice and bulk liquid

Shimizu

Maier

Verdaguer

et al. 2018

Progress in Surface Science

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The structure and growth of water films on surfaces is reviewed, starting from single molecules, two-dimensional wetting layers, and liquid interfaces. This progression follows the increase in temperature and vapor pressure environmental conditions from a few degrees Kelvin in ultra-high vacuum, where Scanning Tunneling and Atomic Force Microscopies (STM and AFM) provide crystallographic information at the molecular level, to ambient conditions where surface sensitive spectroscopic techniques provide electronic structure information. We show how single molecules bind to metal and non-metal surfaces, their diffusion and aggregation. We examine how water molecules can be manipulated by the STM tip via excitation of vibrational and electronic modes, which trigger molecular diffusion and dissociation. We review also the adsorption and structure of water on non-metal substrates including mica, alkali halides, and others under ambient humid conditions. We finally review recent progress in the exploration of the molecular level structure of solid-liquid interfaces, which impact our fundamental understanding of corrosion and electrochemical processes. variety of names: atomic force microscopy (AFM) and its variants of contact and non-contact), lateral friction, and attractive electrostatic force microscopies, known as scanning polarization force microscopy (SPFM) and Kelvin Probe Force Microscopy (KPFM). The non-contact attractive AFM modes allow us to observe water films formed on solids with minimal disruption. We will first discuss adsorption configurations, diffusion, aggregation, and dissociation of water on metal surfaces induced thermally, vibrationally and electronically using STM. These topics were reviewed also by Hodgson and Haq in 2009 [3] from the theoretical point of view. We then move to formation of larger clusters and monolayers. The discussion of the "ice" layers is followed by liquid water films minerals (salts, oxides) in ambient conditions. In the last section, we also review recent studies of liquid water near a solid, electrified surface. Here the knowledge obtained from X-ray absorption spectroscopy (XAS) has proved useful for better understanding of atomistic pictures of electrochemical processes. Single molecules: diffusion, aggregation, dissociation Water on metal surfaces at low coverage-monomers and small clusters STM studies of adsorption of water on metal surfaces started in the early 2000's, with noble metals, including Au, Ag, Cu, and more reactive transition metals, such as Pt, Pd, Rh, Ru have been used as substrates. The first observation of individual water molecules was reported in 2001 by Lauhon and Ho [4] on Cu(001) using low-temperature STM. They pointed out several phenomena occurring during imaging of adsorbed water: 1) stable clusters form at relatively low coverage, 2) imaging of small clusters (less than 6 molecules) often leads to the tip inducing molecular motions, and 3) large clusters have internal structures that are often difficult to resolve. Morgenstern et al. [5-9] st...

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Section: -The Liquid Water-solid Interfacementioning

confidence: 99%

Water at surfaces and interfaces: From molecules to ice and bulk liquid

Shimizu

Maier

Verdaguer

et al. 2018

Progress in Surface Science

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“…However, similar to photoelectron spectroscopies, extremely thin electrodes such as graphene membranes set a limitation here. The cell was also adapted for the investigation of the interaction between water and graphene depending on the incidence X‐ray angle under static conditions . Such flow‐cell designs are being further optimized at ALS .…”

Section: Progress In Analytical Techniques Observed In Electrochemicmentioning

confidence: 99%

Probing Operating Electrochemical Interfaces by Photons and Neutrons

et al. 2015

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The operation of all electrochemical energy-related systems, such as supercapacitors, batteries, fuel cells, etc. depends largely on the processes occurring at electrochemical interfaces at which charge separation and chemical reactions occur. Evolution of structure and composition at the interface between electrodes and electrolytes affects all the device′s functional parameters including power and long-term performance stability. The analytical techniques capable of exploring the interfaces are still very limited, and more often only ex situ studies are performed. This sometimes leads to a loss of important pieces of the puzzle, hindering the development of novel technologies, as in many cases intermediates and electrochemical reaction products cannot be “quenched” for post-process analyses. Techniques capable of operando probing of electrochemical interfaces by photons and neutrons have become an extensively growing field of research. This review aims at highlighting approaches and developing ideas on the adaptation of photoelectron, X-ray absorption, vibrational spectroscopy, nuclear magnetic resonance, and X-ray and neutron reflectometry in electrochemical studies

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“…At present, a few experimental setups for performing AP-XAS in the soft X-ray range at ambient pressure are available at synchrotron radiation laboratories. [7][8][9][10][11] Photoemission and XAS/XMCD are complementary methods that contribute to the characterization of surfaces and nanostructures in experiments carried out in UHV. It is surprising that the development of the ambient-pressure implementation of these techniques has not been synchronous, also considering that XAS in the soft X-ray has several advantages with respect to the NAPXPS: the detection mode can be changed (from total and partial electron yield to transmission or fluorescent photon yield) to obtain different degrees of surface sensitivity; the travel of secondary electrons or photons in the gas is considerably longer than the one of primary photoelectrons measured in XPS and this allows operating NEXAFS effectively at ambient pressure while NAPXPS is still confined to the mbar range.…”

Section: Introductionmentioning

confidence: 99%

A reaction cell for ambient pressure soft x-ray absorption spectroscopy

Castán-Guerrero

Krizmancic

Bonanni

et al. 2018

Review of Scientific Instruments

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We present a new experimental setup for performing X-ray Absorption Spectroscopy (XAS) in the soft X-ray range at ambient pressure. The ambient pressure XAS setup is fully compatible with the ultra high vacuum environment of a synchrotron radiation spectroscopy beamline end station by means of ultrathin SiN membranes acting as windows for the X-ray beam and seal of the atmospheric sample environment. The XAS detection is performed in total electron yield (TEY) mode by probing the drain current from the sample with a picoammeter. The high signal/noise ratio achievable in the TEY mode, combined with a continuous scanning of the X-ray energies, makes it possible recording XAS spectra in a few seconds. The first results show the performance of this setup to record fast XAS spectra from sample surfaces exposed at atmospheric pressure, even in the case of highly insulating samples. The use of a permanent magnet inside the reaction cell enables the measurement of X-ray magnetic circular dichroism at ambient pressure.

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Polarized X-ray Absorption Spectroscopy Observation of Electronic and Structural Changes of Chemical Vapor Deposition Graphene in Contact with Water

Cited by 27 publications

References 18 publications

Water at surfaces and interfaces: From molecules to ice and bulk liquid

Water at surfaces and interfaces: From molecules to ice and bulk liquid

Probing Operating Electrochemical Interfaces by Photons and Neutrons

A reaction cell for ambient pressure soft x-ray absorption spectroscopy

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