Probing Voltage Drop Variations in Graphene with Photoelectron Spectrosopy

Cataloged from PDF version of article.We use X-ray photoelectron spectroscopy (XPS) for characterization of voltage drop variations of large area single-layer graphene on quartz substrates, by application of a voltage bias across two gold electrodes deposited on top. By monitoring the spatial variation of the kinetic energies of emitted Cls photoelectrons, we extract voltage variations in the graphene layer in a chemically specific format. The potential drop is uniform across the entire layer in the pristine sample but is not uniform in the oxidized one, due to cracks and/or morphological defects created during the oxidation process. This new way of data gathering reintroduces XPS as a major analytical tool for extracting electrical as well as chemical information about surface and/or nanostructured materials

A photoelectron spectroscopic investigation of conducting polypyrolle-polyamide composite film

Cataloged from PDF version of article.X-ray photoelectron spectrum of the electrochemically prepared polypyrrole and polypyrrole-polyamide composite films exhibit an additional strong high binding energy peak at 402.0 eV corresponding to N+ moieties. Intensity of this peak is significantly reduced upon electrochemical reduction. Atomic concentrations derived from the observed N+ and F (stemming from the dopant BF4-) peaks reveal a slightly higher cation/anion ratio for this composite and suggest that the composite has a different chemical composition than the corresponding polymers. © 1995 Elsevier Science B.V.X-ray photoelectron spectrum of the electrochemically prepared polypyrrole and polypyrrole-polyamide composite films exhibit an additional strong high binding energy peak at 402.0 eV corresponding to N+ moieties. Intensity of this peak is significantly reduced upon electrochemical reduction. Atomic concentrations derived from the observed N+ and F (stemming from the dopant BF4-) peaks reveal a slightly higher cation/anion ratio for this composite and suggest that the composite has a different chemical composition than the corresponding polymers

Predicting Scattering Scanning Near-field Optical Microscopy of Mass-produced Plasmonic Devices

Scattering scanning near-field optical microscopy enables optical imaging and characterization of plasmonic devices with nanometer-scale resolution well below the diffraction limit. This technique enables developers to probe and understand the waveguide-coupled plasmonic antenna in as-fabricated heat-assisted magnetic recording heads. In order validate and predict results and to extract information from experimental measurements that is physically comparable to simulations, a model was developed to translate the simulated electric field into expected near-field measurements using physical parameters specific to scattering scanning near-field optical microscopy physics. The methods used in this paper prove that scattering scanning near-field optical microscopy can be used to determine critical sub-diffraction-limited dimensions of optical field confinement, which is a crucial metrology requirement for the future of nano-optics, semiconductor photonic devices, and biological sensing where the near-field character of light is fundamental to device operation.Comment: article: 18 pages, 5 figures; SI: 15 pages, 12 figure

In-Situ XPS Monitoring and Characterization of Electrochemically Prepared Au Nanoparticles in an Ionic Liquid

Gold nanoparticles (Au NPs) have been electrochemically prepared in situ and in vacuo using two different electrochemical device configurations, containing an ionic liquid (IL), N-N-diethyl-N-methyl-N-(2-methoxyethyl)ammonium bis(trifluoromethanesulfonyl)imide, that serves both as reaction and as stabilizing media for the NPs. It was observed in both devices that Au NPs were created using an anodically triggered route. The created Au NPs are relatively small (3-7 nm) and reside within the IL medium. X-ray photoelectron spectroscopy is utilized to follow not only the formation of the NPs but also their charging/discharging properties, by monitoring the charging shifts of the Au4f peak representing the electrodes and also the Au NPs as well as the F1s peak of the IL after polarizing one of the electrodes. Accordingly, DC polarization across the electrodes leads to a uniform binding energy shift of F1s of the IL along with that of Au4f of the NPs within. Moreover, this shift corresponds to only half of the applied potential. AC polarization brings out another dimension for demonstrating further the harmony between the charging/discharging property of the IL medium and the Au NPs in temporally and laterally resolved fashions. Polarization of the electrodes result in perfect spectral separation of the Au4f peaks of the NPs from those of the metal in both static (DC) and in time- and position-dependent (AC) modes. © 2017 American Chemical Society

Combined XPS and contact angle studies of ethylene vinyl acetate and polyvinyl acetate blends

Cataloged from PDF version of article.In this study, we prepared thin films by blending ethylene vinyl acetate copolymers (EVA) containing 12-33 (wt.%) vinyl acetate (VA) with polyvinyl acetate (PVAc) and high density polyethylene homopolymers. Large area micropatterns having controlled protrusion sizes were obtained by phase-separation especially for the PVAc/EVA-33 blends using dip coating. These surfaces were characterized by XPS and contact angle measurements. A reasonably linear relation was found between the VA content on the surface (wt.%) obtained from XPS analysis and the VA content in bulk especially for PVAc/EVA-33 blend surfaces. PE segments were more enriched on the surface than that of the bulk for pure EVA copolymer surfaces similar to previous reports and VA enrichment was found on the EVA/HDPE blend surfaces due to high molecular weight of HDPE. Water theta(e) decreased with the increase in the VA content on the blend surface due to the polarity of VA. A good agreement was obtained between gamma(-)(s) and atomic oxygen surface concentration with the increase of VA content. The applicability of Cassie-Baxter equation was tested and found that it gave consistent results with the experimental water contact angles for the case where VA content was lower than 55 wt.% in the bulk composition. (C) 2011 Elsevier B. V. All rights reserved

X-ray photoelectron spectroscopy for identification of morphological defects and disorders in graphene devices

The progress in the development of graphene devices is promising, and they are now considered as an option for the current Si-based electronics. However, the structural defects in graphene may strongly influence the local electronic and mechanical characteristics. Although there are well-established analytical characterization methods to analyze the chemical and physical parameters of this material, they remain incapable of fully understanding of the morphological disorders. In this study, x-ray photoelectron spectroscopy (XPS) with an external voltage bias across the sample is used for the characterization of morphological defects in large area of a few layers graphene in a chemically specific fashion. For the XPS measurements, an external +6 V bias applied between the two electrodes and areal analysis for three different elements, C1s, O1s, and Au4f, were performed. By monitoring the variations of the binding energy, the authors extract the voltage variations in the graphene layer which reveal information about the structural defects, cracks, impurities, and oxidation levels in graphene layer which are created purposely or not. Raman spectroscopy was also utilized to confirm some of the findings. This methodology the authors offer is simple but provides promising chemically specific electrical and morphological information. � 2016 American Vacuum Society

Monitoring the operation of a graphene transistor in an integrated circuit by XPS

One of the transistors in an integrated circuit fabricated with graphene as the current controlling element, is investigated during its operation, using a chemical tool, XPS. Shifts in the binding energy of C1s are used to map out electrical potential variations, and compute sheet resistance of the graphene layer, as well as the contact resistances between the metal electrodes. Measured shifts depend on lateral positions probed, as well as on polarity and magnitude of the gate-voltage. This non-contact and chemically specific characterization can be pivotal in diagnoses. © 2016 Elsevier B.V

XPS enables visualization of electrode potential screening in an ionic liquid medium with temporal- and lateral-resolution

We present an X-ray photoelectron spectroscopic (XPS) investigation of potential screening across two gold electrodes fabricated on a porous polymer surface which is impregnated with the ionic liquid (IL) N-N-diethyl-N-methyl-N-(2-methoxyethyl)ammonium bis(trifluoromethanesulfonyl)imide [DEME-TFSI]. The IL provides a sheet of conducting layers to the insulating polymer film, and allows monitoring charging and screening dynamics at the polymer + IL/vacuum interface in a laterally resolved fashion across the electrodes. Time-resolved measurements are also implemented by recording F1s peaks of the IL, while imposing 10 mHz square-wave (SQW) pulses across the two electrodes in a source-drain geometry. Variations in the F1s binding energy reflect directly the transient local electrical potential, and allow us to visualize screening of the otherwise built-in local voltage drop on and across the metal electrodes in the range of millimeters. Accordingly, the device is partitioned into two oppositely polarized regions, each following polarization of one electrode through the IL medium. On the other extreme, upon imposing relatively fast 1 kHz SQW pulses the charge screening is prevented and the device is brought to assume a simple resistor role. A simple equivalent circuit model also reproduces the observed voltage transients qualitatively. The presented structure and variants of XPS measurements, enabling us to record voltage transients in unexpectedly large lateral distances away from the electrodes, can impact the understanding of various electrochemical concepts. © the Owner Societies 2016

Morphology and optical properties of thin silica films containing bimetallic Ag/Au nanoparticles

We have studied the optical spectra in the UV and visible regions, the morphology by scanning electron microscopy (SEM), and the X-ray photoelectron spectra (XPS) of bimetallic Ag/Au nanoparticles incorporated into transparent silicate films in the sol-gel transition stage. The bimetallic nanoparticles, obtained by a combination of photoreduction and thermal reduction, form structures of the alloy or core-shell type. © 2008 Springer Science+Business Media, Inc

XPS-evidence for in-situ electrochemically-generated carbene formation

Stable N-heterocyclic carbenes (NHC) are a class of compounds that has attracted a huge amount of interest in the last decade. One way to prepare NHCs is through chemical or electrochemical reduction of 1,3-disubstituted imidazolium cations. We are presenting an in-situ electrochemical X-ray Photoelectron Spectroscopy (XPS) study where electrochemically reduced imidazolium cations lead to production of stable NHC. The electroactive imidazolium species is not only the reactant, but also part of the ionic liquid which serves as the electrolyte, the medium and the electroactive material. This allows us to directly probe the difference between the parent imidazolium ion and the NHC through the use of XPS. The interpretation of the results is supported by both observation of reversible redox peaks in the voltammogram and the density functional theory calculations. © 2017 Elsevier Lt