Scanning electrochemical microscopy of graphene/polymer hybrid thin films as supercapacitors: Physical-chemical interfacial processes

Energy Technology Data Exchange (ETDEWEB)

Gupta, Sanju, E-mail: sanju.gupta@wku.edu; Price, Carson [Department of Physics and Astronomy, Western Kentucky University, 1906 College Heights Blvd., Bowling Green, KY 42101-3576 (United States)

2015-10-15

Hybrid electrode comprising an electric double-layer capacitor of graphene nanosheets and a pseudocapacitor of the electrically conducting polymers namely, polyaniline; PAni and polypyrrole; PPy are constructed that exhibited synergistic effect with excellent electrochemical performance as thin film supercapacitors for alternative energy. The hybrid supercapacitors were prepared by layer-by-layer (LbL) assembly based on controlled electrochemical polymerization followed by reduction of graphene oxide electrochemically producing ErGO, for establishing intimate electronic contact through nanoscale architecture and chemical stability, producing a single bilayer of (PAni/ErGO){sub 1}, (PPy/ErGO){sub 1}, (PAni/GO){sub 1} and (PPy/GO){sub 1}. The rationale design is to create thin films that possess interconnected graphene nanosheets (GNS) with polymer nanostructures forming well-defined tailored interfaces allowing sufficient surface adsorption and faster ion transport due to short diffusion distances. We investigated their electrochemical properties and performance in terms of gravimetric specific capacitance, C{sub s}, from cyclic voltammograms. The LbL-assembled bilayer films exhibited an excellent C{sub s} of ≥350 F g{sup −1} as compared with constituents (∼70 F g{sup −1}) at discharge current density of 0.3 A g{sup −1} that outperformed many other hybrid supercapacitors. To gain deeper insights into the physical-chemical interfacial processes occurring at the electrode/electrolyte interface that govern their operation, we have used scanning electrochemical microscopy (SECM) technique in feedback and probe approach modes. We present our findings from viewpoint of reinforcing the role played by heterogeneous electrode surface composed of nanoscale graphene sheets (conducting) and conducting polymers (semiconducting) backbone with ordered polymer chains via higher/lower probe current distribution maps. Also targeted is SECM imaging that allowed to determine

Scanning electrochemical microscopy of graphene/polymer hybrid thin films as supercapacitors: Physical-chemical interfacial processes

Science.gov (United States)

Gupta, Sanju; Price, Carson

2015-10-01

Hybrid electrode comprising an electric double-layer capacitor of graphene nanosheets and a pseudocapacitor of the electrically conducting polymers namely, polyaniline; PAni and polypyrrole; PPy are constructed that exhibited synergistic effect with excellent electrochemical performance as thin film supercapacitors for alternative energy. The hybrid supercapacitors were prepared by layer-by-layer (LbL) assembly based on controlled electrochemical polymerization followed by reduction of graphene oxide electrochemically producing ErGO, for establishing intimate electronic contact through nanoscale architecture and chemical stability, producing a single bilayer of (PAni/ErGO)1, (PPy/ErGO)1, (PAni/GO)1 and (PPy/GO)1. The rationale design is to create thin films that possess interconnected graphene nanosheets (GNS) with polymer nanostructures forming well-defined tailored interfaces allowing sufficient surface adsorption and faster ion transport due to short diffusion distances. We investigated their electrochemical properties and performance in terms of gravimetric specific capacitance, Cs, from cyclic voltammograms. The LbL-assembled bilayer films exhibited an excellent Cs of ≥350 F g-1 as compared with constituents (˜70 F g-1) at discharge current density of 0.3 A g-1 that outperformed many other hybrid supercapacitors. To gain deeper insights into the physical-chemical interfacial processes occurring at the electrode/electrolyte interface that govern their operation, we have used scanning electrochemical microscopy (SECM) technique in feedback and probe approach modes. We present our findings from viewpoint of reinforcing the role played by heterogeneous electrode surface composed of nanoscale graphene sheets (conducting) and conducting polymers (semiconducting) backbone with ordered polymer chains via higher/lower probe current distribution maps. Also targeted is SECM imaging that allowed to determine electrochemical (re)activity of surface ion adsorption sites

Photoelectrochemical kinetics of Eosin Y-sensitized zinc oxide films investigated by scanning electrochemical microscopy under illumination with different LED

International Nuclear Information System (INIS)

Shen Yan; Tefashe, Ushula Mengesha; Nonomura, Kazuteru; Loewenstein, Thomas; Schlettwein, Derck; Wittstock, Gunther

2009-01-01

The overall efficiency of the light-induced charge separation in dye-sensitized solar cells depends on the kinetic competition between back electron transfer and dye regeneration processes by a redox electrolyte. In a previous study, the reduction of the intermittently formed photo-oxidized dye molecules by iodide ions in the electrolyte phase was investigated using the feedback mode of a scanning electrochemical microscope (SECM) and a quantitative model had been derived. Here we provide a more thorough experimental verification of this model by variation of the excitation wavelength, light intensities and mediator concentrations. Nanoporous ZnO/Eosin Y films prepared by self-assembly were used as model electrodes and were used with an iodide/triiodide electrolyte. The experimentally found effective rate constants could be related to the rate constant for the reaction of the dissolved donor with photo-oxidized Eosin Y bound to ZnO and the absorption spectrum of the dye and confirmed the assumption made in the derivation of the model. For the regeneration process of Eosin Y, a rate constant of k ox with different light emitting diodes and light intensities is determined.

Photoelectrochemical kinetics of Eosin Y-sensitized zinc oxide films investigated by scanning electrochemical microscopy under illumination with different LED

Energy Technology Data Exchange (ETDEWEB)

Shen Yan; Tefashe, Ushula Mengesha [Department of Pure and Applied Chemistry, Faculty of Mathematics and Natural Sciences, Carl von Ossietzky University of Oldenburg, D-26111 Oldenburg (Germany); Nonomura, Kazuteru; Loewenstein, Thomas; Schlettwein, Derck [Institute of Applied Physics, Justus Liebig University of Giessen, Heinrich-Buff-Ring 16, D-35392 Giessen (Germany); Wittstock, Gunther, E-mail: gunther.wittstock@uni-oldenburg.d [Department of Pure and Applied Chemistry, Faculty of Mathematics and Natural Sciences, Carl von Ossietzky University of Oldenburg, D-26111 Oldenburg (Germany)

2009-12-30

The overall efficiency of the light-induced charge separation in dye-sensitized solar cells depends on the kinetic competition between back electron transfer and dye regeneration processes by a redox electrolyte. In a previous study, the reduction of the intermittently formed photo-oxidized dye molecules by iodide ions in the electrolyte phase was investigated using the feedback mode of a scanning electrochemical microscope (SECM) and a quantitative model had been derived. Here we provide a more thorough experimental verification of this model by variation of the excitation wavelength, light intensities and mediator concentrations. Nanoporous ZnO/Eosin Y films prepared by self-assembly were used as model electrodes and were used with an iodide/triiodide electrolyte. The experimentally found effective rate constants could be related to the rate constant for the reaction of the dissolved donor with photo-oxidized Eosin Y bound to ZnO and the absorption spectrum of the dye and confirmed the assumption made in the derivation of the model. For the regeneration process of Eosin Y, a rate constant of k{sub ox} with different light emitting diodes and light intensities is determined.

Electron transfer kinetics of cytochrome c immobilized on a phenolic terminated thiol self assembled monolayer determined by scanning electrochemical microscopy

International Nuclear Information System (INIS)

Alizadeh, Vali; Mousavi, Mir Fazlollah; Mehrgardi, Masoud Ayatollahi; Kazemi, Sayed Habib; Sharghi, Hashem

2011-01-01

Highlights: → Preparing a thiolated phenolic self-assembled monolayer surface (SAM). → Application of this SAM to immobilize cytochrome C. → Scanning electrochemical microscopy used for these studies. → Determination of both tunneling electron transfer and bimolecular rate constants between the immobilized protein-substrate and probe. - Abstract: In the present manuscript, the electrochemical behavior of cytochrome c (cyt-c) immobilized onto a phenolic terminated self assembled monolayer (SAM) on a gold electrode is investigated using cyclic voltammetry (CV) and scanning electrochemical microscopy (SECM). The tunneling electron transfer (ET) rate constant between the immobilized protein and the underlying electrode surface, and also the bimolecular ET rate constant between the immobilized protein and a probe has been obtained using approach curves that were obtained by SECM. The approach curves were recorded at different substrate overpotentials in the presence of various concentrations of ferrocyanide as a probe and various surface concentrations of cyt-c; then the standard tunneling ET and bimolecular rate constants are obtained as 3.4 ± 0.3 s -1 and (2.0 ± 0.5) x 10 7 cm 3 mol -1 s -1 , respectively.

Electron transfer kinetics of cytochrome c immobilized on a phenolic terminated thiol self assembled monolayer determined by scanning electrochemical microscopy

Energy Technology Data Exchange (ETDEWEB)

Alizadeh, Vali [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Mousavi, Mir Fazlollah, E-mail: mousavim@modares.ac.ir [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Mehrgardi, Masoud Ayatollahi [Department of Chemistry, University of Isfahan, Isfahan (Iran, Islamic Republic of); Kazemi, Sayed Habib [Department of Chemistry, Institute for Advanced Studies in Basic Sciences (IASBS), Zanjan (Iran, Islamic Republic of); Sharghi, Hashem [Department of Chemistry, Shiraz University, Shiraz (Iran, Islamic Republic of)

2011-07-01

Highlights: > Preparing a thiolated phenolic self-assembled monolayer surface (SAM). > Application of this SAM to immobilize cytochrome C. > Scanning electrochemical microscopy used for these studies. > Determination of both tunneling electron transfer and bimolecular rate constants between the immobilized protein-substrate and probe. - Abstract: In the present manuscript, the electrochemical behavior of cytochrome c (cyt-c) immobilized onto a phenolic terminated self assembled monolayer (SAM) on a gold electrode is investigated using cyclic voltammetry (CV) and scanning electrochemical microscopy (SECM). The tunneling electron transfer (ET) rate constant between the immobilized protein and the underlying electrode surface, and also the bimolecular ET rate constant between the immobilized protein and a probe has been obtained using approach curves that were obtained by SECM. The approach curves were recorded at different substrate overpotentials in the presence of various concentrations of ferrocyanide as a probe and various surface concentrations of cyt-c; then the standard tunneling ET and bimolecular rate constants are obtained as 3.4 {+-} 0.3 s{sup -1} and (2.0 {+-} 0.5) x 10{sup 7} cm{sup 3} mol{sup -1} s{sup -1}, respectively.

Characterization of electro-oxidation catalysts using scanning electrochemical and mass spectral methods

Science.gov (United States)

Jambunathan, Krishnakumar

Low temperature fuel cells have many potential benefits, including high efficiency, high energy density and environmental friendliness. However, logistically appealing fuels for this system, such as reformed hydrocarbons or alcohols, exhibit poor performance because of catalyst poisoning that occurs during oxidation at the anode. This research focuses on the analysis of several model fuels and catalyst materials to understand the impact of catalyst poisoning on reactivity. Two novel experimental tools were developed based upon the local measurement of catalyst performance using scanning, reactivity mapping probes. The Scanning Electrochemical Microscope (SECM) was used to directly measure the rate constant for hydrogen oxidation in the presence and absence of dissolved CO. The Scanning Differential Electrochemical Mass Spectrometer (SDEMS) was exploited to measure the partial and complete oxidation products of methanol and ethanol oxidation. The reactivity of Pt and Pt/Ru catalysts towards the hydrogen oxidation reaction in the absence and presence of adsorbed CO was elucidated using the SECM. Steady state rate constant measurements in the absence of CO showed that the rate of hydrogen oxidation reaction exceeded 1 cms-1 . Steady state rate constant measurements in the presence of CO indicated that the platinum surface is completely inactive due to adsorbed CO. Addition of as little as 6% Ru to the Pt electrode was found to significantly improve the activity of the electrode towards CO removal. SDEMS was used to study the electro-oxidation of methanol on Pt xRuy electrodes at different electrode potentials and temperatures. Screening measurements performed with the SDEMS showed that PtxRu y electrodes containing 6--40% Ru had the highest activity for methanol oxidation. Current efficiencies for CO2 were also calculated under different conditions. SDEMS was also used to study the electro-oxidation of ethanol on Pt xRuy electrodes. The reaction was found to occur

A Study of the Mechanism of the Hydrogen Evolution Reaction on Nickel by Surface Interrogation Scanning Electrochemical Microscopy.

Science.gov (United States)

Liang, Zhenxing; Ahn, Hyun S; Bard, Allen J

2017-04-05

The hydrogen evolution reaction (HER) on Ni in alkaline media was investigated by scanning electrochemical microscopy under two operating modes. First, the substrate generation/tip collection mode was employed to extract the "true" cathodic current associated with the HER from the total current in the polarization curve. Compared to metallic Ni, the electrocatalytic activity of the HER is improved in the presence of the low-valence-state oxide of Ni. This result is in agreement with a previous claim that the dissociative adsorption of water can be enhanced at the Ni/Ni oxide interface. Second, the surface-interrogation scanning electrochemical microscopy (SI-SECM) mode was used to directly measure the coverage of the adsorbed hydrogen on Ni at given potentials. Simulation indicates that the hydrogen coverage follows a Frumkin isotherm with respect to the applied potential. On the basis of the combined analysis of the Tafel slope and surface hydrogen coverage, the rate-determining step is suggested to be the adsorption of hydrogen (Volmer step) in the investigated potential window.

Scanning drop sensor

Energy Technology Data Exchange (ETDEWEB)

Jin, Jian; Xiang, Chengxiang; Gregoire, John M.; Shinde, Aniketa A.; Guevarra, Dan W.; Jones, Ryan J.; Marcin, Martin R.; Mitrovic, Slobodan

2017-05-09

Electrochemical or electrochemical and photochemical experiments are performed on a collection of samples by suspending a drop of electrolyte solution between an electrochemical experiment probe and one of the samples that serves as a test sample. During the electrochemical experiment, the electrolyte solution is added to the drop and an output solution is removed from the drop. The probe and collection of samples can be moved relative to one another so the probe can be scanned across the samples.

Real-time mapping of salt glands on the leaf surface of Cynodon dactylon L. using scanning electrochemical microscopy.

Science.gov (United States)

Parthasarathy, Meera; Pemaiah, Brindha; Natesan, Ravichandran; Padmavathy, Saralla R; Pachiappan, Jayaraman

2015-02-01

Salt glands are specialized organelles present in the leaf tissues of halophytes, which impart salt-tolerance capability to the plant species. These glands are usually identified only by their morphology using conventional staining procedures coupled with optical microscopy. In this work, we have employed scanning electrochemical microscopy to identify the salt glands not only by their morphology but also by their salt excretion behavior. Bermuda grass (Cynodon dactylon L.) species was chosen for the study as they are known to be salt-tolerant and contain salt glands on leaf surfaces. Scanning electrochemical microscopy performed in sodium chloride medium in the presence and absence of potassium ferrocyanide as redox mediator, reveals the identity of salt glands. More insight into the ion expulsion behavior of these glands was obtained by mapping lateral and vertical variations in ion concentrations using surface impedance measurements which indicated five times higher resistance over the salt glands compared to the surrounding tissues and bulk solution. The protocol could be used to understand the developmental processes in plants grown in different soil/water conditions in order to improve salt tolerance of food crops by genetic engineering and hence improve their agricultural productivity.

Voltammetric studies on the electrochemical determination of methylmercury in chloride medium at carbon microelectrodes

Energy Technology Data Exchange (ETDEWEB)

Ribeiro, F. [Centro de Electroquimica e Cinetica da Universidade de Lisboa, Departamento de Quimica e Bioquimica, Faculdade de Ciencias, Universidade de Lisboa, Campo Grande, Ed. C8, 1749-016 Lisbon (Portugal); Neto, M.M.M. [Centro de Electroquimica e Cinetica da Universidade de Lisboa, Departamento de Quimica e Bioquimica, Faculdade de Ciencias, Universidade de Lisboa, Campo Grande, Ed. C8, 1749-016 Lisbon (Portugal) and Departamento de Quimica Agricola e Ambiental, Instituto Superior de Agronomia, Tapada da Ajuda, 1349-017 Lisbon (Portugal)]. E-mail: mm.neto@netcabo.pt; Rocha, M.M. [Centro de Electroquimica e Cinetica da Universidade de Lisboa, Departamento de Quimica e Bioquimica, Faculdade de Ciencias, Universidade de Lisboa, Campo Grande, Ed. C8, 1749-016 Lisbon (Portugal); Fonseca, I.T.E. [Centro de Electroquimica e Cinetica da Universidade de Lisboa, Departamento de Quimica e Bioquimica, Faculdade de Ciencias, Universidade de Lisboa, Campo Grande, Ed. C8, 1749-016 Lisbon (Portugal)

2006-10-10

Electroanalytical techniques have been used to determine methylmercury at low levels in environmental matrices. The electrochemical behaviour of methylmercury at carbon microelectrodes in a hydrochloric acid medium using cyclic, square wave and fast-scan linear-sweep voltammetric techniques has been investigated. The analytical utility of the methylmercury reoxidation peak has been explored, but the recorded peak currents were found to be poorly reproducible. This is ascribed to two factors: the adsorption of insoluble chloromercury compounds on the electrode surface, which appears to be an important contribution to hinder the voltammetric signal of methylmercury; and the competition between the reoxidation of the methylmercury radical and its dimerization reaction, which limits the reproducibility of the methylmercury peak. These problems were successfully overcome by adopting the appropriate experimental conditions. Fast-scan rates were employed and an efficient electrochemical regeneration procedure of the electrode surface was achieved, under potentiostatic conditions in a mercury-free solution containing potassium thiocyanate-a strong complexing agent. The influence of chloride ion concentration was analysed. Interference by metals, such as lead and cadmium, was considered. Calibration plots were obtained in the micromolar and submicromolar concentration ranges, allowing the electrochemical determination of methylmercury in trace amounts. An estuarine water sample was analysed using the new method with a glassy carbon microelectrode.

Voltammetric studies on the electrochemical determination of methylmercury in chloride medium at carbon microelectrodes

International Nuclear Information System (INIS)

Ribeiro, F.; Neto, M.M.M.; Rocha, M.M.; Fonseca, I.T.E.

2006-01-01

Electroanalytical techniques have been used to determine methylmercury at low levels in environmental matrices. The electrochemical behaviour of methylmercury at carbon microelectrodes in a hydrochloric acid medium using cyclic, square wave and fast-scan linear-sweep voltammetric techniques has been investigated. The analytical utility of the methylmercury reoxidation peak has been explored, but the recorded peak currents were found to be poorly reproducible. This is ascribed to two factors: the adsorption of insoluble chloromercury compounds on the electrode surface, which appears to be an important contribution to hinder the voltammetric signal of methylmercury; and the competition between the reoxidation of the methylmercury radical and its dimerization reaction, which limits the reproducibility of the methylmercury peak. These problems were successfully overcome by adopting the appropriate experimental conditions. Fast-scan rates were employed and an efficient electrochemical regeneration procedure of the electrode surface was achieved, under potentiostatic conditions in a mercury-free solution containing potassium thiocyanate-a strong complexing agent. The influence of chloride ion concentration was analysed. Interference by metals, such as lead and cadmium, was considered. Calibration plots were obtained in the micromolar and submicromolar concentration ranges, allowing the electrochemical determination of methylmercury in trace amounts. An estuarine water sample was analysed using the new method with a glassy carbon microelectrode

Instrumentation for in situ flow electrochemical Scanning Transmission X-ray Microscopy (STXM)

Science.gov (United States)

Prabu, Vinod; Obst, Martin; Hosseinkhannazer, Hooman; Reynolds, Matthew; Rosendahl, Scott; Wang, Jian; Hitchcock, Adam P.

2018-06-01

We report the design and performance of a 3-electrode device for real time in situ scanning transmission X-ray microscopy studies of electrochemical processes under both static (sealed, non-flow) conditions and with a continuous flow of electrolytes. The device was made using a combination of silicon microfabrication and 3D printing technologies. The performance is illustrated by results of a study of copper deposition and stripping at a gold working electrode. X-ray absorption spectromicroscopy at the Cu 2p edge was used to follow the evolution as a function of potential and time of the spatial distributions of Cu(0) and Cu(i) species electro-deposited from an aqueous solution of copper sulphate. The results are interpreted in terms of competing mechanisms for the reduction of Cu(ii).

Scanning drop sensor

Energy Technology Data Exchange (ETDEWEB)

Jin, Jian; Xiang, Chengxiang; Gregoire, John

2017-05-09

Electrochemical experiments are performed on a collection of samples by suspending a drop of electrolyte solution between an electrochemical experiment probe and one of the samples that serves as a test sample. During the electrochemical experiment, the electrolyte solution is added to the drop and an output solution is removed from the drop. The probe and collection of samples can be moved relative to one another so the probe can be scanned across the samples.

Note: A quartz cell with Pt single crystal bead electrode for electrochemical scanning tunneling microscope measurements.

Science.gov (United States)

Xia, Zhigang; Wang, Jihao; Hou, Yubin; Lu, Qingyou

2014-09-01

In this paper, we provide and demonstrate a design of a unique cell with Pt single crystal bead electrode for electrochemical scanning tunneling microscope (ECSTM) measurements. The active metal Pt electrode can be protected from air contamination during the preparation process. The transparency of the cell allows the tip and bead to be aligned by direct observation. Based on this, a new and effective alignment method is introduced. The high-quality bead preparations through this new cell have been confirmed by the ECSTM images of Pt (111).

Two-step controllable electrochemical etching of tungsten scanning probe microscopy tips

KAUST Repository

Khan, Yasser; Al-Falih, Hisham; Ng, Tien Khee; Ooi, Boon S.; Zhang, Yaping

2012-01-01

Dynamic electrochemical etching technique is optimized to produce tungsten tips with controllable shape and radius of curvature of less than 10 nm. Nascent features such as dynamic electrochemical etching and reverse biasing after drop-off are utilized, and two-step dynamic electrochemical etching is introduced to produce extremely sharp tips with controllable aspect ratio. Electronic current shut-off time for conventional dc drop-off technique is reduced to ?36 ns using high speed analog electronics. Undesirable variability in tip shape, which is innate to static dc electrochemical etching, is mitigated with novel dynamic electrochemical etching. Overall, we present a facile and robust approach, whereby using a novel etchant level adjustment mechanism, 30° variability in cone angle and 1.5 mm controllability in cone length were achieved, while routinely producing ultra-sharp probes. © 2012 American Institute of Physics.

Multiscale electrochemical analysis of the corrosion of titanium and nitinol for implant applications

International Nuclear Information System (INIS)

Izquierdo, J.; González-Marrero, M.B.; Bozorg, M.; Fernández-Pérez, B.M.; Vasconcelos, H.C.; Santana, J.J.; Souto, R.M.

2016-01-01

Highlights: • Direct screening of differences in the surface reactivity of the passive layers formed on pure titanium and nitinol. • Distinct effect of polarization on the passive layers. • Detection of nickel soluble species released from corrosion pits. - Abstract: Surface electrochemical activity of titanium and nitinol biomaterials in naturally aerated Ringer’s physiological solution was investigated using potentiodynamic polarization and scanning electrochemical microscopy (SECM) techniques. SECM was operated in feedback and redox competition modes as a function of potential applied to the substrate. The kinetics of the electron transfer rate on both materials was characterized by mathematical modelling of the Z-approach curves monitored under feedback conditions. The rate constant values greatly depended on the characteristics of the passive layers formed over the metals under potentiostatic control. A more insulating film was found on nitinol when biased at low polarizations, resulting in smaller tip current increments during tip approach to the investigated surface under positive feedback and competition operation modes. However, at higher anodic polarizations, nitinol passive layers experience breakdown, and therefore tip current values reflect the release of metal cations from the biomaterial surface.

Coating of tips for electrochemical scanning tunneling microscopy by means of silicon, magnesium, and tungsten oxides

Science.gov (United States)

Salerno, Marco

2010-09-01

Different combinations of metal tips and oxide coatings have been tested for possible operation in electrochemical scanning tunneling microscopy. Silicon and magnesium oxides have been thermally evaporated onto gold and platinum-iridium tips, respectively. Two different thickness values have been explored for both materials, namely, 40 and 120 nm for silicon oxide and 20 and 60 nm for magnesium oxide. Alternatively, tungsten oxide has been grown on tungsten tips via electrochemical anodization. In the latter case, to seek optimal results we have varied the pH of the anodizing electrolyte between one and four. The oxide coated tips have been first inspected by means of scanning electron microscopy equipped with microanalysis to determine the morphological results of the coating. Second, the coated tips have been electrically characterized ex situ for stability in time by means of cyclic voltammetry in 1 M aqueous KCl supporting electrolyte, both bare and supplemented with K3[Fe(CN)6] complex at 10 mM concentration in milliQ water as an analyte. Only the tungsten oxide coated tungsten tips have shown stable electrical behavior in the electrolyte. For these tips, the uncoated metal area has been estimated from the electrical current levels, and they have been successfully tested by imaging a gold grating in situ, which provided stable results for several hours. The successful tungsten oxide coating obtained at pH=4 has been assigned to the WO3 form.

Direct evidence of ionic fluxes across ion-selective membranes: a scanning electrochemical microscopic and potentiometric study.

Science.gov (United States)

Gyurcsányi, R E; Pergel, E; Nagy, R; Kapui, I; Lan, B T; Tóth, K; Bitter, I; Lindner, E

2001-05-01

Scanning electrochemical microscopy (SECM) supplemented with potentiometric measurements was used to follow the time-dependent buildup of a steady-state diffusion layer at the aqueous-phase boundary of lead ion-selective electrodes (ISEs). Differential pulse voltammetry is adapted to SECM for probing the local concentration profiles at the sample side of solvent polymeric membranes. Major factors affecting the membrane transport-related surface concentrations were identified from SECM data and the potentiometric transients obtained under different experimental conditions (inner filling solution composition, membrane thickness, surface pretreatment). The amperometrically determined surface concentrations correlated well with the lower detection limits of the lead ion-selective electrodes.

Characterisation of biosynthesised silver nanoparticles by scanning electrochemical microscopy (SECM) and voltammetry.

Science.gov (United States)

Battistel, Dario; Baldi, Franco; Gallo, Michele; Faleri, Claudia; Daniele, Salvatore

2015-01-01

Silver nanoparticles (AgNPs) were biosynthesised by a Klebsiella oxytoca strain BAS-10, which, during its growth, is known to produce a branched exopolysaccharide (EPS). Klebsiella oxytoca cultures, treated with AgNO3 and grown under either aerobic or anaerobic conditions, produced silver nanoparticles embedded in EPS (AgNPs-EPS) containing different amounts of Ag(0) and Ag(I) forms. The average size of the AgNPs-EPS was determined by transmission electron microscopy, while the relative abundance of Ag(0)- or Ag(I)-containing AgNPs-EPS was established by scanning electrochemical microscopy (SECM). Moreover, the release of silver(I) species from the various types of AgNPs-EPS was investigated by combining SECM with anodic stripping voltammetry. These measurements allowed obtaining information on the kinetic of silver ions release from AgNPs-EPS and their concentration profiles at the substrate/water interface. Copyright © 2014 Elsevier B.V. All rights reserved.

ELECTROCHEMICAL STUDIES OF CARBON STEEL CORROSION IN HANFORD DOUBLE SHELL TANK (DST) WASTE

Energy Technology Data Exchange (ETDEWEB)

DUNCAN, J.B.; WINDISCH, C.F.

2006-10-13

This paper reports on the electrochemical scans for the supernatant of Hanford double-shell tank (DST) 241-SY-102 and the electrochemical scans for the bottom saltcake layer for Hanford DST 241-AZ-102. It further reports on the development of electrochemical test cells adapted to both sample volume and hot cell constraints.

Quantifying Chemical and Electrochemical Reactions in Liquids by in situ Electron Microscopy

DEFF Research Database (Denmark)

Canepa, Silvia

and developing a robust imaging analysis method for quantitatively understand chemical and electrochemical process during in situ liquid electron microscopy. By using two custom-made liquid cells (an electrochemical scanning electron microscopy (EC-SEM) platform and Liquid Flow S/TEM holder) beam...... of electrochemical deposition of copper (Cu) by electrochemical liquid scanning electron microscopy (EC-SEM) was done in order to direct observe the formation of dendritic structures. Finally the shape evolution from solid to hollow structures through galvanic replacement reactions were observed for different silver...

Detection of CO2•- in the Electrochemical Reduction of Carbon Dioxide in N,N-Dimethylformamide by Scanning Electrochemical Microscopy.

Science.gov (United States)

Kai, Tianhan; Zhou, Min; Duan, Zhiyao; Henkelman, Graeme A; Bard, Allen J

2017-12-27

The electrocatalytic reduction of CO 2 has been studied extensively and produces a number of products. The initial reaction in the CO 2 reduction is often taken to be the 1e formation of the radical anion, CO 2 •- . However, the electrochemical detection and characterization of CO 2 •- is challenging because of the short lifetime of CO 2 •- , which can dimerize and react with proton donors and even mild oxidants. Here, we report the generation and quantitative determination of CO 2 •- in N,N-dimethylformamide (DMF) with the tip generation/substrate collection (TG/SC) mode of scanning electrochemical microscopy (SECM). CO 2 was reduced at a hemisphere-shaped Hg/Pt ultramicroelectrode (UME) or a Hg/Au film UME, which were utilized as the SECM tips. The CO 2 •- produced can either dimerize to form oxalate within the nanogap between SECM tip and substrate or collected at SECM substrate (e.g., an Au UME). The collection efficiency (CE) for CO 2 •- depends on the distance (d) between the tip and substrate. The dimerization rate (6.0 × 10 8 M -1 s -1 ) and half-life (10 ns) of CO 2 •- can be evaluated by fitting the collection efficiency vs distance curve. The dimerized species of CO 2 •- , oxalate, can also be determined quantitatively. Furthermore, the formal potential (E 0 ') and heterogeneous rate constant (k 0 ) for CO 2 reduction were determined with different quaternary ammonium electrolytes. The significant difference in k 0 is due to a tunneling effect caused by the adsorption of the electrolytes on the electrode surface at negative potentials.

Local electrochemical evaluation of a self-healing coating based on encapsulated healing-agent

NARCIS (Netherlands)

González-García, Y.; García, S.J.; Fischer, H.R.; Hughes, A.E.; Mol, J.M.C.

2011-01-01

In this work local electrochemical techniques are introduced as powerful and complementary techniques for the in-situ evaluation of self-healing systems applied for the protection of metals against corrosion. Scanning vibrating electrode technique (SVET) and scanning electrochemical microscopy

Surface Interrogation Scanning Electrochemical Microscopy for a Photoelectrochemical Reaction: Water Oxidation on a Hematite Surface.

Science.gov (United States)

Kim, Jae Young; Ahn, Hyun S; Bard, Allen J

2018-03-06

To understand the pathway of a photoelectrochemical (PEC) reaction, quantitative knowledge of reaction intermediates is important. We describe here surface interrogation scanning electrochemical microscopy for this purpose (PEC SI-SECM), where a light pulse to a photoactive semiconductor film at a given potential generates intermediates that are then analyzed by a tip generated titrant at known times after the light pulse. The improvements were demonstrated for photoelectrochemical water oxidation (oxygen evolution) reaction on a hematite surface. The density of photoactive sites, proposed to be Fe 4+ species, on a hematite surface was successfully quantified, and the photoelectrochemical water oxidation reaction dynamics were elucidated by time-dependent redox titration experiments. The new configuration of PEC SI-SECM should find expanded usage to understand and investigate more complicated PEC reactions with other materials.

Alizarin Red S as an electrochemical indicator for saccharide recognition

Energy Technology Data Exchange (ETDEWEB)

Schumacher, Soeren, E-mail: soeren.schumacher@ibmt.fraunhofer.de [Fraunhofer Institute for Biomedical Engineering, Am Muehlenberg 13, 14476 Potsdam (Germany); Nagel, Thomas; Scheller, Frieder W.; Gajovic-Eichelmann, Nenad [Fraunhofer Institute for Biomedical Engineering, Am Muehlenberg 13, 14476 Potsdam (Germany)

2011-07-30

Graphical abstract: Display Omitted Highlights: > Transfer of the established Alizarin Red S (ARS) for saccharide-boronic acid interaction to electrochemistry. > Investigation of electrochemical behaviour of ARS and its interaction with phenylboronic acid at pH 7.4. > Through addition of fructose the ARS was displaced. > Displaced ARS could be monitored electrochemically corresponding to the used fructose concentration. - Abstract: In addition to the well-established spectroscopic Alizarin Red S (ARS) assay for the determination of binding constants between arylboronic acids and different saccharides, we report the use of ARS as a reporter in an electrochemical set-up. The electrochemical properties of ARS, the binding to phenyl boronic acid (PBA) and the competition with fructose in phosphate buffer at pH 7.4 were investigated by cyclic voltammetry (CV). By choosing a negative scan direction (starting at +0.2 V), a quasi-reversible process was detected at E{sup 0}' = -0.59V with {Delta}E{sub p} = 0.1V. An irreversible oxidation peak at +0.42 V could also be detected. These peaks are characterised both as a 2-proton-2-electron transfer and corresponds to the oxidation and reduction of the anthraquinone or the ortho-quinone moiety. After addition of phenylboronic acid a new oxidation peaks occurred at -0.42 V which correlates with the ARS-PBA interaction. The peak current increased with increasing phenylboronic acid concentration according to the release of BA and formation of the ARS-PBA ester. After addition of fructose the peak current decreases again, in proportion to the fructose concentration, enabling the use of ARS as an electrochemical reporter for fructose detection up to 50 mM. Also the interaction with other cis-diol containing compounds such as sorbitol, mannitol, glucose and mannose was investigated and a dependence based on already published binding constants to phenylboronic acid could be shown.

Alizarin Red S as an electrochemical indicator for saccharide recognition

International Nuclear Information System (INIS)

Schumacher, Soeren; Nagel, Thomas; Scheller, Frieder W.; Gajovic-Eichelmann, Nenad

2011-01-01

Graphical abstract: Display Omitted Highlights: → Transfer of the established Alizarin Red S (ARS) for saccharide-boronic acid interaction to electrochemistry. → Investigation of electrochemical behaviour of ARS and its interaction with phenylboronic acid at pH 7.4. → Through addition of fructose the ARS was displaced. → Displaced ARS could be monitored electrochemically corresponding to the used fructose concentration. - Abstract: In addition to the well-established spectroscopic Alizarin Red S (ARS) assay for the determination of binding constants between arylboronic acids and different saccharides, we report the use of ARS as a reporter in an electrochemical set-up. The electrochemical properties of ARS, the binding to phenyl boronic acid (PBA) and the competition with fructose in phosphate buffer at pH 7.4 were investigated by cyclic voltammetry (CV). By choosing a negative scan direction (starting at +0.2 V), a quasi-reversible process was detected at E 0 ' = -0.59V with ΔE p = 0.1V. An irreversible oxidation peak at +0.42 V could also be detected. These peaks are characterised both as a 2-proton-2-electron transfer and corresponds to the oxidation and reduction of the anthraquinone or the ortho-quinone moiety. After addition of phenylboronic acid a new oxidation peaks occurred at -0.42 V which correlates with the ARS-PBA interaction. The peak current increased with increasing phenylboronic acid concentration according to the release of BA and formation of the ARS-PBA ester. After addition of fructose the peak current decreases again, in proportion to the fructose concentration, enabling the use of ARS as an electrochemical reporter for fructose detection up to 50 mM. Also the interaction with other cis-diol containing compounds such as sorbitol, mannitol, glucose and mannose was investigated and a dependence based on already published binding constants to phenylboronic acid could be shown.

Electrochemical deposition of coatings of highly entropic alloys from non-aqueous solutions

Directory of Open Access Journals (Sweden)

Jeníček V.

2016-03-01

Full Text Available The paper deals with electrochemical deposition of coatings of highly entropic alloys. These relatively new materials have been recently intensively studied. The paper describes the first results of electrochemical coating with highly entropic alloys by deposition from non-aqueous solutions. An electrochemical device was designed and coatings were deposited. The coatings were characterised with electronic microscopy scanning, atomic absorption spectrometry and X-ray diffraction methods and the combination of methods of thermic analysis of differential scanning calorimetry and thermogravimetry.

Electrochemical Analysis of Neurotransmitters

Science.gov (United States)

Bucher, Elizabeth S.; Wightman, R. Mark

2015-07-01

Chemical signaling through the release of neurotransmitters into the extracellular space is the primary means of communication between neurons. More than four decades ago, Ralph Adams and his colleagues realized the utility of electrochemical methods for the study of easily oxidizable neurotransmitters, such as dopamine, norepinephrine, and serotonin and their metabolites. Today, electrochemical techniques are frequently coupled to microelectrodes to enable spatially resolved recordings of rapid neurotransmitter dynamics in a variety of biological preparations spanning from single cells to the intact brain of behaving animals. In this review, we provide a basic overview of the principles underlying constant-potential amperometry and fast-scan cyclic voltammetry, the most commonly employed electrochemical techniques, and the general application of these methods to the study of neurotransmission. We thereafter discuss several recent developments in sensor design and experimental methodology that are challenging the current limitations defining the application of electrochemical methods to neurotransmitter measurements.

Electrochemical Oscillation of Vanadium Ions in Anolyte

Directory of Open Access Journals (Sweden)

Hao Peng

2017-08-01

Full Text Available Periodic electrochemical oscillation of the anolyte was reported for the first time in a simulated charging process of the vanadium redox flow batteries. The electrochemical oscillation could be explained in terms of the competition between the growth and the chemical dissolution of V2O5 film. Also, the oscillation phenomenon was possible to regular extra power consumption. The results of this paper might enable new methods to improve the charge efficiency and energy saving for vanadium redox flow batteries.

Electrochemically deposited hybrid nickel-cobalt hexacyanoferrate nanostructures for electrochemical supercapacitors

International Nuclear Information System (INIS)

Safavi, A.; Kazemi, S.H.; Kazemi, H.

2011-01-01

Highlights: → Nanostructured hybrid nickel-cobalt hexacyanoferrate is used in supercapacitors. → A high capacitance (765 F g -1 ) is obtained at a specific current of 0.2 A g -1 . → Long cycle-life and excellent stability are demonstrated during 1000 cycles. - Abstract: This study describes the use of electrodeposited nanostructured hybrid nickel-cobalt hexacyanoferrate in electrochemical supercapacitors. Herein, various compositions of nickel and cobalt hexacyanoferrates (Ni/CoHCNFe) nanostructures are electrodeposited on an inexpensive stainless steel substrate using cyclic voltammetric (CV) method. The morphology of the electrodeposited nanostructures is studied using scanning electron microscopy, while their electrochemical characterizations are investigated using CV, galvanostatic charge and discharge and electrochemical impedance spectroscopy. The results show that the nanostructures of hybrid metal cyanoferrate, shows a much higher capacitance (765 F g -1 ) than those obtained with just nickel hexacyanoferrate (379 F g -1 ) or cobalt hexacyanoferrate (277 F g -1 ). Electrochemical impedance spectroscopy results confirm the favorable capacitive behavior of the electrodeposited materials. The columbic efficiency is approximately 95% based on the charge and discharge experiments. Long cycle-life and excellent stability of the nanostructured materials are also demonstrated during 1000 cycles.

Electrochemically deposited hybrid nickel-cobalt hexacyanoferrate nanostructures for electrochemical supercapacitors

Energy Technology Data Exchange (ETDEWEB)

Safavi, A., E-mail: safavi@chem.susc.ac.ir [Department of Chemistry, College of Sciences, Shiraz University, Shiraz 71454 (Iran, Islamic Republic of); Nanotechnology Research Institute, Shiraz University, Shiraz (Iran, Islamic Republic of); Kazemi, S.H., E-mail: habibkazemi@iasbs.ac.ir [Department of Chemistry, Institute for Advanced Studies in Basic Sciences (IASBS), Zanjan 45137-66731 (Iran, Islamic Republic of); Kazemi, H. [Department of Chemistry, College of Sciences, Shiraz University, Shiraz 71454 (Iran, Islamic Republic of)

2011-10-30

Highlights: > Nanostructured hybrid nickel-cobalt hexacyanoferrate is used in supercapacitors. > A high capacitance (765 F g{sup -1}) is obtained at a specific current of 0.2 A g{sup -1}. > Long cycle-life and excellent stability are demonstrated during 1000 cycles. - Abstract: This study describes the use of electrodeposited nanostructured hybrid nickel-cobalt hexacyanoferrate in electrochemical supercapacitors. Herein, various compositions of nickel and cobalt hexacyanoferrates (Ni/CoHCNFe) nanostructures are electrodeposited on an inexpensive stainless steel substrate using cyclic voltammetric (CV) method. The morphology of the electrodeposited nanostructures is studied using scanning electron microscopy, while their electrochemical characterizations are investigated using CV, galvanostatic charge and discharge and electrochemical impedance spectroscopy. The results show that the nanostructures of hybrid metal cyanoferrate, shows a much higher capacitance (765 F g{sup -1}) than those obtained with just nickel hexacyanoferrate (379 F g{sup -1}) or cobalt hexacyanoferrate (277 F g{sup -1}). Electrochemical impedance spectroscopy results confirm the favorable capacitive behavior of the electrodeposited materials. The columbic efficiency is approximately 95% based on the charge and discharge experiments. Long cycle-life and excellent stability of the nanostructured materials are also demonstrated during 1000 cycles.

Scanning Kelvin probe force microscopy as a means of predicting the electrochemical characteristics of the surface of a modified AA4xxx/AA3xxx (Al alloys) brazing sheet

International Nuclear Information System (INIS)

Afshar, F. Norouzi; Wit, J.H.W. de; Terryn, H.; Mol, J.M.C.

2013-01-01

Highlights: ► Macro- and micro-electrochemical surface properties of an aluminium brazing sheet were investigated. ► Electrochemical surface properties before and after brazing were studied and compared. ► Scanning Kelvin probe force microscopy and potentiodynamic polarization measurements were performed. ► The electrochemical responses were correlated to the pre- and post-brazing treatment microstructure. -- Abstract: Macro- and micro-electrochemical properties of clad and core surfaces of a modified AA4xxx/AA3xxx brazing sheet material, before and after brazing, have been evaluated and compared. By scanning Kelvin probe force microscopy (SKPFM), the Volta potential distribution over the brazed and non-brazed clad surfaces was measured. The changes in the Volta potential maps were correlated to the macro-electrochemical responses of the surfaces and the microstructural features that evolve as a result of brazing. By performing potentiodynamic polarization experiments and microscopic analysis of the corroded surfaces and cross sections, the suitability of SKPFM analysis for corrosion performance prediction of the aluminium brazing sheet material in a sea water acidified accelerated test (SWAAT) environment was confirmed. Considering the purity of Si phase in the structures of both brazed and non-brazed material, it is suggested that Si can be applied as a reliable local reference in both structures to compare the changes in Volta potential differences as the result of different heat treatments of aluminium brazing sheet. Increasing the copper content of the re-solidified clad material as a result of brazing treatment was found to increase the Volta potential of the matrix which in turn reduces the cathodic protection power of the re-solidified clad material towards the core material

High resolution scanning optical imaging of a frozen planar polymer light-emitting electrochemical cell: an experimental and modelling study

Institute of Scientific and Technical Information of China (English)

Faleh AlTal; Jun Gao

2017-01-01

Light-emitting electrochemical cells (LECs) are organic photonic devices based on a mixed electronic and ionic conductor.The active layer of a polymer-based LEC consists of a luminescent polymer,an ion-solvating/transport polymer,and a compatible salt.The LEC p-n or p-i-n junction is ultimately responsible for the LEC performance.The LEC junction,however,is still poorly understood due to the difficulties of characterizing a dynamic-junction LEC.In this paper,we present an experimental and modeling study of the LEC junction using scanning optical imaging techniques.Planar LECs with an interelectrode spacing of 560 μm have been fabricated,activated,frozen and scanned using a focused laser beam.The optical-beam-induced-current (OBIC) and photoluminescence (PL) data have been recorded as a function of beam location.The OBIC profile has been simulated in COMSOL that allowed for the determination of the doping concentration and the depletion width of the LEC junction.

High resolution scanning optical imaging of a frozen planar polymer light-emitting electrochemical cell:an experimental and modelling study

Institute of Scientific and Technical Information of China (English)

Faleh AlTal; Jun Gao

2017-01-01

Light-emitting electrochemical cells(LECs) are organic photonic devices based on a mixed electronic and ionic conductor.The active layer of a polymer-based LEC consists of a luminescent polymer,an ion-solvating/transport polymer,and a compatible salt.The LEC p-n or p-i-n junction is ultimately responsible for the LEC performance.The LEC junction,however,is still poorly understood due to the difficulties of characterizing a dynamic-junction LEC.In this paper,we present an experimental and modeling study of the LEC junction using scanning optical imaging techniques.Planar LECs with an interelectrode spacing of 560μm have been fabricated,activated,frozen and scanned using a focused laser beam.The optical-beam-induced-current(OBIC)and photoluminescence(PL) data have been recorded as a function of beam location.The OBIC profile has been simulated in COMSOL that allowed for the determination of the doping concentration and the depletion width of the LEC junction.

Results from a Novel Method for Corrosion Studies of Electroplated Lithium Metal Based on Measurements with an Impedance Scanning Electrochemical Quartz Crystal Microbalance

Directory of Open Access Journals (Sweden)

Martin Winter

2013-07-01

Full Text Available A new approach to study the chemical stability of electrodeposited lithium on a copper metal substrate via measurements with a fast impedance scanning electrochemical quartz crystal microbalance is presented. The corrosion of electrochemically deposited lithium was compared in two different electrolytes, based on lithium difluoro(oxalato borate (LiDFOB and lithium hexafluorophosphate, both salts being dissolved in solvent blends of ethylene carbonate and diethyl carbonate. For a better understanding of the corrosion mechanisms, scanning electron microscopy images of electrodeposited lithium were also consulted. The results of the EQCM experiments were supported by AC impedance measurements and clearly showed two different corrosion mechanisms caused by the different salts and the formed SEIs. The observed mass decrease of the quartz sensor of the LiDFOB-based electrolyte is not smooth, but rather composed of a series of abrupt mass fluctuations in contrast to that of the lithium hexafluorophosphate-based electrolyte. After each slow decrease of mass a rather fast increase of mass is observed several times. The slow mass decrease can be attributed to a consolidation process of the SEI or to the partial dissolution of the SEI leaving finally lithium metal unprotected so that a fast film formation sets in entailing the observed fast mass increases.

Functionalization of single-walled carbon nanotubes with protein by click chemistry as sensing platform for sensitized electrochemical immunoassay

International Nuclear Information System (INIS)

Qi Honglan; Ling Chen; Huang Ru; Qiu Xiaoying; Shangguan Li; Gao Qiang; Zhang Chengxiao

2012-01-01

Highlights: ► Single-walled carbon nanotubes were functionalized with protein by click chemistry. ► The SWNTs conjugated with protein showed excellent dispersion in water and kept good bioacitvity. ► A competitive electrochemical immunoassay for the determination of anti-IgG was developed with high sensitivity and good stability. - Abstract: The application of the Cu(I)-catalyzed [3 + 2] Huisgen cycloaddition to the functionalization of single-walled carbon nanotubes (SWNTs) with the protein and the use of the artificial SWNTs as a sensing platform for sensitive immunoassay were reported. Covalent functionalization of azide decorated SWNTs with alkyne modified protein was firstly accomplished by the Cu(I)-catalyzed [3 + 2] Huisgen cycloaddition. FT-IR spectroscopy, Raman spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscopy and transmission electron micrograph were used to characterize the protein-functionalized SWNTs. It was found that the SWNTs conjugated with the proteins showed excellent dispersion in water and kept good bioacitivity when immunoglobulin (IgG) and horseradish peroxidase (HRP) were chosen as model proteins. As a proof-of-concept, IgG-functionalized SWNTs were immobilized onto the surface of a glassy carbon electrode by simple casting method as immunosensing platform and a sensitive competitive electrochemical immunoassay was developed for the determination of anti-immunoglobulin (anti-IgG) using HRP as enzyme label. The fabrication of the immunosensor were characterized by cyclic voltammetry and electrochemical impedance spectroscopy with the redox probe [Fe(CN) 6 ] 3−/4− . The SWNTs as immobilization platform showed better sensitizing effect, a detection limit of 30 pg mL −1 (S/N = 3) was obtained for anti-IgG. The proposed strategy provided a stable immobilization method and sensitized recognition platform for analytes. This work demonstrated that the click coupling of SWNTs with protein was an effective

Refined tip preparation by electrochemical etching and ultrahigh vacuum treatment to obtain atomically sharp tips for scanning tunneling microscope and atomic force microscope

International Nuclear Information System (INIS)

Hagedorn, Till; Ouali, Mehdi El; Paul, William; Oliver, David; Miyahara, Yoichi; Gruetter, Peter

2011-01-01

A modification of the common electrochemical etching setup is presented. The described method reproducibly yields sharp tungsten tips for usage in the scanning tunneling microscope and tuning fork atomic force microscope. In situ treatment under ultrahigh vacuum (p ≤10 -10 mbar) conditions for cleaning and fine sharpening with minimal blunting is described. The structure of the microscopic apex of these tips is atomically resolved with field ion microscopy and cross checked with field emission.

Preparation and characterization of porphyrin-polythiophene stacked films as prepared by electrochemical method under stirring condition

International Nuclear Information System (INIS)

Sugawa, Kosuke; Akiyama, Tsuyoshi; Yamada, Sunao

2008-01-01

Porphyrin-polythiophene (pTh) stacked films consisting of meso-tetrathienylporphyrin (TThP) and bithiophene (BiTh) were prepared on transparent indium-tin-oxide (ITO) electrodes by sequential electrochemical scanning of applied potential between 0 and + 2 V vs Ag wire in the electrolyte solution of BiTh and TThP under stirring condition. First, the pTh films were prepared by electrochemical polymerization and then TThP was incorporated into the as-prepared pTh film by subsequent electrochemical scanning as described above in the TThP solution. The operation of solution stirring during electrochemical scanning achieved the formation of robust stacked films. UV/Vis and fluorescence spectra confirmed that the amount of TThP moiety increased with increasing the number of electrochemical scanning cycles in the TThP solution. In order to evaluate the incorporation profile of TThP, surface analyses and depth profiles of stacked films were carried out by XPS spectroscopy. The results suggested that all films formed porphyrin-polythiophene stacked structure precisely, and that TThP was exclusively incorporated around the outermost region of the pTh film

Electrochemical characterization of praseodymia doped zircon. Catalytic effect on the electrochemical reduction of molecular oxygen in polar organic solvents

Energy Technology Data Exchange (ETDEWEB)

Domenech, Antonio, E-mail: antonio.domenech@uv.es [Departament de Quimica Analitica, Universitat de Valencia, Dr. Moliner, 50, 46100 Burjassot, Valencia (Spain); Montoya, Noemi; Alarcon, Javier [Departament de Quimica Inorganica, Universitat de Valencia, Dr. Moliner, 50, 46100 Burjassot, Valencia (Spain)

2011-08-01

Highlights: > Electrochemical characterization of Pr centers in praseodymia-doped zircon. > Study of the catalytic effect on the reduction of peroxide radical anion in nonaqueous solvents. > Assessment of non-uniform distribution of Pr centers in the zircon grains. - Abstract: The voltammetry of microparticles and scanning electrochemical microscopy methodologies are applied to characterize praseodymium centers in praseodymia-doped zircon (Pr{sub x}Zr{sub (1-y)}Si{sub (1-z)}O{sub 4}; y + z = x; 0.02 < x < 0.10) specimens prepared via sol-gel synthetic routes. In contact with aqueous electrolytes, two overlapping Pr-centered cathodic processes, attributable to the Pr (IV) to Pr (III) reduction of Pr centers in different sites are obtained. In water-containing, air-saturated acetone and DMSO solutions as solvent, Pr{sub x}Zr{sub (1-y)}Si{sub (1-z)}O{sub 4} materials produce a significant catalytic effect on the electrochemical reduction of peroxide radical anion electrochemically generated. These electrochemical features denote that most of the Pr centers are originally in its 4+ oxidation state in the parent Pr{sub x}Zr{sub (1-y)}Si{sub (1-z)}O{sub 4} specimens. The variation of the catalytic performance of such specimens with potential scan rate, water concentration and Pr loading suggests that Pr is not uniformly distributed within the zircon grains, being concentrated in the outer region of such grains.

Force modulation and electrochemical gating of conductance in a cytochrome

Science.gov (United States)

Davis, Jason J.; Peters, Ben; Xi, Wang

2008-09-01

Scanning probe methods have been used to measure the effect of electrochemical potential and applied force on the tunnelling conductance of the redox metalloprotein yeast iso-1-cytochrome c (YCC) at a molecular level. The interaction of a proximal probe with any sample under test will, at this scale, be inherently perturbative. This is demonstrated with conductive probe atomic force microscopy (CP-AFM) current-voltage spectroscopy in which YCC, chemically adsorbed onto pristine Au(111) via its surface cysteine residue, is observed to become increasingly compressed as applied load is increased, with concomitant decrease in junction resistance. Electrical contact at minimal perturbation, where probe-molecule coupling is comparable to that in scanning tunnelling microscopy, brings with it the observation of negative differential resistance, assigned to redox-assisted probe-substrate tunnelling. The role of the redox centre in conductance is also resolved in electrochemical scanning tunnelling microscopy assays where molecular conductance is electrochemically gateable through more than an order of magnitude.

Intermittent Contact Alternating Current Scanning Electrochemical Microscopy: A Method for Mapping Conductivities in Solid Li Ion Conducting Electrolyte Samples

Energy Technology Data Exchange (ETDEWEB)

Catarelli, Samantha Raisa; Lonsdale, Daniel [Uniscan Instruments Ltd., Macclesfield (United Kingdom); Cheng, Lei [Energy Storage and Distribution Resources Division, Lawrence Berkeley National Laboratory, Berkeley, CA (United States); Materials Sciences and Engineering Department, University of California Berkeley, Berkeley, CA (United States); Syzdek, Jaroslaw [Bio-Logic USA LLC, Knoxville, TN (United States); Doeff, Marca, E-mail: mmdoeff@lbl.gov [Energy Storage and Distribution Resources Division, Lawrence Berkeley National Laboratory, Berkeley, CA (United States)

2016-03-31

Intermittent contact alternating current scanning electrochemical microscopy (ic-ac-SECM) has been used to determine the electrochemical response to an ac signal of several types of materials. A conductive gold foil and insulating Teflon sheet were first used to demonstrate that the intermittent contact function allows the topography and conductivity to be mapped simultaneously and independently in a single experiment. Then, a dense pellet of an electronically insulating but Li ion conducting garnet phase, Al-substituted Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} (LLZO), was characterized using the same technique. The polycrystalline pellet was prepared by classical ceramic sintering techniques and was comprised of large (~150 μm) grains. Critical information regarding the contributions of grain and grain boundary resistances to the total conductivity of the garnet phase was lacking due to ambiguities in the impedance data. In contrast, the use of the ic-ac-SECM technique allowed spatially resolved information regarding local conductivities to be measured directly. Impedance mapping of the pellet showed that the grain boundary resistance, while generally higher than that of grains, varied considerably, revealing the complex nature of the LLZO sample.

A new protocol for the distribution of MnO2 nanoparticles on rGO sheets and the resulting electrochemical performance

Science.gov (United States)

Samdani, Jitendra; Samdani, Kunda; Kim, Nam Hoon; Lee, Joong Hee

2017-03-01

Herein, reduced graphene oxide (rGO)/MnO2 hybrid materials were prepared via a direct redox reaction between MnCl2 and KMnO4 on reduced graphene oxide (rGO). A systematic study was carried out to understand the role of KMnO4. The morphology and microstructure of the as-prepared composite was characterized using field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Raman Spectroscopy. Results indicate that the concentrations of KMnO4 have a detrimental effect on the distribution of MnO2 nanoparticles on rGO sheets and hence on electrochemical properties. The electrochemical capacitive behavior of the as-prepared composite was investigated using cyclic voltammetry (CV), galvanostatic charge discharge, and electrochemical impedance spectroscopy (EIS) in 1 M Na2SO4 aqueous electrolyte solution. At the optimum concentration of KMnO4, the as-prepared rGM-1 composite shows a high specific capacitance of 366 F/g at a scan rate of 10 mV/s. The composite also exhibits good electrocatalytic activity towards the oxidation of dopamine (DA), exhibiting a low detection limit of 2.3 × 10-7 M with a wide linear range between 2.5 × 10-7 M and 2.30 × 10-4 M. Hence, the use of rGO/MnO2 at an optimized concentration of KMnO4 is a potential competitive candidate in supercapacitor and biosensor applications.

Fabrication and characterization of a nanometer-sized optical fiber electrode based on selective chemical etching for scanning electrochemical/optical microscopy.

Science.gov (United States)

Maruyama, Kenichi; Ohkawa, Hiroyuki; Ogawa, Sho; Ueda, Akio; Niwa, Osamu; Suzuki, Koji

2006-03-15

We have already reported a method for fabricating ultramicroelectrodes (Suzuki, K. JP Patent, 2004-45394, 2004). This method is based on the selective chemical etching of optical fibers. In this work, we undertake a detailed investigation involving a combination of etched optical fibers with various types of tapered tip (protruding-shape, double- (or pencil-) shape and triple-tapered electrode) and insulation with electrophoretic paint. Our goal is to establish a method for fabricating nanometer-sized optical fiber electrodes with high reproducibility. As a result, we realized pencil-shaped and triple-tapered electrodes that had radii in the nanometer range with high reproducibility. These nanometer-sized electrodes showed well-defined sigmoidal curves and stable diffusion-limited responses with cyclic voltammetry. The pencil-shaped optical fiber, which has a conical tip with a cone angle of 20 degrees , was effective for controlling the electrode radius. The pencil-shaped electrodes had higher reproducibility and smaller electrode radii (r(app) etched optical fiber electrodes. By using a pencil-shaped electrode with a 105-nm radius as a probe, we obtained simultaneous electrochemical and optical images of an implantable interdigitated array electrode. We achieved nanometer-scale resolution with a combination of scanning electrochemical microscopy SECM and optical microscopy. The resolution of the electrochemical and optical images indicated sizes of 300 and 930 nm, respectively. The neurites of living PC12 cells were also successfully imaged on a 1.6-microm scale by using the negative feedback mode of an SECM.

Micropatterning on cylindrical surfaces via electrochemical etching using laser masking

International Nuclear Information System (INIS)

Cho, Chull Hee; Shin, Hong Shik; Chu, Chong Nam

2014-01-01

Highlights: • Various micropatterns were fabricated on the cylindrical surface of a stainless steel shaft. • Selective electrochemical dissolution was achieved via a series process of laser masking and electrochemical etching. • Laser masking characteristics on the non-planar surface were investigated. • A uniform mask layer was formed on the cylindrical surface via synchronized laser line scanning with a rotary system. • The characteristics of electrochemical etching on the non-planar surface were investigated. - Abstract: This paper proposes a method of selective electrochemical dissolution on the cylindrical surfaces of stainless steel shafts. Selective electrochemical dissolution was achieved via electrochemical etching using laser masking. A micropatterned recast layer was formed on the surface via ytterbium-doped pulsed fiber laser irradiation. The micropatterned recast layer could be used as a mask layer during the electrochemical etching process. Laser masking condition to form adequate mask layer on the planar surface for etching cannot be used directly on the non-planar surface. Laser masking condition changes depending on the morphological surface. The laser masking characteristics were investigated in order to form a uniform mask layer on the cylindrical surface. To minimize factors causing non-uniformity in the mask layer on the cylindrical surface, synchronized laser line scanning with a rotary system was applied during the laser masking process. Electrochemical etching characteristics were also investigated to achieve deeper etched depth, without collapsing the recast layer. Consequently, through a series process of laser masking and electrochemical etching, various micropatternings were successfully performed on the cylindrical surfaces

Selective electrochemical gold deposition onto p-Si (1 0 0) surfaces

Energy Technology Data Exchange (ETDEWEB)

Santinacci, L; Etcheberry, A [Institut Lavoisier de Versailles (UMR CNRS 8180), University of Versailles-Saint-Quentin, 45 avenue des Etats-Unis, F-78035 Versailles cedex (France); Djenizian, T [Laboratoire Chimie Provence (UMR CNRS 6264), University of Aix-Marseille I-II-III, Centre Saint-Jerome, F-13397 Marseille Cedex 20 (France); Schwaller, P [Laboratory for Mechanics of Materials and Nanostructures, Swiss Federal Laboratory for Materials Testing and Research, Feuerwerkstr. 39, CH-3602 Thun (Switzerland); Suter, T [Laboratory for Corrosion and Materials Integrity, Swiss Federal Laboratory for Materials Testing and Research, Ueberlandstr. 129, CH-8600 Duebendorf (Switzerland); Schmuki, P [Department of Materials Science, LKO-WW4, Friedrich-Alexander-University Erlangen-Nuremberg, Martensstr. 7, D-91058 Erlangen (Germany)], E-mail: lionel.santinacci@uvsq.fr

2008-09-07

In this paper, we report selective electrochemical gold deposition onto p-type Si (1 0 0) into nanoscratches produced through a thin oxide layer using an atomic force microscope. A detailed description of the substrate engraving process is presented. The influence of the main scratching parameters such as the normal applied force, the number of scans and the scanning velocity are investigated as well as the mechanical properties of the substrate. Gold deposition is carried out in a KAu(CN){sub 2} + KCN solution by applying cathodic voltages for various durations. The gold deposition process is investigated by cyclic voltammetry. Reactivity enhancement at the scratched locations was studied by comparing the electrochemical behaviour of intact and engraved surfaces using a micro-electrochemical setup. Selective electrochemical gold deposition is achieved: metallic patterns with a sub-500 nm lateral resolution are obtained demonstrating, therefore, the bearing potential of this patterning technique.

Refined tip preparation by electrochemical etching and ultrahigh vacuum treatment to obtain atomically sharp tips for scanning tunneling microscope and atomic force microscope.

Science.gov (United States)

Hagedorn, Till; El Ouali, Mehdi; Paul, William; Oliver, David; Miyahara, Yoichi; Grütter, Peter

2011-11-01

A modification of the common electrochemical etching setup is presented. The described method reproducibly yields sharp tungsten tips for usage in the scanning tunneling microscope and tuning fork atomic force microscope. In situ treatment under ultrahigh vacuum (p ≤10(-10) mbar) conditions for cleaning and fine sharpening with minimal blunting is described. The structure of the microscopic apex of these tips is atomically resolved with field ion microscopy and cross checked with field emission. © 2011 American Institute of Physics

A study on the initiation of pitting corrosion in carbon steel in chloride-containing media using scanning electrochemical probes

International Nuclear Information System (INIS)

Lin Bin; Hu Ronggang; Ye Chenqing; Li Yan; Lin Changjian

2010-01-01

Scanning electrochemical probes of corrosion potential and chloride ions were developed for the in situ monitoring of localized corrosion processes of reinforcing steel in NaCl-containing solution. The results indicated that the chloride ions (Cl - ) preferentially adsorbed and accumulated at the imperfect/defective sites, resulting in initiation and propagation of pitting corrosion on the reinforcing steel surface. An electron microprobe analyzer (EMPA) was used to examine the corrosion morphology and elemental distribution at the corroded location to investigate the origins of the preferential Cl - adsorption and pitting corrosion. By combining the in situ and ex situ images, we concluded that manganese sulfide inclusions in reinforcing steel are the most susceptible defects to pitting corrosion in chloride-containing solution.

Chemical Production of Graphene Catalysts for Electrochemical Energy Conversion

DEFF Research Database (Denmark)

Seselj, Nedjeljko

by scanning tunneling microscopy (STM), to investigate the nature of L-cysteine bonds on Au. Synthesized electrocatalysts were characterized by spectroscopic, microscopic and electrochemical techniques. Electrocatalysis was examined by electrochemical oxidation of formic acid, methanol and ethanol, and oxygen......Recently developed FC technology is among many approaches aiming at solving the global energy challenges. FCs are electrochemical devices that convert chemical energy from fuel molecules into electrical energy via electrochemical reactions. FCs are, however, limited by the scarce and expensive...... was achieved via L-cysteine linker molecules that provided pathways for fast electron transfers during the electrocatalytic reactions. Electrochemical properties of selfassembled L-cysteine monolayers immobilized on single-crystal Au(111) surfaces were studied in ionic liquids and their structures imaged...

Simultaneous noncontact topography and electrochemical imaging by SECM/SICM featuring ion current feedback regulation.

Science.gov (United States)

Takahashi, Yasufumi; Shevchuk, Andrew I; Novak, Pavel; Murakami, Yumi; Shiku, Hitoshi; Korchev, Yuri E; Matsue, Tomokazu

2010-07-28

We described a hybrid system of scanning electrochemical microscopy (SECM) and scanning ion conductance microscopy (SICM) with ion current feedback nanopositioning control for simultaneous imaging of noncontact topography and spatial distribution of electrochemical species. A nanopipette/nanoring electrode probe provided submicrometer resolution of the electrochemical measurement on surfaces with complex topology. The SECM/SICM probe had an aperture radius of 220 nm. The inner and outer radii of the SECM Au nanoring electrode were 330 and 550 nm, respectively. Characterization of the probe was performed with scanning electron microscopy (SEM), cyclic voltammetry (CV), and approach curve measurements. SECM/SICM was applied to simultaneous imaging of topography and electrochemical responses of enzymes (horse radish peroxidase (HRP) and glucose oxidase (GOD)) and single live cells (A6 cells, superior cervical ganglion (SCG) cells, and cardiac myocytes). The measurements revealed the distribution of activity of the enzyme spots on uneven surfaces with submicrometer resolution. SECM/SICM acquired high resolution topographic images of cells together with the map of electrochemical signals. This combined technique was also applied to the evaluation of the permeation property of electroactive species through cellular membranes.

Localization of proteins in paint cross-sections by scanning electrochemical microscopy as an alternative immunochemical detection technique

Energy Technology Data Exchange (ETDEWEB)

Sciutto, Giorgia; Prati, Silvia [Microchemistry and Microscopy Art Diagnostic Laboratory, University of Bologna, Via Guaccimanni 42, Ravenna 48121 (Italy); Department of Chemistry “G. Ciamician”, University of Bologna, Via Selmi, Bologna 2 40126 (Italy); Mazzeo, Rocco, E-mail: rocco.mazzeo@unibo.it [Microchemistry and Microscopy Art Diagnostic Laboratory, University of Bologna, Via Guaccimanni 42, Ravenna 48121 (Italy); Department of Chemistry “G. Ciamician”, University of Bologna, Via Selmi, Bologna 2 40126 (Italy); Zangheri, Martina; Roda, Aldo; Bardini, Luca; Valenti, Giovanni; Rapino, Stefania [Department of Chemistry “G. Ciamician”, University of Bologna, Via Selmi, Bologna 2 40126 (Italy); Marcaccio, Massimo, E-mail: massimo.marcaccio@unibo.it [Department of Chemistry “G. Ciamician”, University of Bologna, Via Selmi, Bologna 2 40126 (Italy)

2014-06-01

Highlights: • Advanced immuno-electrochemical detection of proteins in paint samples by SECM. • Analysis performed directly on cross-section with high spatial resolution. • Identification of HRP catalytic activity for a selective location of analyte. • Satisfactory results were obtained for aged real samples. • The way forward for an extensive application of SECM in conservation science is shown. - Abstract: The qualitative identification of proteinaceous substances, as well as their location within a complex paint stratigraphy, is one of the most challenging issues in the characterization of painting materials. Nevertheless, information on paint components represent a crucial task for studies concerning both the ancient painting techniques adopted and the state of conservation, being fundamental investigations for the selection of appropriate conservation actions. The present research was aimed at developing a new detection approach for the immunochemical localization of ovalbumin in paint cross-sections based on the use of scanning electrochemical microscopy (SECM). The immunochemical analyses were performed using an anti-ovalbumin primary antibody and a secondary antibody labelled with horseradish peroxidase (HRP). SECM measurements were performed in feedback mode using benzoquinone (BQ)/hydroquinone (H{sub 2}Q) redox couple. In presence of hydrogen peroxide (H{sub 2}O{sub 2}), HRP catalyzes the re-oxidation of H{sub 2}Q to BQ and the increment of BQ concentration in correspondence of the target protein was detected by SECM through the electrochemical reduction of the regenerated BQ at the microelectrode. Indeed, the localization of ovalbumin was possible thanks to a clear discrimination of SECM currents, achieved by the comparison of the measurements recorded before and after H{sub 2}O{sub 2} administration, based on the HRP on/off approach. The method was evaluated both on samples from standard mocks-up and on a historical sample, collected from a

Electrochemical stability of subnanometer Pt clusters

DEFF Research Database (Denmark)

Quinson, Jonathan; Röefzaad, Melanie; Deiana, Davide

2018-01-01

In the present work, the degradation of size-selected Pt nanoclusters is studied under electrochemical conditions. This model catalyst mimics carbon supported Pt nanoclusters and nanoparticles typically employed in proton exchange membrane fuel cells (PEMFCs). Insight into the early stage...... of degradation is given by high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) and confirmed by transmission electron microscopy (TEM). In contrast to common assumptions, it is demonstrated that even extremely small Pt clusters exhibit a remarkable stability under electrochemical...... - is observed. In light of the findings reported, developing highly-dispersed subnanometer Pt clusters as catalyst for PEMFCs is a realistic approach provided the operation conditions are suitably adjusted. Furthermore, mitigation strategies to improve the stability of few-atoms catalyst under electrochemical...

Electrochemical properties of double wall carbon nanotube electrodes

OpenAIRE

Pumera, Martin

2007-01-01

AbstractElectrochemical properties of double wall carbon nanotubes (DWNT) were assessed and compared to their single wall (SWNT) counterparts. The double and single wall carbon nanotube materials were characterized by Raman spectroscopy, scanning and transmission electron microscopy and electrochemistry. The electrochemical behavior of DWNT film electrodes was characterized by using cyclic voltammetry of ferricyanide and NADH. It is shown that while both DWNT and SWNT were significantly funct...

Well-ordered structure of methylene blue monolayers on Au(111) surface: electrochemical scanning tunneling microscopy studies.

Science.gov (United States)

Song, Yonghai; Wang, Li

2009-02-01

Well-ordered structure of methylene blue (MB) monolayers on Au(111) surface has been successfully obtained by controlling the substrate potential. Electrochemical scanning tunneling microscopy (ECSTM) examined the monolayers of MB on Au(111) in 0.1 M HClO(4) and showed long-range ordered, interweaved arrays of MB with quadratic symmetry on the substrate in the potential range of double-layer charging. High-resolution ECSTM image further revealed the details of the MB monolayers structure of c(5 x 5 radical 3)rect and the flat-lying orientation of ad-molecules. The dependence of molecular organization on the substrate potential and the formation mechanism of well-ordered structure on Au(111) surface were investigated in detail. The obtained well-ordered structure at the interface between a metal and an aqueous electrolyte might possibly be used as high-density device for signal memory and templates for the advanced nanopatterning of surfaces. (c) 2008 Wiley-Liss, Inc.

Non-destructive Patterning of Carbon Electrodes by Using the Direct Mode of Scanning Electrochemical Microscopy.

Science.gov (United States)

Stratmann, Lutz; Clausmeyer, Jan; Schuhmann, Wolfgang

2015-11-16

Patterning of glassy carbon surfaces grafted with a layer of nitrophenyl moieties was achieved by using the direct mode of scanning electrochemical microscopy (SECM) to locally reduce the nitro groups to hydroxylamine and amino functionalities. SECM and atomic force microscopy (AFM) revealed that potentiostatic pulses applied to the working electrode lead to local destruction of the glassy carbon surface, most likely caused by etchants generated at the positioned SECM tip used as the counter electrode. By applying galvanostatic pulses, and thus, limiting the current during structuring, corrosion of the carbon surface was substantially suppressed. After galvanostatic patterning, unambiguous proof of the formation of the anticipated amino moieties was possible by modulation of the pH value during the feedback mode of SECM imaging. This patterning strategy is suitable for the further bio-modification of microstructured surfaces. Alkaline phosphatase, as a model enzyme, was locally bound to the modified areas, thus showing that the technique can be used for the development of protein microarrays. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Multifunctional scanning ion conductance microscopy

Science.gov (United States)

Page, Ashley; Unwin, Patrick R.

2017-01-01

Scanning ion conductance microscopy (SICM) is a nanopipette-based technique that has traditionally been used to image topography or to deliver species to an interface, particularly in a biological setting. This article highlights the recent blossoming of SICM into a technique with a much greater diversity of applications and capability that can be used either standalone, with advanced control (potential–time) functions, or in tandem with other methods. SICM can be used to elucidate functional information about interfaces, such as surface charge density or electrochemical activity (ion fluxes). Using a multi-barrel probe format, SICM-related techniques can be employed to deposit nanoscale three-dimensional structures and further functionality is realized when SICM is combined with scanning electrochemical microscopy (SECM), with simultaneous measurements from a single probe opening up considerable prospects for multifunctional imaging. SICM studies are greatly enhanced by finite-element method modelling for quantitative treatment of issues such as resolution, surface charge and (tip) geometry effects. SICM is particularly applicable to the study of living systems, notably single cells, although applications extend to materials characterization and to new methods of printing and nanofabrication. A more thorough understanding of the electrochemical principles and properties of SICM provides a foundation for significant applications of SICM in electrochemistry and interfacial science. PMID:28484332

Electrochemical behavior of pitch-based activated carbon fibers for electrochemical capacitors

International Nuclear Information System (INIS)

Lee, Hye-Min; Kwac, Lee-Ku; An, Kay-Hyeok; Park, Soo-Jin; Kim, Byung-Joo

2016-01-01

Highlights: • Electrode materials for electrochemical capacitors were developed using pitch-based activated carbon fibers with steam activation. • Activated carbon fibers showed enhanced specific surface area from 1520 to 3230 m 2 /g. • The increase in the specific capacitance of the samples was determined by charged pore structure during charging and discharging. - Abstract: In the present study, electrode materials for electrochemical capacitors were developed using pitch-based activated carbon fibers with steam activation. The surface and structural characteristics of activated carbon fibers were observed using scanning electron microscopy and X-ray diffraction, respectively. Pore characteristics were investigated using N 2 /77 K adsorption isotherms. The activated carbon fibers were applied as electrodes for electrical double-layer capacitors and analyzed in relation to the activation time. The specific surface area and total pore volume of the activated carbon fibers were determined to be 1520–3230 m 2 /g and 0.61–1.87 cm 3 /g, respectively. In addition, when the electrochemical characteristics were analyzed, the specific capacitance was confirmed to have increased from 1.1 F/g to 22.5 F/g. From these results, it is clear that the pore characteristics of pitch-based activated carbon fibers changed considerably in relation to steam activation and charge/discharge cycle; therefore, it was possible to improve the electrochemical characteristics of the activated carbon fibers.

Competitive effect of KOH activation on the electrochemical performances of carbon nanotubes for EDLC: Balance between porosity and conductivity

International Nuclear Information System (INIS)

Xu Bin; Wu Feng; Su Yuefeng; Cao Gaoping; Chen Shi; Zhou Zhiming; Yang Yusheng

2008-01-01

This work is focused on the competitive effects on the performance of the electric double layer capacitors (EDLCs) between porosity increase and simultaneous conductivity decrease for KOH-activated carbon nanotubes (CNTs). A series of the CNTs have been activated with KOH to enhance their surface areas for application in EDLCs. The microstructure of the activated carbon nanotubes (ACNTs) is characterized with N 2 adsorption, transmission electron microscopy (TEM) observation and electric conductivity measurement. Their electrochemical performances are evaluated in aqueous KOH electrolyte with galvanostatic charge/discharge, cyclic voltammetry, and ac impedance spectroscopy. It is found that the KOH activation enhances the specific surface area of the CNTs and its specific capacitance but decreases its electric conductivity and the rate performance in EDLC. By controlling the activation of the CNTs to balance the porosity and conductivity, ACNTs with both high capacitance and good rate performance are obtained

Electrochemical impedance spectroscopy of oxidized porous silicon

Energy Technology Data Exchange (ETDEWEB)

Mula, Guido, E-mail: guido.mula@unica.it [Dipartimento di Fisica, Università degli Studi di Cagliari, Cittadella Universitaria di Monserrato, S.P. 8 km 0.700, 09042 Cagliari (Italy); Tiddia, Maria V. [Dipartimento di Fisica, Università degli Studi di Cagliari, Cittadella Universitaria di Monserrato, S.P. 8 km 0.700, 09042 Cagliari (Italy); Ruffilli, Roberta [Nanochemistry, Istituto Italiano di Tecnologia, Via Morego 30, 16163 Genova (Italy); Falqui, Andrea [Nanochemistry, Istituto Italiano di Tecnologia, Via Morego 30, 16163 Genova (Italy); Dipartimento di Scienze Chimiche e Geologiche, Università degli Studi di Cagliari, Cittadella Universitaria di Monserrato, S.P. 8 km 0.700, 09042 Cagliari (Italy); Palmas, Simonetta; Mascia, Michele [Dipartimento di Ingegneria Meccanica Chimica e dei Materiali, Università degli Studi di Cagliari, Piazza d' Armi, 09126 Cagliari (Italy)

2014-04-01

We present a study of the electrochemical oxidation process of porous silicon. We analyze the effect of the layer thickness (1.25–22 μm) and of the applied current density (1.1–11.1 mA/cm{sup 2}, values calculated with reference to the external samples surface) on the oxidation process by comparing the galvanostatic electrochemical impedance spectroscopy (EIS) measurements and the optical specular reflectivity of the samples. The results of EIS were interpreted using an equivalent circuit to separate the contribution of different sample parts. A different behavior of the electrochemical oxidation process has been found for thin and thick samples: whereas for thin samples the oxidation process is univocally related to current density and thickness, for thicker samples this is no more true. Measurements by Energy Dispersive Spectroscopy using a Scanning Electron Microscopy confirmed that the inhomogeneity of the electrochemical oxidation process is increased by higher thicknesses and higher currents. A possible explanation is proposed to justify the different behavior of thin and thick samples during the electrochemical process. - Highlights: • A multidisciplinary approach on porous Si electrochemical oxidation is proposed. • Electrochemical, optical, and structural characterizations are used. • Layer thickness and oxidation current effects are shown. • An explanation of the observed behavior is proposed.

Microstructures and electrochemical behaviors of the friction stir welding dissimilar weld.

Science.gov (United States)

Shen, Changbin; Zhang, Jiayan; Ge, Jiping

2011-06-01

By using optical microscope, the microstructures of 5083/6082 friction stir welding (FSW) weld and parent materials were analyzed. Meanwhile, at ambient temperature and in 0.2 mol/L NaHS03 and 0.6 mol/L NaCl solutionby gravimetric test, potentiodynamic polarization curve test, electrochemical impedance spectra (EIS) and scanning electron microscope (SEM) observation, the electrochemical behavior of 5083/6082 friction stir welding weld and parent materials were comparatively investigated by gravimetric test, potentiodynamic polarization curve test, electrochemical impedance spectra (EIS) and scanning electron microscope (SEM) observation. The results indicated that at given processing parameters, the anti-corrosion property of the dissimilar weld was superior to those of the 5083 and 6082 parent materials. Copyright © 2011 The Research Centre for Eco-Environmental Sciences, Chinese Academy of Sciences. Published by Elsevier B.V. All rights reserved.

Electrochemical capacitor behavior of copper sulfide (CuS) nanoplatelets

Energy Technology Data Exchange (ETDEWEB)

Justin Raj, C.; Kim, Byung Chul; Cho, Won-Je; Lee, Won-Gil; Seo, Yongseong; Yu, Kook-Hyun, E-mail: yukook@dongguk.edu

2014-02-15

Highlights: • The electrochemical supercapacitor electrode was fabricated using CuS nanoplatelets. • CuS electrodes shows better electrochemical properties in aqueous LiClO{sub 4} electrolyte. • The heat treated CuS electrode shows an excellent pseudocapacitance performance than bare CuS electrode. -- Abstract: Copper sulfide (CuS) nanoplatelets have been fabricated by simple low temperature chemical bath deposition technique for electrochemical supercapacitor electrodes. The morphology and structural properties of the electrodes were analyzed using scanning electron microscopy and X-ray diffraction. The effect of heat treatment on electrochemical properties of CuS electrodes were examined by cyclic voltammetry, electrochemical impedance spectroscopy and galvanostatic charge/discharge tests. Results show that bare and heat treated CuS has pseudocapacitive characteristic within the potential range of −0.6 to 0.3 V (vs. Ag/AgCl) in aqueous 1 M LiClO{sub 4} solution. The pseudocapacitance is induced mainly by lithium ions insertion/extraction with the CuS electrodes. The specific capacitance of 72.85 F g{sup −1} was delivered by heat treated CuS film at a scan rate of 5 mV s{sup −1} with an energy and power density of 6.23 W h kg{sup −1} and 1.75 kW kg{sup −1} at 3 Ag{sup −1} constant discharge current which is comparatively higher than that of as deposited CuS electrode.

Optimization of the use of carbon paste electrodes (CPE for electrochemical study of the chalcopyrite

Directory of Open Access Journals (Sweden)

Daniela G. Horta

2009-01-01

Full Text Available The use of carbon paste electrodes (CPE of mineral sulfides can be useful for electrochemical studies to overcome problems by using massive ones. Using CPE-chalcopyrite some variables were electrochemically evaluated. These variables were: (i the atmosphere of preparation (air or argon of CPE and elapsed time till its use; (ii scan rate for voltammetric measurements and (iii chalcopyrite concentration in the CPE. Based on cyclic voltammetry, open-circuit potential and electrochemical impedance results the recommendations are: oxygen-free atmosphere to prepare and kept the CPE until around two ours, scan rates from 10 to 40 mV s-1, and chalcopyrite concentrations > 20%.

Respiration activity of Escherichia coli entrapped in a cone-shaped microwell and cylindrical micropore monitored by scanning electrochemical microscopy (SECM).

Science.gov (United States)

Kaya, Takatoshi; Numai, Daisuke; Nagamine, Kuniaki; Aoyagi, Shigeo; Shiku, Hitoshi; Matsue, Tomokazu

2004-06-01

The metabolic activity of E. coli cells embedded in collagen gel microstructures in a cone-shaped well and in a cylindrical micropore was investigated using scanning electrochemical microscopy (SECM), based on the oxygen consumption rate and the conversion rate from ferrocyanide to ferricyanide. The analysis of the concentration profiles for oxygen and ferrocyanide afforded the oxygen consumption rate and the ferrocyanide production rate. A comparison indicated that the ferrocyanide production rates were larger than the oxygen consumption rate, and also that the rates observed in the cylindrical micropore were larger than those observed in the cone-shaped well. The ferrocyanide production rate of a single E. coli cell was calculated to be (5.4 +/- 2.6) x 10(-19) mol s(-1), using a cylindrical micropore system.

Preparation of Chemically Etched Tips for Ambient Instructional Scanning Tunneling Microscopy

Science.gov (United States)

Zaccardi, Margot J.; Winkelmann, Kurt; Olson, Joel A.

2010-01-01

A first-year laboratory experiment that utilizes concepts of electrochemical tip etching for scanning tunneling microscopy (STM) is described. This experiment can be used in conjunction with any STM experiment. Students electrochemically etch gold STM tips using a time-efficient method, which can then be used in an instructional grade STM that…

The electrochemical interface of Ag(111) in 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ionic liquid—A combined in-situ scanning probe microscopy and impedance study

International Nuclear Information System (INIS)

Li, Mian-Gang; Chen, Li; Zhong, Yun-Xin; Chen, Zhao-Bin; Yan, Jia-Wei; Mao, Bing-Wei

2016-01-01

The electrochemical interface between Ag(111) and 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide (EMITFSI) has been investigated by in-situ scanning probe microscopy (SPM) and electrochemical impedance spectroscopy (EIS). In-situ scanning tunneling microscopy (STM) characterization has revealed that there is neither surface reconstruction nor strong adsorption of EMITFSI on Ag(111) surface so that EIS investigation can be fulfilled under well-defined surface condition and in the absence of pseudo capacitive process. In-situ atom force microscopy (AFM) force curve measurements further disclose that there exists five layered structures near and normal to the surface, among them three layered structures being charged and forming the electric double layer (EDL) of the interface. An electric equivalent circuit is proposed, which comprises two serial parallel branches involving the innermost layered structure and the next two layered structures in the EDL, respectively. The inner layer circuit is given by a constant phase element (CPE) in parallel to a resistor, while the outer layer circuit is given by a capacity in parallel with a resistor-Warburg element branch. Slow response is observed for the inner layer, which is attributed to the hindrance of reorientation and/or redistribution of ions in the more ordered and robust inner layer region. The inner layer capacitance and outer layer capacitance have opposing potential dependence, and the resultant double layer capacitance shows weak potential dependence.

Investigation the effect of porosity on corrosion of macroporous silicon in 1.0 M sodium hydroxide solution using weight loss measurements, electrochemical methods and scanning electron microscope

International Nuclear Information System (INIS)

Lai, Chuan; Xiang, Zhen

2015-01-01

Highlights: • The dissolution of silicon wafers conforms Faraday’s laws of electrolysis. • The porosity effect on macroporous silicon corrosion was investigated. • The corrosion rate increase linearly with porosity increasing. • The porosity effect on activation parameters was obtained. - Abstract: In this study, the macroporous silicon has been fabricated by electrochemical anodization. The dissolution of n-type silicon wafers in etching solution conforms Faraday’s laws of electrolysis. The fabricated macroporous silicon with different porosity corrosion in 1.0 M NaOH was systemically investigated by weight loss measurements, electrochemical methods and scanning electron microscope. Results show that with the porosity increasing, the corrosion rate of macroporous silicon in 1.0 M NaOH increases linearly. In addition, the increase of corrosion rate of macroporous silicon with relative higher porosity was determined by the pre-exponential factor.

One-pot hydrothermal synthesis, characterization and electrochemical properties of CuS nanoparticles towards supercapacitor applications

International Nuclear Information System (INIS)

Krishnamoorthy, Karthikeyan; Rao, Alluri Nagamalleswara; Jae Kim, Sang; Kumar Veerasubramani, Ganesh

2014-01-01

In this article, we have investigated the electrochemical properties of CuS nanoparticles for supercapacitor applications. The CuS nanoparticles are prepared by a facile one-pot hydrothermal approach using copper nitrate and thiourea as starting materials. The x-ray diffraction study revealed the formation of covellite CuS. The field-emission scanning electron microscope studies suggested the formation of cubic shaped CuS nanoparticles. The electrochemical studies such as cyclic voltammetry, galvanostatic charge-discharge analysis and electrochemical impedance spectroscopy confirmed the pseudocapacitive nature of the CuS electrodes. The CuS electrode shows a specific capacitance of about 101.34 F g −1 from the cyclic voltammetry at a scan rate of 5 mV s −1 . The electrochemical impedance spectra analyzed using Nyquist plot confirmed the pseudocapacitive behavior of the CuS electrodes. (paper)

Carbon nanotubes modified with antimony nanoparticles: A novel material for electrochemical sensing

International Nuclear Information System (INIS)

Moraes, Fernando C.; Cesarino, Ivana; Cesarino, Vivian; Mascaro, Lucia H.; Machado, Sergio A.S.

2012-01-01

Highlights: ► A novel material for the electrochemical sensing was developed. ► Sensor based CNTs modified with Sb-nanoparticles was characterised and applied. ► The proposed sensor was suitable and sensitive for the determination of bisphenol A. - Abstract: In this study, a novel material for the electrochemical determination of bisphenol A using a nanocomposite based on multi-walled carbon nanotubes modified with antimony nanoparticles has been investigated. The morphology, structure, and electrochemical performance of the nanocomposite electrodes were characterised by field emission gun scanning electron microscopy, energy-dispersive X-ray spectroscopy, and cyclic voltammetry. A scan rate study and electrochemical impedance spectroscopy showed that the bisphenol A oxidation product is adsorbed on nanocomposite electrode surface. Differential pulse voltammetry in phosphate buffer solution at pH 6, allowed the development of a method to determine bisphenol A levels in the range of 0.5–5.0 μmol L −1 , with a detection limit of 5.24 nmol L −1 (1.19 μg L −1 ).

Electrochemical Corrosion of Stainless Steel in Thiosulfate Solutions Relevant to Gold Leaching

Science.gov (United States)

Choudhary, Lokesh; Wang, Wei; Alfantazi, Akram

2016-01-01

This study aims to characterize the electrochemical corrosion behavior of stainless steel in the ammoniacal thiosulfate gold leaching solutions. Electrochemical corrosion response was investigated using potentiodynamic polarization and electrochemical impedance spectroscopy, while the semi-conductive properties and the chemical composition of the surface film were characterized using Mott-Schottky analysis and X-ray photoelectron spectroscopy, respectively. The morphology of the corroded specimens was analyzed using scanning electron microscopy. The stainless steel 316L showed no signs of pitting in the ammoniacal thiosulfate solutions.

Membrane Separated Flow Cell for Parallelized Electrochemical Impedance Spectroscopy and Confocal Laser Scanning Microscopy to Characterize Electro-Active Microorganisms

International Nuclear Information System (INIS)

Stöckl, Markus; Schlegel, Christin; Sydow, Anne; Holtmann, Dirk; Ulber, Roland; Mangold, Klaus-Michael

2016-01-01

Highlights: • Development of a membrane separated electrochemical flow cell. • Simultaneous combination of EIS and CLSM. • Monitoring of bacterial cell attachment to anode of MFC. • Cell attachment of Shewanella oneidensis is shown. - Abstract: Understanding the attachment of electro-active bacteria to electrode surfaces and their subsequent biofilm formation is one of the major challenges for the establishment of bacterial bioelectrochemial systems (BES). For a constant observation of biofilm growth, providing information on different stages of biofilm formation, continuous monitoring methods are required. In this paper a combination of two powerful analytical methods, Electrochemical Impedance Spectroscopy (EIS) and Confocal Laser Scanning Microscopy (CLSM), for biofilm monitoring is presented. A custom-built flow cell with a transparent indium tin oxide working electrode (WE) was constructed allowing monitoring of cell attachment to a working electrode simultaneously by EIS and CLSM. Cyclic Voltammetry (CV) and EIS of an iron (II)/iron (III) redox couple indicate that the flow cell is suitable for electrochemical experiments. An engineered Shewanella oneidensis MR-1 (ATCC700550) producing eGFP was used as electro-active model organism to demonstrate the practical application of the flow cell as BES to monitor cell attachment simultaneously with EIS and CLSM. Applying the flow cell as MFC (transparent working electrode poised as anode) produced a typical current curve for such a system. From the equivalent circuit used to interpret EIS data the charge transfer resistance R CT is sensitive to attachment of microorganisms. Fitted R CT was increased initially after cell inoculation and then lowered constantly with progressing experimental time. In parallel taken CLSM images show that bacteria already adhered to the WE 5 min after inoculation. A mono- respectively bilayer of electro-active cells was observed after 17 h on the WE surface. With the presented

Electrochemical migration of tin in electronics and microstructure of the dendrites

DEFF Research Database (Denmark)

Minzari, Daniel; Grumsen, Flemming Bjerg; Jellesen, Morten Stendahl

2011-01-01

The macro-, micro-, and nano-scale morphology and structure of tin dendrites, formed by electrochemical migration on a surface mount ceramic chip resistor having electrodes consisting of tin with small amounts of Pb (∼2wt.%) was investigated by scanning electron microscopy and transmission electr...... by the dehydration of the hydrated oxide originally formed in solution ex-situ in ambient air.......The macro-, micro-, and nano-scale morphology and structure of tin dendrites, formed by electrochemical migration on a surface mount ceramic chip resistor having electrodes consisting of tin with small amounts of Pb (∼2wt.%) was investigated by scanning electron microscopy and transmission electron...... microscopy including Energy dispersive X-ray spectroscopy and electron diffraction. The tin dendrites were formed under 5 or 12V potential bias in 10ppm by weight NaCl electrolyte as a micro-droplet on the resistor during electrochemical migration experiments. The dendrites formed were found to have...

Oxygen-free in situ scanning tunnelling microscopy

DEFF Research Database (Denmark)

Zhang, Jingdong; Ulstrup, Jens

2007-01-01

Scanning tunneling microscopy under full electrochemical potential control (in situ STM) has been used extensively as an efficient method to characterize microstructures at solid/liquid interfaces at the atomic and molecular levels. However, under ambient conditions oxygen may interfere in open i...

FABRICATION AND CHARACTERIZATION OF POLYANILINE-GRAPHENE COMPOSITE AS ELECTRODE IN ELECTROCHEMICAL CAPACITOR

Directory of Open Access Journals (Sweden)

H. Adelkhani

2016-06-01

Full Text Available In this study, polyaniline-graphene composites with different nano-structures are synthesized and the behaviour of the obtained composites serving as electrode materials in electrochemical capacitors is studied. The morphology, crystal structure, and thermal stability of the composites are examined using scanning electron microscopy (SEM, X-ray diffraction (XRD, and Thermal gravimetric analysis (TGA. Electrochemical properties are characterized by cyclic voltammetry (CV. According to the results, the obtained composites show different crystal structures and different thermal stabilities, and consequently different electrochemical capacities, when used as electrodes in electrochemical capacitors. A nano-fibre composite is shown to have a good degree of crystallization, 5.17% water content, 637oC degradation onset temperature, and 379 Fg-1 electrochemical capacity.

Single-Molecule Electrochemical Gating in Ionic Liquids

DEFF Research Database (Denmark)

Kay, Nicola J.; Higgins, Simon J.; Jeppesen, Jan O.

2012-01-01

The single-molecular conductance of a redox active molecular bridge has been studied in an electrochemical single-molecule transistor configuration in a room-temperature ionic liquid (RTIL). The redox active pyrrolo-tetrathiafulvalene (pTTF) moiety was attached to gold contacts at both ends through...... −(CH2)6S– groups, and gating of the redox state was achieved with the electrochemical potential. The water-free, room-temperature, ionic liquid environment enabled both the monocationic and the previously inaccessible dicationic redox states of the pTTF moiety to be studied in the in situ scanning...... and decreases again as the second redox process is passed. This is described as an “off–on–off–on–off” conductance switching behavior. This molecular conductance vs electrochemical potential relation could be modeled well as a sequential two-step charge transfer process with full or partial vibrational...

Scanning electrochemical microscopy. 47. Imaging electrocatalytic activity for oxygen reduction in an acidic medium by the tip generation-substrate collection mode.

Science.gov (United States)

Fernández, José L; Bard, Allen J

2003-07-01

The oxygen reduction reaction (ORR) in acidic medium was studied on different electrode materials by scanning electrochemical microscopy (SECM) operating in a new variation of the tip generation-substrate collection mode. An ultramicroelectrode tip placed close to the substrate electrode oxidizes water to oxygen at a constant current. The substrate is held at a potential where the tip-generated oxygen is reduced and the resulting substrate current is measured. By changing the substrate potential, it is possible to obtain a polarization (current-potential) curve, which depends on the electrocatalytic activity of the substrate material. The main difference between this mode and the classical feedback SECM mode of operation is that the feedback diffusion process is not required for the measurement, allowing its application for studying the ORR in acidic solutions. Activity-sensitive images of heterogeneous surfaces, e.g., with Pt and Au electrodes, were obtained from the substrate current when the x-y plane was scanned with the tip. The usefulness of this technique for imaging electrocatalytic activity of smooth metallic electrodes and of highly dispersed fuel cell-type electrocatalysts was demonstrated. The application of this method to the combinatorial chemical analysis of electrode materials and electrocatalysts is discussed.

A new protocol for the distribution of MnO2 nanoparticles on rGO sheets and the resulting electrochemical performance

International Nuclear Information System (INIS)

Samdani, Jitendra; Samdani, Kunda; Kim, Nam Hoon; Lee, Joong Hee

2017-01-01

Highlights: • The role of KMnO 4 for the deposition of MnO 2 on rGO was studied. • The as-synthesized rGM-1 shows good stability and a high specific capacitance value (366 F/g). • rGM-1 effectively detects dopamine with a detection limit of 2.3 × 10 −7 M. - Abstract: Herein, reduced graphene oxide (rGO)/MnO 2 hybrid materials were prepared via a direct redox reaction between MnCl 2 and KMnO 4 on reduced graphene oxide (rGO) . A systematic study was carried out to understand the role of KMnO 4 . The morphology and microstructure of the as-prepared composite was characterized using field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Raman Spectroscopy. Results indicate that the concentrations of KMnO 4 have a detrimental effect on the distribution of MnO 2 nanoparticles on rGO sheets and hence on electrochemical properties. The electrochemical capacitive behavior of the as-prepared composite was investigated using cyclic voltammetry (CV), galvanostatic charge discharge, and electrochemical impedance spectroscopy (EIS) in 1 M Na 2 SO 4 aqueous electrolyte solution. At the optimum concentration of KMnO 4 , the as-prepared rGM-1 composite shows a high specific capacitance of 366 F/g at a scan rate of 10 mV/s. The composite also exhibits good electrocatalytic activity towards the oxidation of dopamine (DA), exhibiting a low detection limit of 2.3 × 10 −7 M with a wide linear range between 2.5 × 10 −7 M and 2.30 × 10 −4 M. Hence, the use of rGO/MnO 2 at an optimized concentration of KMnO 4 is a potential competitive candidate in supercapacitor and biosensor applications.

In situ monitoring of the electrochemical dissolution of tungsten

Energy Technology Data Exchange (ETDEWEB)

Krebsz, Melinda [Christian Doppler Laboratory for Combinatorial Oxide Chemistry at ICTAS, Johannes Kepler University Linz (Austria); Kollender, Jan Philipp [Institute for Chemical Technology of Inorganic Materials (ICTAS), Johannes Kepler University Linz (Austria); Hassel, Achim Walter [Christian Doppler Laboratory for Combinatorial Oxide Chemistry at ICTAS, Johannes Kepler University Linz (Austria); Institute for Chemical Technology of Inorganic Materials (ICTAS), Johannes Kepler University Linz (Austria)

2017-09-15

In the present work, which is aimed to monitor in situ the electrochemical dissolution of tungsten by using a Flow-Type Scanning Droplet Cell Microscope (FT-SDCM) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS), novel results are reported. The anodic oxide growth and its dissolution on the surface of W have been monitored in situ. The results of this current study show the importance of coupling electrochemical experiments to ICP-MS. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Electrochemical preparation of poly(methylene blue)/graphene nanocomposite thin films

International Nuclear Information System (INIS)

Erçarıkcı, Elif; Dağcı, Kader; Topçu, Ezgi; Alanyalıoğlu, Murat

2014-01-01

Highlights: • Poly(MB)/graphene thin films are prepared by a simple electrochemical approach. • Graphene layers in the film show a broad band in visible region of absorbance spectra. • Morphology of composite films indicates both disordered and ordered regions. • XRD reveals that nanocomposite films include rGO layers after electropolymerization process. • Chemically prepared graphene is better than electrochemically prepared graphene for electrooxidation of nitrite. - Abstract: Poly(methylene blue)/graphene nanocomposite thin films were prepared by electropolymerization of methylene blue in the presence of graphene which have been synthesized by two different methods of a chemical oxidation process and an electrochemical approach. Synthesized nanocomposite thin films were characterized by using cyclic voltammetry, UV–vis. absorption spectroscopy, powder X-ray diffraction, and scanning tunneling microscopy techniques. Electrocatalytical properties of prepared poly(methylene blue)/graphene nanocomposite films were compared toward electrochemical oxidation of nitrite. Under optimized conditions, electrocatalytical effect of nanocomposite films of chemically prepared graphene through electrochemical oxidation of nitrite was better than that of electrochemically prepared graphene

Prospecção e monitoramento informacional no processo de inteligência competitiva Information scanning and information mining in the process of competitive intelligence

Directory of Open Access Journals (Sweden)

Marta Lígia Pomim Valentim

2004-01-01

Full Text Available A prospecção e o monitoramento informacional são atividades base para a inteligência competitiva, entendida como um processo dinâmico, composto pela gestão da informação e pela gestão do conhecimento. O processo de inteligência competitiva (I. C. nas organizações ocorre a partir de diferentes atividades informacionais, dentre elas estão as ligadas a prospecção e ao monitoramento. O papel destas atividades é essencial, pois alimentam todo o processo com dados, informação e conhecimento, constroem diversas estruturas formais e informais de informação dentro da organização, além do que, as atividades de prospecção e monitoramento geram serviços e produtos informacionais sistematizados, com alto valor agregado.The information scanning and information mining are activities base for the competitive intelligence, understood as a dynamic process, composed by the information management and knowledge management. The process of competitive intelligence (I. C. in the organizations it happens starting from different informational activities, they are the tied up ones information scanning and information mining. The function of these activities is essential, because they feed the whole process with data, information and knowledge, they build several formal structures and you inform inside of information of the organization, in addition, the information scanning and information mining activities generate information services and products systematized, with high value aggregate.

Facile preparation of polypyrrole/graphene oxide nanocomposites with large areal capacitance using electrochemical codeposition for supercapacitors

Science.gov (United States)

Zhou, Haihan; Han, Gaoyi; Xiao, Yaoming; Chang, Yunzhen; Zhai, Hua-Jin

2014-10-01

A simple and low-cost electrochemical codeposition method has been introduced to fabricate polypyrrole/graphene oxide (PPy/GO) nanocomposites and the areal capacitance of conducting polymer/GO composites is reported for the first time. Fourier transform infrared spectroscopy (FTIR), Transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and X-ray diffraction (XRD) are implemented to determine the PPy/GO nanocomposites are successfully prepared and the interaction between PPy and GO. The as-prepared PPy/GO nanocomposites show the curly sheet-like morphology, superior capacitive behaviors and cyclic stability. Furthermore, the varying deposition time is implemented to investigate the impact of the loading amount on electrochemical behavior of the composites, and a high areal capacitance of 152 mF cm-2 is achieved at 10 mV s-1 CV scan. However, the thicker films caused by the long deposition time would result in larger diffusion resistance of electrolyte ions, consequently exhibit the relatively lower capacitance value at the high current density. The GCD tests indicate moderate deposition time is more suitable for the fast charge/discharge. Considering the very simple and effective synthetic process, the PPy/GO nanocomposites with relatively high areal capacitance are competitive candidate for supercapacitor application, and its capacitive performances can be easily tuned by varying the deposition time.

Pulse electrochemical meso/micro/nano ultraprecision machining technology.

Science.gov (United States)

Lee, Jeong Min; Kim, Young Bin; Park, Jeong Woo

2013-11-01

This study demonstrated meso/micro/nano-ultraprecision machining through electrochemical reactions using intermittent DC pulses. The experiment focused on two machining methods: (1) pulse electrochemical polishing (PECP) of stainless steel, and (2) pulse electrochemical nano-patterning (PECNP) on a silicon (Si) surface, using atomic force microscopy (AFM) for fabrication. The dissolution reaction at the stainless steel surface following PECP produced a very clean, smooth workpiece. The advantages of the PECP process included improvements in corrosion resistance, deburring of the sample surface, and removal of hydrogen from the stainless steel surface as verified by time-of-flight secondary-ion mass spectrometry (TOF-SIMS). In PECNP, the electrochemical reaction generated within water molecules produced nanoscale oxide textures on a Si surface. Scanning probe microscopy (SPM) was used to evaluate nanoscale-pattern processing on a Si wafer surface produced by AFM-PECNP For both processes using pulse electrochemical reactions, three-dimensional (3-D) measurements and AFM were used to investigate the changes on the machined surfaces. Preliminary results indicated the potential for advancing surface polishing techniques and localized micro/nano-texturing technology using PECP and PECNP processes.

Influence of graphene microstructures on electrochemical performance for supercapacitors

Directory of Open Access Journals (Sweden)

Youning Gong

2015-10-01

Full Text Available The influence of variant graphenes on electrochemical performance for supercapacitors was studied comparatively and systematically by using SEM, FTIR and Raman spectroscopy, cyclic voltammetry (CV, galvanostatic charge/discharge and electrochemical impedance spectroscopy (EIS. The results revealed that: 1 the nitrogen-doped graphene (N-G electrode exhibited the highest specific capacitance at the same voltage scan rate; 2 the specific capacitance of the N-G reached up to 243.5 F/g at 1 A/g, while regular graphite oxide (GO was 43.5 F/g and reduced graphene oxide (rGO was 67.9 F/g; 3 N-G exhibited the best supercapacitance performance and the superior electrochemical properties, which made it an ideal electrode material for supercapacitors.

Carbons, ionic liquids and quinones for electrochemical capacitors

Directory of Open Access Journals (Sweden)

Raul eDiaz

2016-04-01

Full Text Available Carbons are the main electrode materials used in electrochemical capacitors, which are electrochemical energy storage devices with high power densities and long cycling lifetimes. However, increasing their energy density will improve their potential for commercial implementation. In this regard, the use of high surface area carbons and high voltage electrolytes are well known strategies to increase the attainable energy density, and lately ionic liquids have been explored as promising alternatives to current state of the art acetonitrile-based electrolytes. Also, in terms of safety and sustainability ionic liquids are attractive electrolyte materials for electrochemical capacitors. In addition, it has been shown that the matching of the carbon pore size with the electrolyte ion size further increases the attainable electric double layer (EDL capacitance and energy density.The use of pseudocapacitive reactions can significantly increase the attainable energy density, and quinonic-based materials offer a potentially sustainable and cost effective research avenue for both the electrode and the electrolyte. This perspective will provide an overview of the current state of the art research on electrochemical capacitors based on combinations of carbons, ionic liquids and quinonic compounds, highlighting performances and challenges and discussing possible future research avenues. In this regard, current interest is mainly focused on strategies which may ultimately lead to commercially competitive sustainable high performance electrochemical capacitors for different applications including those requiring mechanical flexibility and biocompatibility.

Single-Molecule Electrochemical Transistor Utilizing a Nickel-Pyridyl Spinterface

DEFF Research Database (Denmark)

Brooke, Richard J.; Jin, Chengjun; Szumski, Doug S.

2015-01-01

Using a scanning tunnelling microscope break-junction technique, we produce 4,4′-bipyridine (44BP) single-molecule junctions with Ni and Au contacts. Electrochemical control is used to prevent Ni oxidation and to modulate the conductance of the devices via nonredox gating - the first time this has...... been shown using non-Au contacts. Remarkably the conductance and gain of the resulting Ni-44BP-Ni electrochemical transistors is significantly higher than analogous Au-based devices. Ab-initio calculations reveal that this behavior arises because charge transport is mediated by spin-polarized Ni d...

Determining Li+-Coupled Redox Targeting Reaction Kinetics of Battery Materials with Scanning Electrochemical Microscopy.

Science.gov (United States)

Yan, Ruiting; Ghilane, Jalal; Phuah, Kia Chai; Pham Truong, Thuan Nguyen; Adams, Stefan; Randriamahazaka, Hyacinthe; Wang, Qing

2018-02-01

The redox targeting reaction of Li + -storage materials with redox mediators is the key process in redox flow lithium batteries, a promising technology for next-generation large-scale energy storage. The kinetics of the Li + -coupled heterogeneous charge transfer between the energy storage material and redox mediator dictates the performance of the device, while as a new type of charge transfer process it has been rarely studied. Here, scanning electrochemical microscopy (SECM) was employed for the first time to determine the interfacial charge transfer kinetics of LiFePO 4 /FePO 4 upon delithiation and lithiation by a pair of redox shuttle molecules FcBr 2 + and Fc. The effective rate constant k eff was determined to be around 3.70-6.57 × 10 -3 cm/s for the two-way pseudo-first-order reactions, which feature a linear dependence on the composition of LiFePO 4 , validating the kinetic process of interfacial charge transfer rather than bulk solid diffusion. In addition, in conjunction with chronoamperometry measurement, the SECM study disproves the conventional "shrinking-core" model for the delithiation of LiFePO 4 and presents an intriguing way of probing the phase boundary propagations induced by interfacial redox reactions. This study demonstrates a reliable method for the kinetics of redox targeting reactions, and the results provide useful guidance for the optimization of redox targeting systems for large-scale energy storage.

Multifunctional Graphene-based Hybrid Nanomaterials for Electrochemical Energy Storage.

Science.gov (United States)

Gupta, Sanju

Intense research in renewable energy is stimulated by global demand of electric energy. Electrochemical energy storage and conversion systems namely, supercapacitors and batteries, represent the most efficient and environmentally benign technologies. Moreover, controlled nanoscaled architectures and surface chemistry of electrochemical electrodes is enabling emergent next-generation efficient devices approaching theoretical limit of energy and power densities. This talk will present our recent activities to advance design, development and deployment of composition, morphology and microstructure controlled two- and three-dimensional graphene-based hybrids architectures. They are chemically and molecularly bridged with carbon nanotubes, conducting polymers, transition metal oxides and mesoproprous silicon wrapped with graphene nanosheets as engineered electrodes for supercapacitor cathodes and battery anodes. They showed significant enhancement in terms of gravimetric specific capacitance, interfacial capacitance, charging-discharging rate and cyclability. We will also present fundamental physical-chemical interfacial processes (ion transfer kinetics and diffusion), imaging electroactive sites, and topography at electrode/electrolyte interface governing underlying electrochemical mechanisms via scanning electrochemical microscopy. KY NSF EPSCoR.

Synthesis and electrochemical properties of tin oxide-based composite by rheological technique

International Nuclear Information System (INIS)

He Zeqiang; Li Xinhai; Xiong Lizhi; Wu Xianming; Xiao Zhuobing; Ma Mingyou

2005-01-01

Novel rheological technique was developed to synthesize tin oxide-based composites. The microstructure, morphology, and electrochemical performance of the materials were investigated by X-ray diffraction, scanning electron microscopy and electrochemical methods. The particles of tin oxide-based materials form an inactive matrix. The average size of the particles is about 150 nm. The material delivers a charge capacity of more than 570 mAh g -1 . The capacity loss per cycle is about 0.15% after being cycled 30 times. The good electrochemical performance indicates that this kind of tin oxide-based material is promising anode for lithium-ion battery

Electrochemical copolymerization of thiophene derivatives; a precursor to photovoltaic devices

International Nuclear Information System (INIS)

Kumar, Prajwal; Ranjith, K.; Gupta, Satyajit; Ramamurthy, Praveen C.

2011-01-01

Highlights: → This work presents an electrochemical technique for the polymerization and copolymerization of thiophene derivatives. → Copolymerization of thiophene based monomers like 7,9-dithiophene-2yl-8H-cyclopenta[a]acenaphthalene-8-one and 3-hexylthiophene are synthesized. → Study of the structural, optical, thermal, conductivity, morphological, band gap and impedance measurements of the copolymer indicates a suitable material for photovoltaic applications. - Abstract: This work presents an electrochemical technique for the polymerization and copolymerization of thiophene derivatives like 7,9-dithiophene-2yl-8H-cyclopenta[a]acenaphthalene-8-one and 3-hexylthiophene. The structural characterization of chemically synthesized monomers and electrochemically synthesized polymers was carried out by nuclear magnetic resonance and Fourier transform infrared spectroscopy. Thermal characterizations indicate that copolymer has increased thermal stability than that of homopolymer. Morphological studies of the polymerized films carried out by scanning electron microscopy shows network structure of copolymer. Optical properties of the homopolymers and copolymer were studied by UV-visible spectrometer and it was observed that band gap of copolymer is less than the homopolymers. HOMO and LUMO levels, band gap values of the respective polymers were also calculated from the cyclic voltammetry technique with various scan rates. By the peak current obtained from various scan rates shows that all polymerization reactions are diffusion controlled process. Charge transfer resistances of polymers were determined using Nyquist plots. Conductivity of synthesized polymers shows higher conductivity for copolymer than homopolymers.

Efficient electrochemical degradation of multiwall carbon nanotubes.

Science.gov (United States)

Reipa, Vytas; Hanna, Shannon K; Urbas, Aaron; Sander, Lane; Elliott, John; Conny, Joseph; Petersen, Elijah J

2018-07-15

As the production mass of multiwall carbon nanotubes (MWCNT) increases, the potential for human and environmental exposure to MWCNTs may also increase. We have shown that exposing an aqueous suspension of pristine MWCNTs to an intense oxidative treatment in an electrochemical reactor, equipped with an efficient hydroxyl radical generating Boron Doped Diamond (BDD) anode, leads to their almost complete mineralization. Thermal optical transmittance analysis showed a total carbon mass loss of over two orders of magnitude due to the electrochemical treatment, a result consistent with measurements of the degraded MWCNT suspensions using UV-vis absorbance. Liquid chromatography data excludes substantial accumulation of the low molecular weight reaction products. Therefore, up to 99% of the initially suspended MWCNT mass is completely mineralized into gaseous products such as CO 2 and volatile organic carbon. Scanning electron microscopy (SEM) images show sporadic opaque carbon clusters suggesting the remaining nanotubes are transformed into structure-less carbon during their electrochemical mineralization. Environmental toxicity of pristine and degraded MWCNTs was assessed using Caenorhabditis elegans nematodes and revealed a major reduction in the MWCNT toxicity after treatment in the electrochemical flow-by reactor. Published by Elsevier B.V.

Scanning electrochemical microscopy for the fabrication of copper nanowires: Atomic contacts with quantized conductance, and molecular adsorption effect

International Nuclear Information System (INIS)

Janin, Marion; Ghilane, Jalal; Lacroix, Jean-Christophe

2012-01-01

Highlights: ► Electrochemistry and SECM to generate copper nanowires with quantized conductance. ► Stable atomic contacts lasting for several hundreds of seconds have been obtained. ► The quantized conductances are independent of the tip and gap size. ► The method allows contacts to be generated in the presence of chosen molecules. ► Four-electrode configuration opens the route to redox gated atomic contact. - Abstract: Scanning electrochemical microscopy, SECM, is proposed as a tool for the fabrication of copper nanowires. In a first step, configuration based on two electrodes, a platinum UME (cathode) and a copper substrate (anode), operating in the SECM configuration was employed. For nanowires generated in water the conductance changes stepwise and varies by integer values of the conductance quantum G 0 . The formation of atomic contacts is supported by the ohmic behavior of the I–V curve. It depends neither on the UME tip radius nor on the initial gap size between tip and substrate. Atomic contacts generated in aqueous solutions of sodium dodecyl sulfate (SDS) below the critical micellar concentration (CMC) have conductances below 1G 0 attributed to molecular adsorption on the contact. In some cases, the nanowires have low conductance, 0.01G 0 . The corresponding I–V curve shows tunneling rather than ohmic behavior, suggesting that molecular junctions are formed with a few surfactant molecules trapped between the two electrodes. Finally, copper nanowires with quantized conductance have been generated using the SECM operating in a four-electrode setup. Thanks to the reference electrode, this configuration leads to better control of the potential of each working electrode; this setup will make it possible to evaluate the conductance variation and/or modulation upon electrochemical stimuli.

Use of Local Electrochemical Methods (SECM, EC-STM) and AFM to Differentiate Microstructural Effects (EBSD) on Very Pure Copper

Energy Technology Data Exchange (ETDEWEB)

Martinez-Lombardia, Esther; Graeve, Iris De; Terryn, Herman [Vrije Universiteit Brussel, Brussels (Belgium); Lapeire, Linsey; Verbeken, Kim; Kestens, Leo [Ghent University, Zwijnaarde (Ghent) (Belgium); Maurice, Vincent; Klein, Lorena; Marcus, Philippe [Institut de Recherche de Chimie Paris, Paris (France); Gonzalez-Garcia, Yaiza; Mol, Arjan [Delft University of Technology, Delft (Netherlands)

2017-02-15

When aiming for an increased and more sustainable use of metals a thorough knowledge of the corrosion phenomenon as function of the local metal microstructure is of crucial importance. In this work, we summarize the information presented in our previous publications and present an overview of the different local (electrochemical) techniques that have been proven to be effective in studying the relation between different microstructural variables and their different electrochemical behavior. Atomic force microscopy (AFM), scanning electrochemical microscopy (SECM), and electrochemical scanning tunneling microscopy (EC-STM) were used in combination with electron backscatter diffraction (EBSD). Consequently, correlations could be identified between the grain orientation and grain boundary characteristics, on the one hand, and the electrochemical behavior on the other hand. The grain orientation itself has an influence on the corrosion, and the orientation of the neighboring grains also seems to play a decisive role in the dissolution rate. With respect to intergranular corrosion, only coherent twin boundaries seem to be resistant.

The possibility of multi-layer nanofabrication via atomic force microscope-based pulse electrochemical nanopatterning

Science.gov (United States)

Kim, Uk Su; Morita, Noboru; Lee, Deug Woo; Jun, Martin; Park, Jeong Woo

2017-05-01

Pulse electrochemical nanopatterning, a non-contact scanning probe lithography process using ultrashort voltage pulses, is based primarily on an electrochemical machining process using localized electrochemical oxidation between a sharp tool tip and the sample surface. In this study, nanoscale oxide patterns were formed on silicon Si (100) wafer surfaces via electrochemical surface nanopatterning, by supplying external pulsed currents through non-contact atomic force microscopy. Nanoscale oxide width and height were controlled by modulating the applied pulse duration. Additionally, protruding nanoscale oxides were removed completely by simple chemical etching, showing a depressed pattern on the sample substrate surface. Nanoscale two-dimensional oxides, prepared by a localized electrochemical reaction, can be defined easily by controlling physical and electrical variables, before proceeding further to a layer-by-layer nanofabrication process.

Real-time monitoring of quorum sensing in 3D-printed bacterial aggregates using scanning electrochemical microscopy.

Science.gov (United States)

Connell, Jodi L; Kim, Jiyeon; Shear, Jason B; Bard, Allen J; Whiteley, Marvin

2014-12-23

Microbes frequently live in nature as small, densely packed aggregates containing ∼10(1)-10(5) cells. These aggregates not only display distinct phenotypes, including resistance to antibiotics, but also, serve as building blocks for larger biofilm communities. Aggregates within these larger communities display nonrandom spatial organization, and recent evidence indicates that this spatial organization is critical for fitness. Studying single aggregates as well as spatially organized aggregates remains challenging because of the technical difficulties associated with manipulating small populations. Micro-3D printing is a lithographic technique capable of creating aggregates in situ by printing protein-based walls around individual cells or small populations. This 3D-printing strategy can organize bacteria in complex arrangements to investigate how spatial and environmental parameters influence social behaviors. Here, we combined micro-3D printing and scanning electrochemical microscopy (SECM) to probe quorum sensing (QS)-mediated communication in the bacterium Pseudomonas aeruginosa. Our results reveal that QS-dependent behaviors are observed within aggregates as small as 500 cells; however, aggregates larger than 2,000 bacteria are required to stimulate QS in neighboring aggregates positioned 8 μm away. These studies provide a powerful system to analyze the impact of spatial organization and aggregate size on microbial behaviors.

Cyclic voltammetry and scanning electrochemical microscopy studies of methylene blue immobilized on the self-assembled monolayer of n-dodecanethiol

International Nuclear Information System (INIS)

Salamifar, Seyed Ehsan; Mehrgardi, Masoud Ayatollahi; Kazemi, Sayed Habib; Mousavi, Mir Fazllollah

2010-01-01

Electron transfer (ET) kinetics through n-dodecanethiol (C 12 SH) self-assembled monolayer on gold electrode was studied using cyclic voltammetry (CV), scanning electrochemical microscopy (SECM) and electrochemical impedance spectroscopy (EIS). An SECM model for compensating pinhole contribution, was used to measure the ET kinetics of solution-phase probes of ferrocyanide/ferricyanide (Fe(CN) 6 4-/3- ) and ferrocenemethanol/ferrociniummethanol (FMC 0/+ ) through the C 12 SH monolayer yielding standard tunneling rate constant (k ET 0 ) of (4 ± 1) x 10 -11 and (3 ± 1) x 10 -10 cm s -1 for Fe(CN) 6 4-/3- and FMC 0/+ respectively. Decay tunneling constants (β) of 0.97 and 0.96 A -1 for saturated alkane thiol chains were obtained using Fe(CN) 6 4- and FMC respectively. Also, it was found that methylene blue (MB) molecules are effectively immobilized on the C 12 SH monolayer and can mediate the ET between the solution-phase probes and underlying gold substrate. SECM-mediated model was used to simultaneously measure the bimolecular ET between the solution-phase probes and the monolayer-immobilized MB molecules, as well as tunneling ET between the monolayer-immobilized MB molecules and the underlying gold electrode, allowing the measurement of k BI = (5 ± 1) x 10 6 and (4 ± 2) x 10 7 cm 3 mol -1 s -1 for the bimolecular ET and k ET/MB 0 =(1±0.3)x10 -3 and (7 ± 3) x 10 -2 s -1 for the standard tunneling rate constant of ET using Fe(CN) 6 4-/3- and FMC 0/+ probes respectively.

Phase Competition Induced Bio-Electrochemical Resistance and Bio-Compatibility Effect in Nanocrystalline Zr x -Cu100-x Thin Films.

Science.gov (United States)

Badhirappan, Geetha Priyadarshini; Nallasivam, Vignesh; Varadarajan, Madhuri; Leobeemrao, Vasantha Priya; Bose, Sivakumar; Venugopal, Elakkiya; Rajendran, Selvakumar; Angleo, Peter Chrysologue

2018-07-01

Nano-crystalline Zrx-Cu100-x (x = 20-100 at.%) thin films with thickness ranging from 50 to 185 nm were deposited by magnetron co-sputtering with individual Zr and Cu targets. The as-sputtered thin films were characterized by Field Emission Scanning Electron Microscope (FE-SEM), Atomic Force Microscopy (AFM) and Glancing Incidence X-ray Diffraction (GIXRD) for structural and morphological properties. The crystallite size was found to decrease from 57 nm to 37 nm upon increasing the Zr content from 20 to 30 at.% with slight increase in the lattice strain from 0.17 to 0.33%. Further, increase in Zr content to 40 at.% leads to increase in the crystallite size to 57 nm due to stabilization of C10Zr7 phase along with the presence of nanocrystalline Cu-Zr phase. A bimodal distribution of grain size was observed from FE-SEM micrograph was attributed to the highest surface roughness in Zr30Cu70 thin films comprised of Cu10Zr7, Cu9Zr2, Cu-Zr intermetallic phases. In-vitro electrochemical behaviors of nano-crystalline Zrx-Cu100-x thin films in simulated body fluid (SBF) were investigated using potentiodynamic polarization studies. Electrochemical impedance spectroscopy (EIS) data fitting by equivalent electrical circuit fit model suggests that inner bulk layer contributes to high bio-corrosion resistance in Zrx-Cu100-x thin films with increase in Zr content. The results of cyto-compatibility assay suggested that Zr-Cu thin film did not introduce cytotoxicity to osteoblast cells, indicating its suitability as a bio-coating for minimally invasive medical devices.

In operando observation system for electrochemical reaction by soft X-ray absorption spectroscopy with potential modulation method

International Nuclear Information System (INIS)

Nagasaka, Masanari; Kosugi, Nobuhiro; Yuzawa, Hayato; Horigome, Toshio

2014-01-01

In order to investigate local structures of electrolytes in electrochemical reactions under the same scan rate as a typical value 100 mV/s in cyclic voltammetry (CV), we have developed an in operando observation system for electrochemical reactions by soft X-ray absorption spectroscopy (XAS) with a potential modulation method. XAS spectra of electrolytes are measured by using a transmission-type liquid flow cell with built-in electrodes. The electrode potential is swept with a scan rate of 100 mV/s at a fixed photon energy, and soft X-ray absorption coefficients at different potentials are measured at the same time. By repeating the potential modulation at each fixed photon energy, it is possible to measure XAS of electrochemical reaction at the same scan rate as in CV. We have demonstrated successful measurement of the Fe L-edge XAS spectra of aqueous iron sulfate solutions and of the change in valence of Fe ions at different potentials in the Fe redox reaction. The mechanism of these Fe redox processes is discussed by correlating the XAS results with those at different scan rates

Patterned electrochemical deposition of copper using an electron beam

Directory of Open Access Journals (Sweden)

Mark den Heijer

2014-02-01

Full Text Available We describe a technique for patterning clusters of metal using electrochemical deposition. By operating an electrochemical cell in the transmission electron microscope, we deposit Cu on Au under potentiostatic conditions. For acidified copper sulphate electrolytes, nucleation occurs uniformly over the electrode. However, when chloride ions are added there is a range of applied potentials over which nucleation occurs only in areas irradiated by the electron beam. By scanning the beam we control nucleation to form patterns of deposited copper. We discuss the mechanism for this effect in terms of electron beam-induced reactions with copper chloride, and consider possible applications.

In Situ Characterization of Ni and Ni/Fe Thin Film Electrodes for Oxygen Evolution in Alkaline Media by a Raman-Coupled Scanning Electrochemical Microscope Setup.

Science.gov (United States)

Steimecke, Matthias; Seiffarth, Gerda; Bron, Michael

2017-10-17

We present a spectroelectrochemical setup, in which Raman microscopy is combined with scanning electrochemical microscopy (SECM) in order to provide both spectroscopic and electrochemical information on the very same location of an electrode at the same time. The setup is applied to a subject of high academic and practical interest, namely, the oxygen evolution reaction at Ni and Ni/Fe electrodes. It comprises a transparent substrate electrode, onto which Ni and Ni/Fe thin films are deposited. An ultramicroelectrode (UME) is placed closely above the substrate to obtain electrochemical information, while a Raman microscope probes the same sample spot from below. To obtain information on oxygen evolution activity and structural changes, increasingly positive potentials from 0.1 up to 0.7 V vs Hg|HgO|1 M KOH were applied to the Ni/Fe-electrodes in 0.1 M KOH solution. Evolved oxygen is detected by reduction at a Pt UME, allowing for the determination of onset potentials, while the substrate current, which is recorded in parallel, is due to both overlapping oxygen evolution and the oxidation of Ni(OH) 2 to NiOOH. An optimum of 15% Fe in Ni/Fe films with respect to oxygen evolution activity was determined. At the same time, the potential-dependent formation of γ-NiOOH characterized by the Raman double band at 475 and 557 cm -1 allows for the conclusion that a certain amount of disorder introduced by Fe atoms is necessary to obtain high oxygen evolution reaction (OER) activity.

Optical and electrochemical studies of polyaniline/SnO2 fibrous nanocomposites

International Nuclear Information System (INIS)

Manivel, P.; Ramakrishnan, S.; Kothurkar, Nikhil K.; Balamurugan, A.; Ponpandian, N.; Mangalaraj, D.; Viswanathan, C.

2013-01-01

Graphical abstract: Fiber with porous like structure of PANI/SnO 2 nanocomposites were prepared by simplest in situ chemical polymerization method. The PL emission spectra revealed that the band from 404 and 436 nm which is related with oxygen vacancies. The excellent electrochemical properties of composite electrode show the specific capacitance of 173 F/g at a scan rate of 25 m V/s. Display Omitted Highlights: ► Self assembled PANI/SnO 2 nanocomposites were synthesized by simple polymerization method. ► Electrochemical behavior of PANI/SnO 2 nanocomposites electrode was analyzed by CV. ► Nanocomposites exhibit a higher specific capacitance of 173 F/g, compared with pure SnO 2 . -- Abstract: Polyaniline (PANI)/tin oxide (SnO 2 ) fibrous nanocomposites were successfully prepared by an in situ chemical polymerization method with suitable conditions. The obtained composites were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy, photoluminescence (PL), electrical conductivity and cyclic voltammetry studies (CV). The XRD pattern of the as-prepared sample shows the presence of tetragonal SnO 2 and the crystalline structure of SnO 2 was not affected with the incorporation of PANI. The FTIR analysis confirms the uniform attachment of PANI on the surface of SnO 2 nanostructures. SEM images show a fibrous agglomerated structure of PANI/SnO 2 . The PL emission spectra revealed that the band from 404 and 436 nm which is related with oxygen vacancies. The electrochemical behavior of the PANI/SnO 2 composite electrode was evaluated in a H 2 SO 4 solution using cyclic voltammetry. The composite electrode exhibited a specific capacitance of 173 F/g at a scan rate 25 mV/s. Thus the as-prepared PANI/SnO 2 composite shows excellent electrochemical properties, suggesting that this composite is a promising material for supercapacitors.

Advances and Perspectives in Chemical Imaging in Cellular Environments Using Electrochemical Methods

Directory of Open Access Journals (Sweden)

Robert A. Lazenby

2018-05-01

Full Text Available This review discusses a broad range of recent advances (2013–2017 in chemical imaging using electrochemical methods, with a particular focus on techniques that have been applied to study cellular processes, or techniques that show promise for use in this field in the future. Non-scanning techniques such as microelectrode arrays (MEAs offer high time-resolution (<10 ms imaging; however, at reduced spatial resolution. In contrast, scanning electrochemical probe microscopies (SEPMs offer higher spatial resolution (as low as a few nm per pixel imaging, with images collected typically over many minutes. Recent significant research efforts to improve the spatial resolution of SEPMs using nanoscale probes and to improve the temporal resolution using fast scanning have resulted in movie (multiple frame imaging with frame rates as low as a few seconds per image. Many SEPM techniques lack chemical specificity or have poor selectivity (defined by the choice of applied potential for redox-active species. This can be improved using multifunctional probes, ion-selective electrodes and tip-integrated biosensors, although additional effort may be required to preserve sensor performance after miniaturization of these probes. We discuss advances to the field of electrochemical imaging, and technological developments which are anticipated to extend the range of processes that can be studied. This includes imaging cellular processes with increased sensor selectivity and at much improved spatiotemporal resolution than has been previously customary.

Synthesis and electrochemical properties of MnO2 nanorods/graphene composites for supercapacitor applications

International Nuclear Information System (INIS)

Deng, SiXu; Sun, Dan; Wu, ChunHui; Wang, Hao; Liu, JingBing; Sun, YuXiu; Yan, Hui

2013-01-01

MnO 2 nanorods/graphene composite materials have been fabricated using a facile hydrothermal method for supercapacitor applications. The prepared composite materials are characterized by means of X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and transmission electron microscope (TEM). Electrochemical performances are evaluated using cyclic voltammetry (CV), galvanostatic charge–discharge and electrochemical impedance spectrometry (EIS). It indicates that ratio of MnO 2 nanorods to graphene in composite materials has significant influence on the electrochemical performance of composite electrodes. We have achieved the maximum specific capacitance of 218 F g −1 at the scan rate of 5 mV s −1 in 1 M Na 2 SO 4 aqueous solution. Additionally, MnO 2 nanorods/graphene composite materials exhibit highest energy density of 16 Wh kg −1 at power density of 95 W kg −1 and excellent capacitance retention with no more than 6% capacitance loss after 1000 cycles at the most favorable composites ratio

Preparation and electrochemical characterization of MnOOH nanowire-graphene oxide

International Nuclear Information System (INIS)

Wang Lin; Wang Dianlong

2011-01-01

Highlights: → MnOOH nanowire-graphene oxide composites are prepared by hydrothermal reaction in distilled water or 5% ammonia aqueous solution at 130 deg. C, with MnO 2 -graphene oxide composites which are synthesized by a redox reaction between KMnO 4 and graphene oxide. → MnO 2 is deoxidized to MnOOH on graphene oxide through hydrothermal reaction without any extra reductants. → It is found that the electrochemical resistance of MnOOH nanowire-graphene oxide composites decreases and the capacitance increases to 76 F g -1 when hydrothermal reaction is conducted in ammonia aqueous solution. → MnOOH nanowire-graphene oxide composites prepared by hydrothermal reaction in 5% ammonia aqueous solution have excellent capacitance retention ratio at scan rate from 5 mV s -1 to 40 mV s -1 . - Abstract: MnOOH nanowire-graphene oxide composites are prepared by hydrothermal reaction in distilled water or 5% ammonia aqueous solution at 130 deg. C with MnO 2 -graphene oxide composites which are synthesized by a redox reaction between KMnO 4 and graphene oxide. Powder X-ray diffraction (XRD) analyses and energy dispersive X-ray analyses (EDAX) show MnO 2 is deoxidized to MnOOH on graphene oxide through hydrothermal reaction without any extra reductants. The electrochemical capacitance of MnOOH nanowire-graphene oxide composites prepared in 5% ammonia aqueous solution is 76 F g -1 at current density of 0.1 A g -1 . Moreover, electrochemical impedance spectroscopy (EIS) suggests the electrochemical resistance of MnOOH nanowire-graphene oxide composites is reduced when hydrothermal reaction is conducted in ammonia aqueous solution. The relationship between the electrochemical capacitance and the structure of MnOOH nanowire-graphene oxide composites is characterized by cyclic voltammetry (CV) and field emission scanning electron microscopy (FESEM). The results indicate the electrochemical performance of MnOOH nanowire-graphene oxide composites strongly depends on their

Electrochemical sensing of etoposide using carbon quantum dot modified glassy carbon electrode.

Science.gov (United States)

Nguyen, Hoai Viet; Richtera, Lukas; Moulick, Amitava; Xhaxhiu, Kledi; Kudr, Jiri; Cernei, Natalia; Polanska, Hana; Heger, Zbynek; Masarik, Michal; Kopel, Pavel; Stiborova, Marie; Eckschlager, Tomas; Adam, Vojtech; Kizek, Rene

2016-04-25

In this study, enhancement of the electrochemical signals of etoposide (ETO) measured by differential pulse voltammetry (DPV) by modifying a glassy carbon electrode (GCE) with carbon quantum dots (CQDs) is demonstrated. In comparison with a bare GCE, the modified GCE exhibited a higher sensitivity towards electrochemical detection of ETO. The lowest limit of detection was observed to be 5 nM ETO. Furthermore, scanning electron microscopy (SEM), fluorescence microscopy (FM), and electrochemical impedance spectroscopy (EIS) were employed for the further study of the working electrode surface after the modification with CQDs. Finally, the GCE modified with CQDs under optimized conditions was used to analyse real samples of ETO in the prostate cancer cell line PC3. After different incubation times (1, 3, 6, 9, 12, 18 and 24 h), these samples were then prepared prior to electrochemical detection by the GCE modified with CQDs. High performance liquid chromatography with an electrochemical detection method was employed to verify the results from the GCE modified with CQDs.

Effect of black clay soil moisture on the electrochemical behavior of API X70 pipeline steel

Science.gov (United States)

Hendi, R.; Saifi, H.; Belmokre, K.; Ouadah, M.; Smili, B.; Talhi, B.

2018-03-01

The effect of moisture content variation (20–100 wt.%) on the electrochemical behavior of API X70 pipeline steel buried in the soil of Skikda (East of Algeria) was studied using electrochemical techniques, scanning electron microscopy (SEM), X ray diffraction analysis (XRD) and weight loss measurement. The electrochemical measurements showed that the corrosion current Icorr is directly proportional to the moisture content up to 50 wt.%, beyond this content, this value becomes almost constant. The result were confirmed by electrochemical impedance spectroscopy; the capacitance of the double layer formed on the surface is the highest at 50 wt.%. A single time constant was detected by plotting the Bode diagrams. The steel surface degradation has been appreciated using the scanning electron microscopy observations. A few pitting corrosion at 20 wt.% moisture, followed by more degradation at 50 wt.% have been revealed. However, when the moisture amount exceeded 50 wt.%, the surface became entirely covered by a corrosion product. XRD analysis revealed the dominance of FeOOH and Fe3O4 phases on steel surface for a moisture content of 50 wt.%.

Cyclic voltammetry and scanning electrochemical microscopy studies of methylene blue immobilized on the self-assembled monolayer of n-dodecanethiol

Energy Technology Data Exchange (ETDEWEB)

Salamifar, Seyed Ehsan [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Mehrgardi, Masoud Ayatollahi [Department of Chemistry, University of Isfahan, Isfahan (Iran, Islamic Republic of); Kazemi, Sayed Habib [Department of Chemistry, Institute for Advanced Studies in Basic Sciences (IASBS), Zanjan (Iran, Islamic Republic of); Mousavi, Mir Fazllollah, E-mail: mousavim@modares.ac.i [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of)

2010-12-30

Electron transfer (ET) kinetics through n-dodecanethiol (C{sub 12}SH) self-assembled monolayer on gold electrode was studied using cyclic voltammetry (CV), scanning electrochemical microscopy (SECM) and electrochemical impedance spectroscopy (EIS). An SECM model for compensating pinhole contribution, was used to measure the ET kinetics of solution-phase probes of ferrocyanide/ferricyanide (Fe(CN){sub 6}{sup 4-/3-}) and ferrocenemethanol/ferrociniummethanol (FMC{sup 0/+}) through the C{sub 12}SH monolayer yielding standard tunneling rate constant (k{sub ET}{sup 0}) of (4 {+-} 1) x 10{sup -11} and (3 {+-} 1) x 10{sup -10} cm s{sup -1} for Fe(CN){sub 6}{sup 4-/3-} and FMC{sup 0/+} respectively. Decay tunneling constants ({beta}) of 0.97 and 0.96 A{sup -1} for saturated alkane thiol chains were obtained using Fe(CN){sub 6}{sup 4-} and FMC respectively. Also, it was found that methylene blue (MB) molecules are effectively immobilized on the C{sub 12}SH monolayer and can mediate the ET between the solution-phase probes and underlying gold substrate. SECM-mediated model was used to simultaneously measure the bimolecular ET between the solution-phase probes and the monolayer-immobilized MB molecules, as well as tunneling ET between the monolayer-immobilized MB molecules and the underlying gold electrode, allowing the measurement of k{sub BI} = (5 {+-} 1) x 10{sup 6} and (4 {+-} 2) x 10{sup 7} cm{sup 3} mol{sup -1} s{sup -1} for the bimolecular ET and k{sub ET/MB}{sup 0}=(1{+-}0.3)x10{sup -3} and (7 {+-} 3) x 10{sup -2} s{sup -1} for the standard tunneling rate constant of ET using Fe(CN){sub 6}{sup 4-/3-} and FMC{sup 0/+} probes respectively.

Measurement of the quantum conductance of germanium by an electrochemical scanning tunneling microscope break junction based on a jump-to-contact mechanism.

Science.gov (United States)

Xie, Xufen; Yan, Jiawei; Liang, Jinghong; Li, Jijun; Zhang, Meng; Mao, Bingwei

2013-10-01

We present quantum conductance measurements of germanium by means of an electrochemical scanning tunneling microscope (STM) break junction based on a jump-to-contact mechanism. Germanium nanowires between a platinum/iridium tip and different substrates were constructed to measure the quantum conductance. By applying appropriate potentials to the substrate and the tip, the process of heterogeneous contact and homogeneous breakage was realized. Typical conductance traces exhibit steps at 0.025 and 0.05 G0. The conductance histogram indicates that the conductance of germanium nanowires is located between 0.02 and 0.15 G0 in the low-conductance region and is free from the influence of substrate materials. However, the distribution of conductance plateaus is too discrete to display distinct peaks in the conductance histogram of the high-conductance region. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A Comprehensive Pitting Study of High Velocity Oxygen Fuel Inconel 625 Coating by Using Electrochemical Testing Techniques

Science.gov (United States)

Niaz, Akbar; Khan, Sajid Ullah

2016-01-01

In the present work, Inconel 625 was coated on a mild steel substrate using a high velocity oxygen fuel coating process. The pitting propensity of the coating was tested by using open circuit potential versus time, potentiodynamic polarization, electrochemical potentiokinetic reactivation, and scanning electrochemical microscopy. The pitting propensity of the coating was compared with bulk Inconel 625 alloy. The results confirmed that there were regions of different electrochemical activities on the coating which have caused pitting corrosion.

Modified porous silicon for electrochemical sensor of para-nitrophenol

International Nuclear Information System (INIS)

Belhousse, S.; Belhaneche-Bensemra, N.; Lasmi, K.; Mezaache, I.; Sedrati, T.; Sam, S.; Tighilt, F.-Z.; Gabouze, N.

2014-01-01

Highlights: • Hybrid device based on Porous silicon (PSi) and polythiophene (PTh) was prepared. • Three types of PSi/PTh hybrid structures were elaborated: PSi/PTh, oxide/PSi/PTh and Amino-propyltrimethoxysilane (APTMES)/oxide/PSi/PTh. • PTh was grafted on PSi using electrochemical polymerization. • The electrodetection of para-nitrophenol (p-NPh) was performed by cyclic voltammetry. • Oxide/PSi/PTh and APTMES/oxide/PSi/PTh, based electrochemical sensor showed a good response toward p-NPh. - Abstract: Hybrid structures based on polythiophene modified porous silicon was used for the electrochemical detection of para-nitrophenol, which is a toxic derivative of parathion insecticide and it is considered as a major toxic pollutant. The porous silicon was prepared by anodic etching in hydrofluodic acid. Polythiophene films were then grown by electropolymerisation of thiophene monomer on three different surfaces: hydrogenated PSi, oxidized PSi and amine-terminated PSi. The morphology of the obtained structures were observed by scanning electron microscopy and characterized by spectroscopy (FTIR). Cyclic voltammetry was used to study the electrochemical response of proposed structures to para-nitrophenol. The results show a high sensitivity of the sensor and a linearity of the electrochemical response in a large concentration interval ranging from 1.5 × 10 −8 M to the 3 × 10 −4 M

Electrochemical Synthesis of Graphene/MnO2 Nano-Composite for Application to Supercapacitor Electrode.

Science.gov (United States)

Jeong, Kwang Ho; Lee, Hyeon Jeong; Simpson, Michael F; Jeong, Mun

2016-05-01

Graphene/MnO2 nano-composite was electrochemically synthesized for application to an electrode material for electrochemical supercapacitors. The nanosized needle-like MnO2 was obtained by use of a graphene substrate. The prepared composite exhibited an ideal supercapacitive behavior. A capacitance retention of 94% was achieved with a 4 h deposition time (an initial capacitance of 574 mF/cm2 at a scan rate of 20 mV/s) and the retention declined with further deposition time. The results demonstrate enhanced contact between the electrode and electrolyte and improved power density as an electrochemical capacitor.

Conductive polymer/reduced graphene oxide/Au nano particles as efficient composite materials in electrochemical supercapacitors

Science.gov (United States)

Shabani Shayeh, J.; Ehsani, A.; Ganjali, M. R.; Norouzi, P.; Jaleh, B.

2015-10-01

Polyaniline/reduced graphene oxide/Au nano particles (PANI/rGO/AuNPs) as a hybrid supercapacitor were deposited on a glassy carbon electrode (GCE) by cyclic voltammetry (CV) method as ternary composites and their electrochemical performance was evaluated in acidic medium. Scanning electron micrographs clearly revealed the formation of nanocomposites on the surface of the working electrode. Scanning electron micrographs (SEM) clearly revealed the formation of nanocomposites on the surface of working electrode. Different electrochemical methods including galvanostatic charge-discharge (CD) experiments, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were carried out in order to investigate the applicability of the system as a supercapacitor. Based on the cyclic voltammogram results obtained, PANI/rGO/AuNPs gave higher specific capacitance, power and energy values than PANI at a current density of 1 mA cm-2. Specific capacitance (SC) of PANI and PANI/rGO/AuNPs electrodes calculated using CV method are 190 and 303 F g-1, respectively. The present study introduces new nanocomposite materials for electrochemical redox capacitors with advantages including long life cycle and stability due to synergistic effects of each component.

Corrosion behaviour of zinc and aluminum magnesium alloys by scanning reference electrode technique (SRET) and electrochemical noise (EN)

International Nuclear Information System (INIS)

Klassen, R.D.; Roberge, P.R.; Lafront, A.-M.; Oteyaka, M.O.; Ghali, E.

2005-01-01

The corrosion characteristics of five permanent mould magnesium alloys were studied. Two contained aluminum (AZ91D and AZ91E) and three contained zinc as the primary alloying element (ZA104 (Zn 10%, Al 4%), ZAC and ZACS). ZAC contained a small amount of calcium and ZACS contained small amounts of calcium and strontium. Two techniques were used in this study, namely 1) scanning reference electrode technique (SRET) and 2) electrochemical noise (EN). The test solution for each case was 5% NaCl saturated with Mg(OH)2 at room temperature. According to the EN measurements, the corrosion rate of AZ91D was the lowest followed by AZ91E, ZACS, ZAC and ZA104. The EN measurements showed that both the frequency and magnitude of current transients were much higher for the zinc based alloys than for the aluminum based alloys. The SRET measurements illustrated that localized corrosion occurred more frequently on the ZA104 sample than on the AZ91D sample. It seemed that increasing the level of zinc and lowering the level of aluminum relative to the levels in AZ91D does not improve corrosion resistance. (author)

Multilayered films of cobalt oxyhydroxide nanowires/manganese oxide nanosheets for electrochemical capacitor

Energy Technology Data Exchange (ETDEWEB)

Zheng, Huajun [State Key Laboratory Breeding Base of Green Chemistry Synthesis Technology, Zhejiang University of Technology, Hangzhou 310014 (China); ARC Centre of Excellence for Functional Nanomaterials, School of Chemical Engineering and AIBN, The University of Queensland, St Lucia, Brisbane, QLD 4072 (Australia); Tang, Fengqiu; Mukherji, Aniruddh; Yan, Xiaoxia; Wang, Lianzhou (Max) Lu, Gao Qing [ARC Centre of Excellence for Functional Nanomaterials, School of Chemical Engineering and AIBN, The University of Queensland, St Lucia, Brisbane, QLD 4072 (Australia); Lim, Melvin [Division of Environmental and Water Resources Engineering, School of Civil and Environmental Engineering, Nanyang Technological University, 639798 (Singapore)

2010-01-15

Multilayered films of cobalt oxyhydroxide nanowires (CoOOHNW) and exfoliated manganese oxide nanosheet (MONS) are fabricated by potentiostatic deposition and electrostatic self-assembly on indium-tin oxide coated glass substrates. The morphology and chemical composition of these films are characterized by scanning electron microscopy (SEM) and X-ray photoelectron spectra (XPS) and the potential application as electrochemical supercapacitors are investigated using cyclic voltammetry and charge-discharge measurements. These ITO/CoOOHNW/MONS multilayered film electrodes exhibit excellent electrochemical capacitance properties, including high specific capacitance (507 F g{sup -1}) and long cycling durability (less 2% capacity loss after 5000 charge/discharge cycles). These characteristics indicate that these newly developed films may find important application for electrochemical capacitors. (author)

One-Step Hydrothermal-Electrochemical Route to Carbon-Stabilized Anatase Powders

Science.gov (United States)

Tao, Ying; Yi, Danqing; Zhu, Baojun

2013-04-01

Black carbon-stabilized anatase particles were prepared by a simple one-step hydrothermal-electrochemical method using glucose and titanium citrate as the carbon and titanium source, respectively. Morphological, chemical, structural, and electrochemical characterizations of these powders were carried out by Raman spectroscopy, Fourier-transform infrared spectroscopy, x-ray diffraction, scanning electron microscopy, and cyclic voltammetry. It was revealed that 200-nm carbon/anatase TiO2 was homogeneously dispersed, and the powders exhibited excellent cyclic performance at high current rates of 0.05 V/s. The powders are interesting potential materials that could be used as anodes for lithium-ion batteries.

Electrochemical properties of opal-V6O13 composites

International Nuclear Information System (INIS)

Vernardou, D.; Apostolopoulou, M.; Louloudakis, D.; Spanakis, E.; Katsarakis, N.; Koudoumas, E.; McGrath, J.; Pemble, M.E.

2014-01-01

Highlights: • Opal-V 6 O 13 composites grown at 95 °C for 50 h. • The deposition period affects the void filling of the opals. • The electrochemical performance is correlated with the oxide’s characteristics. -- Abstract: Vanadium oxides were hydrothermally grown on opal glass substrates at 95 °C. The deposition period was observed to affect the structure of the oxides and the voids filling of the opal surfaces. V 6 O 13 grown on opal for 50 h presented satisfactory electrochemical performance and electrochromic response with a contrast ratio of 2. The specific capacitance of this composite reached a value of 192 F g −1 , which was stable up to 500 continuous charge intercalation/deintercalation scans. The importance of achieving crystalline V 6 O 13 and high opal surface coverage towards the enhancement of the electrochemical properties is presented

Fabrication and electrochemical performance of graphene—ZnO nanocomposites

International Nuclear Information System (INIS)

Li Zhen-Peng; Men Chuan-Ling; Wang Wan; Cao Jun

2014-01-01

Graphene—ZnO nanocomposites were synthesized successfully through a one-step solvothermal approach. The morphology, structure, and composition of the prepared nanocomposites were investigated by scanning electron microscopy (SEM), transmission electron microscope (TEM), laser micro Raman spectroscopy, and Fourier transform infra-red spectroscopy (FT-IR). The outcomes confirmed that this approach is comparatively steady, practicable, and operable compared with other reported methods. The electrochemical performance of the graphene-ZnO electrodes was analyzed through cyclic voltammetry, altering-current (AC) impedance, and chronopotentiometry tests. The graphene—ZnO electrodes exhibited an improved electrode performance with higher specific capacitance (115 F·g −1 ), higher electrochemical stability, and higher energy density than the graphene electrodes and most reported graphene—ZnO electrodes. Graphene—ZnO nanocomposites have a steady reversible charge/discharge behavior, which makes them promising candidates for electrochemical capacitors (ECs). (condensed matter: electronic structure, electrical, magnetic, and optical properties)

Microstructure and mechanical properties of friction welded AISI 1040/AISI 304L steels before and after electrochemical corrosion

Energy Technology Data Exchange (ETDEWEB)

Sarsilmaz, Furkan [Firat Univ., Elazig (Turkey). Dept. of Mechatronics Engineering; Kirik, Ihsan [Batman Univ. (Turkey); Ozdemir, Niyazi [Firat Univ., Elazig (Turkey)

2018-03-01

The aim of the present study is to investigate the effect of welding parameters both on the electrochemical corrosion behavior and tensile strength of pre- and post-electrochemical corrosion of friction welded dissimilar steels. The microstructural changes of AISI 1040/AISI 304L friction welded couples and also parent materials were analyzed by using scanning electron microscopy. The electrochemical behaviors of AISI1040/AISI304L joints were comparatively investigated by potentiodynamic polarization curve test and by electrochemical impedance spectra. Moreover, tensile strength experiments were carried out determining the behavior of friction welded joints of pre- and post-electrochemical corrosion and results indicated that the maximum tensile test value of the dissimilar welded pre-electrochemical corrosion was higher than those of post-electrochemical corrosion and was also very close to AISI 1040 parent material value.

Electrochemical properties of arc-black and carbon nano-balloon as electrochemical capacitor electrodes

International Nuclear Information System (INIS)

Sato, T; Suda, Y; Uruno, H; Takikawa, H; Tanoue, H; Ue, H; Aoyagi, N; Okawa, T; Shimizu, K

2012-01-01

In this study, we used two types of carbon nanomaterials, arc-black (AcB) which has an amorphous structure and carbon nano-balloon (CNB) which has a graphitic structure as electrochemical capacitor electrodes. We made a coin electrode from these carbon materials and fabricated an electric double-layer capacitor (EDLC) that sandwiches a separator between the coin electrodes. On the other hand, RuO 2 was loaded on these carbon materials, and we fabricated a pseudo-capacitor that has an ion insertion mechanism into RuO 2 . For comparison with these carbon materials, activated carbon (AC) was also used for a capacitor electrode. The electrochemical properties of all the capacitors were evaluated in 1M H 2 SO 4 aqueous solution. As a result of EDLC performance, AcB electrode had a higher specific capacitance than AC electrode at a high scan rate (≥ 100 mV/s). In the evaluation of pseudo-capacitor performance, RuO 2 -loaded CNB electrode showed a high specific capacitance of 734 F/g per RuO 2 weight.

A highly selective copper-indium bimetallic electrocatalyst for the electrochemical reduction of aqueous CO2to CO

KAUST Repository

Rasul, Shahid; Anjum, Dalaver H.; Jedidi, Abdesslem; Minenkov, Yury; Cavallo, Luigi; Takanabe, Kazuhiro

2014-01-01

The challenge in the electrochemical reduction of aqueous carbon dioxide is in designing a highly selective, energy-efficient, and non-precious-metal electrocatalyst that minimizes the competitive reduction of proton to form hydrogen during aqueous

Electrochemical characterization of the underpotential deposition of tellurium on Au electrode

International Nuclear Information System (INIS)

Zhu, W.; Yang, J.Y.; Zhou, D.X.; Bao, S.Q.; Fan, X.A.; Duan, X.K.

2007-01-01

Electrochemical characterization of the underpotential deposition (UPD) of tellurium on Au substrate has been performed in this paper. The mechanism of Te deposition and its voltammetry dependence on the Te ion concentration were studied, and it suggests that variations in the metal ion concentration may affect the UPD process kinetics. The effect of tellurium adsorbates on UPD behavior of Te has also been investigated. The results show that the tellurium adsorbates could be irreversibly adsorbed upon the Au substrate surface under the open-circuit conditions. Subsequent removal of the Te adsorbates was also proved to be very difficult within the Au double-layer region, and a standard electrochemical cleaning procedure is necessary to remove the Te adsorbates completely. When the potential was cycled into the Au oxidation region, a substantial loss of Te adsobates was observed, which occurs simultaneously with the Au oxidation features. Scan rate dependent cyclic voltammetry experiments reveal that the peak current in the Te UPD peak is not a linear function of the scan rate, ν, but of a 2/3 power of the scan rate, ν 2/3 . It is in good consistent with a two-dimension nucleation and growth mechanism

MnO2 prepared by hydrothermal method and electrochemical performance as anode for lithium-ion battery.

Science.gov (United States)

Feng, Lili; Xuan, Zhewen; Zhao, Hongbo; Bai, Yang; Guo, Junming; Su, Chang-Wei; Chen, Xiaokai

2014-01-01

Two α-MnO2 crystals with caddice-clew-like and urchin-like morphologies are prepared by the hydrothermal method, and their structure and electrochemical performance are characterized by scanning electron microscope (SEM), X-ray diffraction (XRD), galvanostatic cell cycling, cyclic voltammetry, and electrochemical impedance spectroscopy (EIS). The morphology of the MnO2 prepared under acidic condition is urchin-like, while the one prepared under neutral condition is caddice-clew-like. The identical crystalline phase of MnO2 crystals is essential to evaluate the relationship between electrochemical performances and morphologies for lithium-ion battery application. In this study, urchin-like α-MnO2 crystals with compact structure have better electrochemical performance due to the higher specific capacity and lower impedance. We find that the relationship between electrochemical performance and morphology is different when MnO2 material used as electrochemical supercapacitor or as anode of lithium-ion battery. For lithium-ion battery application, urchin-like MnO2 material has better electrochemical performance.

Electrochemical and surface studies of some Porphines as corrosion inhibitor for J55 steel in sweet corrosion environment

Energy Technology Data Exchange (ETDEWEB)

Singh, Ambrish, E-mail: ambrish.16752@ipu.co.in [State Key Laboratory of Oil and Gas Reservoir Geology and Exploitation (Southwest Petroleum University), Chengdu, Sichuan 610500 (China); Department of Chemistry, LFTS, Lovely Professional University, Phagwara, Punjab 144402 (India); Lin, Yuanhua, E-mail: yhlin28@163.com [State Key Laboratory of Oil and Gas Reservoir Geology and Exploitation (Southwest Petroleum University), Chengdu, Sichuan 610500 (China); Ansari, K.R.; Quraishi, M.A. [Department of Applied Chemistry, Indian Institute of Technology, Banaras Hindu University, Varanasi, U.P. (India); Ebenso, Eno. E. [Department of Chemistry, School of Mathematical & Physical Sciences, North-West University(Mafikeng Campus), Private Bag X2046, Mmabatho 2735 (South Africa); Chen, Songsong; Liu, Wanying [CNPC Key Lab for Tubular Goods Engineering (Southwest Petroleum University), Chengdu, Sichuan 610500 (China)

2015-12-30

Graphical abstract: Corrosion inhibition of J55 steel in 3.5 wt.% NaCl solution saturated with CO2 by the three Porphines 5,10,15,20-Tetra(4-pyridyl)-21H,23H-porphine (P1), 5,10,15,20-Tetraphenyl-21H,23H-porphine (P2), 5,10,15,20-Tetrakis(4-hydroxyphenyl)-21H,23H-porphine (P3), electrochemical impedance spectroscopy (EIS), contact angle measurement, scanning electrochemical microscopy (SECM), and atomic force microscopy (AFM). - Highlights: • J55 steel protection in 3.5% NaCl solution saturated with CO2 by Porphines. • Weight loss and impedance results are in good agreement. • The adsorption of Porphines obeys the Langmuir adsorption isotherm. • Scanning electrochemical microscopy is used to discuss the insulated and conductive surface. • Examination of surface morphology by AFM. - Abstract: Corrosion inhibition of J55 steel in 3.5 wt.% NaCl solution saturated with CO{sub 2} by the three Porphines 5,10,15,20-Tetra(4-pyridyl)-21H,23H-porphine (P1), 5,10,15,20-Tetraphenyl-21H,23H-porphine (P2), 5,10,15,20-Tetrakis(4-hydroxyphenyl)-21H,23H-porphine (P3), electrochemical impedance spectroscopy (EIS), Contact angle measurement, scanning electrochemical microscopy (SECM), and atomic force microscopy (AFM). Adsorption of such Porphines on the J55 steel surface obeyed to the Langmuir adsorption isotherm. Atomic force microscopy (AFM), SECM, and Contact angle results confirm the formation of inhibitor film on J55 steel surface thereby mitigating corrosion.

Electrochemical and surface studies of some Porphines as corrosion inhibitor for J55 steel in sweet corrosion environment

International Nuclear Information System (INIS)

Singh, Ambrish; Lin, Yuanhua; Ansari, K.R.; Quraishi, M.A.; Ebenso, Eno. E.; Chen, Songsong; Liu, Wanying

2015-01-01

Graphical abstract: Corrosion inhibition of J55 steel in 3.5 wt.% NaCl solution saturated with CO2 by the three Porphines 5,10,15,20-Tetra(4-pyridyl)-21H,23H-porphine (P1), 5,10,15,20-Tetraphenyl-21H,23H-porphine (P2), 5,10,15,20-Tetrakis(4-hydroxyphenyl)-21H,23H-porphine (P3), electrochemical impedance spectroscopy (EIS), contact angle measurement, scanning electrochemical microscopy (SECM), and atomic force microscopy (AFM). - Highlights: • J55 steel protection in 3.5% NaCl solution saturated with CO2 by Porphines. • Weight loss and impedance results are in good agreement. • The adsorption of Porphines obeys the Langmuir adsorption isotherm. • Scanning electrochemical microscopy is used to discuss the insulated and conductive surface. • Examination of surface morphology by AFM. - Abstract: Corrosion inhibition of J55 steel in 3.5 wt.% NaCl solution saturated with CO_2 by the three Porphines 5,10,15,20-Tetra(4-pyridyl)-21H,23H-porphine (P1), 5,10,15,20-Tetraphenyl-21H,23H-porphine (P2), 5,10,15,20-Tetrakis(4-hydroxyphenyl)-21H,23H-porphine (P3), electrochemical impedance spectroscopy (EIS), Contact angle measurement, scanning electrochemical microscopy (SECM), and atomic force microscopy (AFM). Adsorption of such Porphines on the J55 steel surface obeyed to the Langmuir adsorption isotherm. Atomic force microscopy (AFM), SECM, and Contact angle results confirm the formation of inhibitor film on J55 steel surface thereby mitigating corrosion.

Electrochemically fabricated polyaniline nanowire-modified electrode for voltammetric detection of DNA hybridization

International Nuclear Information System (INIS)

Zhu Ningning; Chang Zhu; He Pingang; Fang Yuzhi

2006-01-01

A novel and sensitive electrochemical DNA biosensor based on electrochemically fabricated polyaniline nanowire and methylene blue for DNA hybridization detection is presented. Nanowires of conducting polymers were directly synthesized through a three-step electrochemical deposition procedure in an aniline-containing electrolyte solution, by using the glassy carbon electrode (GCE) as the working electrode. The morphology of the polyaniline films was examined using a field emission scanning electron microscope (SEM). The diameters of the nanowires range from 80 to 100 nm. The polyaniline nanowires-coated electrode exhibited very good electrochemical conductivity. Oligonucleotides with phosphate groups at the 5' end were covalently linked onto the amino groups of polyaniline nanowires on the electrode. The hybridization events were monitored with differential pulse voltammetry (DPV) measurement using methylene blue (MB) as an indicator. The approach described here can effectively discriminate complementary from non-complementary DNA sequence, with a detection limit of 1.0 x 10 -12 mol l -1 of complementary target, suggesting that the polyaniline nanowires hold great promises for sensitive electrochemical biosensor applications

A new protocol for the distribution of MnO{sub 2} nanoparticles on rGO sheets and the resulting electrochemical performance

Energy Technology Data Exchange (ETDEWEB)

Samdani, Jitendra; Samdani, Kunda; Kim, Nam Hoon [Department of BIN Convergence Technology, Chonbuk National University, Jeonju, Jeonbuk, 561-756 (Korea, Republic of); Lee, Joong Hee, E-mail: jhl@chonbuk.ac.kr [Department of BIN Convergence Technology, Chonbuk National University, Jeonju, Jeonbuk, 561-756 (Korea, Republic of); Center for Carbon Composites Materials, Department of Polymer & Nano Science and Technology, Chonbuk National University, Jeonju, Jeonbuk, 561-756 (Korea, Republic of)

2017-03-31

Highlights: • The role of KMnO{sub 4} for the deposition of MnO{sub 2} on rGO was studied. • The as-synthesized rGM-1 shows good stability and a high specific capacitance value (366 F/g). • rGM-1 effectively detects dopamine with a detection limit of 2.3 × 10{sup −7} M. - Abstract: Herein, reduced graphene oxide (rGO)/MnO{sub 2} hybrid materials were prepared via a direct redox reaction between MnCl{sub 2} and KMnO{sub 4} on reduced graphene oxide (rGO){sub .} A systematic study was carried out to understand the role of KMnO{sub 4}. The morphology and microstructure of the as-prepared composite was characterized using field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Raman Spectroscopy. Results indicate that the concentrations of KMnO{sub 4} have a detrimental effect on the distribution of MnO{sub 2} nanoparticles on rGO sheets and hence on electrochemical properties. The electrochemical capacitive behavior of the as-prepared composite was investigated using cyclic voltammetry (CV), galvanostatic charge discharge, and electrochemical impedance spectroscopy (EIS) in 1 M Na{sub 2}SO{sub 4} aqueous electrolyte solution. At the optimum concentration of KMnO{sub 4}, the as-prepared rGM-1 composite shows a high specific capacitance of 366 F/g at a scan rate of 10 mV/s. The composite also exhibits good electrocatalytic activity towards the oxidation of dopamine (DA), exhibiting a low detection limit of 2.3 × 10{sup −7} M with a wide linear range between 2.5 × 10{sup −7} M and 2.30 × 10{sup −4} M. Hence, the use of rGO/MnO{sub 2} at an optimized concentration of KMnO{sub 4} is a potential competitive candidate in supercapacitor and biosensor applications.

Applications of Silver Nanowires on Transparent Conducting Film and Electrode of Electrochemical Capacitor

Directory of Open Access Journals (Sweden)

Yuan-Jun Song

2014-01-01

Full Text Available Silver nanowire has potential applications on transparent conducting film and electrode of electrochemical capacitor due to its excellent conductivity. Transparent conducting film (G-film was prepared by coating silver nanowires on glass substrate using Meyer rod method, which exhibited better performance than carbon nanotube and graphene. The conductivity of G-film can be improved by increasing sintering temperature. Electrode of electrochemical capacitor (I-film was fabricated through the same method with G-film on indium tin oxide (ITO. CV curves of I-film under different scanning rates had obvious redox peaks, which indicated that I-film exhibited excellent electrochemical pseudocapacitance performance and good reversibility during charge/discharge process. In addition, the specific capacitance of I-film was measured by galvanostatic charge/discharge experiments, indicating that I-film exhibits high special capacitance and excellent electrochemical stability.

3,5-Diamino-1,2,4-triazole@electrochemically reduced graphene oxide film modified electrode for the electrochemical determination of 4-nitrophenol

International Nuclear Information System (INIS)

Kumar, Deivasigamani Ranjith; Kesavan, Srinivasan; Baynosa, Marjorie Lara; Shim, Jae-Jin

2017-01-01

Highlights: •Triazole film was formed on electrochemically reduced graphene oxide. •pDAT@ERGO/GC was utilized for the electrochemical determination of 4-nitrophenol. •pDAT@ERGO/GC electrode offered wide concentration and nanomolar detection limit. •The fabricated electrode was employed in water sample analyses. -- Abstract: In this study, an eco-friendly benign method for the modification of electrochemically reduced graphene oxide (ERGO) on glassy carbon (GC) surface and electrochemical polymerized 3,5-diamino-1,2,4-triazole (DAT) film composite (pDAT@ERGO/GC) electrode was developed. The surface morphologies of the pDAT@ERGO/GC modified electrode were analyzed by field emission scanning electron microscopy (FESEM). FESEM images indicated that the ERGO supported pDAT has an almost homogeneous morphology structure with a size of 70 to 80 nm. It is due to the water oxidation reaction occurred while pDAT@ERGO/GC fabrication peak at +1.4 V leads to O 2 evolution and oxygen functional group functionalization on ERGO, which confirmed by X-ray photoelectron spectroscopy (XPS). In contrast, the bare GC modified with pDAT showed randomly arranged irregular bulky morphology structure compared to those of pDAT@ERGO/GC. Electrochemical reduction of graphene oxide was confirmed by Raman spectroscopy, XPS, and electrochemical impedance spectroscopy (EIS). The pDAT@ERGO/GC modified electrode was used for the electrochemical determination of 4-nitrophenol (4-NP). The 4-NP oxidation peak was observed at +0.25 V, and the differential pulse voltammetry demonstrated wide concentration range (5–1500 μM), high sensitivity (0.7113 μA μM −1 ), and low limit of detection (37 nM). Moreover, the pDAT@ERGO/GC electrode was applied to real water sample analysis by standard addition method, where in good recoveries (97.8% to 102.4%) were obtained.

Time dependence of the natural passivation process on AISI 304 in an alkaline medium: Atomic force microscopy and scanning Kelvin probe force microscopy as additional tools to electrochemical impedance spectroscopy

Science.gov (United States)

Benaioun, N. E.; Maafa, I.; Florentin, A.; Denys, E.; Hakiki, N. E.; Moulayat, N.; Bubendorff, J. L.

2018-04-01

Thin surface films formed on AISI 304 samples in an alkaline solution of pH = 13 are studied by atomic force microscopy (AFM), scanning Kelvin probe force microscopy (SKPFM) and electrochemical impedance spectroscopy (EIS) as a function of immersion time. The results reveal that changes on EIS diagrams correspond to topographical modifications on the sample surface as shown by AFM. Both techniques are therefore complementary. The oxide layer is chemically homogenous as shown by SKPFM imaging and our ultra-thin passive layer is an efficient barrier against corrosion.

Electrochemical Properties for Co-Doped Pyrite with High Conductivity

Directory of Open Access Journals (Sweden)

Yongchao Liu

2015-09-01

Full Text Available In this paper, the hydrothermal method was adopted to synthesize nanostructure Co-doped pyrite (FeS2. The structural properties and morphology of the synthesized materials were characterized using X-ray diffraction (XRD and scanning electron microscopy (SEM, respectively. Co in the crystal lattice of FeS2 could change the growth rate of different crystal planes of the crystal particles, which resulted in various polyhedrons with clear faces and sharp outlines. In addition, the electrochemical performance of the doping pyrite in Li/FeS2 batteries was evaluated using the galvanostatic discharge test, cyclic voltammetry and electrochemical impedance spectroscopy. The results showed that the discharge capacity of the doped material (801.8 mAh·g−1 with a doping ratio of 7% was significantly higher than that of the original FeS2 (574.6 mAh·g−1 because of the enhanced conductivity. Therefore, the doping method is potentially effective for improving the electrochemical performance of FeS2.

Studies on the electrochemical behavior of heavy lanthanide ions and the synthesis, characterization of heavy metal chelate complexes

International Nuclear Information System (INIS)

Kang, Sam Woo; Chang, Choo Hwan; Son, Byung Chan; Suh, Moo Yul; Kim, Chae Kyun

1991-01-01

Electrochemical behavior of some heavy lanthanide ions(Gd 3+ , Tb 3+ , Dy 3+ , Ho 3+ , Er 3+ , Tm 3+ , Yb 3+ and Lu 3+ ) in various supporting electrolytes has been investigated by dc polarography, differential pulse polarography and cyclic voltammetry. The peak potentials and the peak currents, their dependency on the concentration and pH effects, the reversibility of the electrode reactions are described. The reduction of Gd 3+ , Tb 3+ , Dy 3+ , Ho 3+ , Er 3+ , Tm 3+ and Lu 3+ ions in 0.1M lithium chloride solution proceeds by a three-electron change directly to the metallic state, whereas the reduction of Yb 3+ proceeds by a one-electron change followed by a two-electron change. It was found that, in differential pulse polarography and cyclic voltammetry, the peak potential, peak current and current function showed constant value in the pH range of 4.0-6.0 by varying pH and scan rates. And also the current function is found to decrease as the sweep rate is increased when the pH reaches 4.0. This fact may indicate a chemical reaction coupled with the electrochemical reaction at lower pH values(pH 3+ ion is possible to determine voltammetrically within the error of ±3.5% in the presence of other competitive lanthanide ions. (Author)

Electrochemical study of the AISI 409 ferritic stainless steel: passive film stability and pitting nucleation and growth

International Nuclear Information System (INIS)

Souza, Juliana Sarango de; Oliveira, Leandro Antônio de; Antunes, Renato Altobelli; Sayeg, Isaac Jamil

2017-01-01

The aim of the present work was to study the passive film stability and pitting corrosion behavior of the AISI 409 stainless steel. The electrochemical tests were carried out in 0.1 M NaCl solution at room temperature. The general electrochemical behavior was assessed using electrochemical impedance spectroscopy (EIS) measurements whereas the semiconducting properties of the passive film were evaluated by the Mott-Schottky approach. Pitting corrosion was investigated using potentiodynamic and potentiostatic polarization tests. Surface morphology was examined using confocal laser scanning microscopy and scanning electron microscopy (SEM). Energy dispersive X-ray spectroscopy (EDS) analyses were carried out to identify the composition of precipitates that could act as preferential sites for the onset of pitting corrosion. The results showed that the passive film presents n-type semiconductive behavior. Grain boundaries played an important role as pitting initiation sites for the AISI 409 stainless steel. (author)

Electrochemical study of the AISI 409 ferritic stainless steel: passive film stability and pitting nucleation and growth

Energy Technology Data Exchange (ETDEWEB)

Souza, Juliana Sarango de [Universidade Federal de São Paulo (UNIFESP), Diadema, SP (Brazil). Departamento de Ciências Exatas e da Terra; Oliveira, Leandro Antônio de; Antunes, Renato Altobelli, E-mail: renato.antunes@ufabc.edu.br [Universidade Federal do ABC (CECS/UFABC), Santo André, SP (Brazil). Centro de Engenharia, Modelagem e Ciências Sociais Aplicadas; Sayeg, Isaac Jamil [Universidade de São Paulo (USP), SP (Brazil). Instituto de Geociências

2017-11-15

The aim of the present work was to study the passive film stability and pitting corrosion behavior of the AISI 409 stainless steel. The electrochemical tests were carried out in 0.1 M NaCl solution at room temperature. The general electrochemical behavior was assessed using electrochemical impedance spectroscopy (EIS) measurements whereas the semiconducting properties of the passive film were evaluated by the Mott-Schottky approach. Pitting corrosion was investigated using potentiodynamic and potentiostatic polarization tests. Surface morphology was examined using confocal laser scanning microscopy and scanning electron microscopy (SEM). Energy dispersive X-ray spectroscopy (EDS) analyses were carried out to identify the composition of precipitates that could act as preferential sites for the onset of pitting corrosion. The results showed that the passive film presents n-type semiconductive behavior. Grain boundaries played an important role as pitting initiation sites for the AISI 409 stainless steel. (author)

Modified porous silicon for electrochemical sensor of para-nitrophenol

Energy Technology Data Exchange (ETDEWEB)

Belhousse, S., E-mail: all_samia_b@yahoo.fr [Centre de Recherche en Technologie des Semi-conducteurs pour l’Energétique (CRTSE), Division Thin Films-Surface and Interface, 2, Bd. Frantz Fanon, B.P. 140, Alger-7 merveilles, Algiers (Algeria); Belhaneche-Bensemra, N., E-mail: nbelhaneche@yahoo.fr [Ecole Nationale Polytechnique (ENP), 10, Avenue Hassen Badi, B.P. 182, 16200, El Harrach, Algiers (Algeria); Lasmi, K., E-mail: kahinalasmi@yahoo.fr [Centre de Recherche en Technologie des Semi-conducteurs pour l’Energétique (CRTSE), Division Thin Films-Surface and Interface, 2, Bd. Frantz Fanon, B.P. 140, Alger-7 merveilles, Algiers (Algeria); Mezaache, I., E-mail: lyeso_44@hotmail.fr [Ecole Nationale Polytechnique (ENP), 10, Avenue Hassen Badi, B.P. 182, 16200, El Harrach, Algiers (Algeria); Sedrati, T., E-mail: tarek_1990m@hotmail.fr [Ecole Nationale Polytechnique (ENP), 10, Avenue Hassen Badi, B.P. 182, 16200, El Harrach, Algiers (Algeria); Sam, S., E-mail: Sabrina.sam@polytechnique.edu [Centre de Recherche en Technologie des Semi-conducteurs pour l’Energétique (CRTSE), Division Thin Films-Surface and Interface, 2, Bd. Frantz Fanon, B.P. 140, Alger-7 merveilles, Algiers (Algeria); Tighilt, F.-Z., E-mail: mli_zola@yahoo.fr [Centre de Recherche en Technologie des Semi-conducteurs pour l’Energétique (CRTSE), Division Thin Films-Surface and Interface, 2, Bd. Frantz Fanon, B.P. 140, Alger-7 merveilles, Algiers (Algeria); Gabouze, N., E-mail: ngabouze@yahoo.fr [Centre de Recherche en Technologie des Semi-conducteurs pour l’Energétique (CRTSE), Division Thin Films-Surface and Interface, 2, Bd. Frantz Fanon, B.P. 140, Alger-7 merveilles, Algiers (Algeria)

2014-11-15

Highlights: • Hybrid device based on Porous silicon (PSi) and polythiophene (PTh) was prepared. • Three types of PSi/PTh hybrid structures were elaborated: PSi/PTh, oxide/PSi/PTh and Amino-propyltrimethoxysilane (APTMES)/oxide/PSi/PTh. • PTh was grafted on PSi using electrochemical polymerization. • The electrodetection of para-nitrophenol (p-NPh) was performed by cyclic voltammetry. • Oxide/PSi/PTh and APTMES/oxide/PSi/PTh, based electrochemical sensor showed a good response toward p-NPh. - Abstract: Hybrid structures based on polythiophene modified porous silicon was used for the electrochemical detection of para-nitrophenol, which is a toxic derivative of parathion insecticide and it is considered as a major toxic pollutant. The porous silicon was prepared by anodic etching in hydrofluodic acid. Polythiophene films were then grown by electropolymerisation of thiophene monomer on three different surfaces: hydrogenated PSi, oxidized PSi and amine-terminated PSi. The morphology of the obtained structures were observed by scanning electron microscopy and characterized by spectroscopy (FTIR). Cyclic voltammetry was used to study the electrochemical response of proposed structures to para-nitrophenol. The results show a high sensitivity of the sensor and a linearity of the electrochemical response in a large concentration interval ranging from 1.5 × 10{sup −8} M to the 3 × 10{sup −4}M.

Improved electrochemical nucleic acid biosensor based on polyaniline-polyvinyl sulphonate

Energy Technology Data Exchange (ETDEWEB)

Prabhakar, Nirmal [Biomolecular Electronics and Conducting Polymer Research Group, National Physical Laboratory, Dr. K.S. Krishnan Marg, New Delhi-110012 (India); Centre for Biomedical Engineering, Indian Institute of Technology, Hauz Khas, New Delhi-110016 (India); Sumana, G.; Arora, Kavita [Biomolecular Electronics and Conducting Polymer Research Group, National Physical Laboratory, Dr. K.S. Krishnan Marg, New Delhi-110012 (India); Singh, Harpal [Centre for Biomedical Engineering, Indian Institute of Technology, Hauz Khas, New Delhi-110016 (India); Malhotra, B.D. [Biomolecular Electronics and Conducting Polymer Research Group, National Physical Laboratory, Dr. K.S. Krishnan Marg, New Delhi-110012 (India)], E-mail: bansi.malhotra@gmail.com

2008-05-01

DNA biosensor based on polyaniline (PANI)-polyvinyl sulphonate (PVS) has been fabricated using electrochemical entrapment technique for detection of organophosphorus pesticides (chlorpyrifos and malathion). These double stranded calf thymus DNA (dsCT-DNA) entrapped PANI-PVS/indium-tin-oxide (ITO) bioelectrodes have been characterized using square wave voltammetry (SWV), Fourier transform infra-red spectroscopy (FT-IR), scanning electron microscopy (SEM) and electrochemical impedance techniques, respectively. These dsCT-DNA entrapped PANI-PVS/ITO bioelectrodes have been found to have response time of 30 s, stability of about 6 months and detection limit for chlorpyrifos and malathion as 0.5 ppb and 0.01 ppm, respectively.

Improved electrochemical nucleic acid biosensor based on polyaniline-polyvinyl sulphonate

International Nuclear Information System (INIS)

Prabhakar, Nirmal; Sumana, G.; Arora, Kavita; Singh, Harpal; Malhotra, B.D.

2008-01-01

DNA biosensor based on polyaniline (PANI)-polyvinyl sulphonate (PVS) has been fabricated using electrochemical entrapment technique for detection of organophosphorus pesticides (chlorpyrifos and malathion). These double stranded calf thymus DNA (dsCT-DNA) entrapped PANI-PVS/indium-tin-oxide (ITO) bioelectrodes have been characterized using square wave voltammetry (SWV), Fourier transform infra-red spectroscopy (FT-IR), scanning electron microscopy (SEM) and electrochemical impedance techniques, respectively. These dsCT-DNA entrapped PANI-PVS/ITO bioelectrodes have been found to have response time of 30 s, stability of about 6 months and detection limit for chlorpyrifos and malathion as 0.5 ppb and 0.01 ppm, respectively

Electrochemical Biosensors - Sensor Principles and Architectures

Science.gov (United States)

Grieshaber, Dorothee; MacKenzie, Robert; Vörös, Janos; Reimhult, Erik

2008-01-01

Quantification of biological or biochemical processes are of utmost importance for medical, biological and biotechnological applications. However, converting the biological information to an easily processed electronic signal is challenging due to the complexity of connecting an electronic device directly to a biological environment. Electrochemical biosensors provide an attractive means to analyze the content of a biological sample due to the direct conversion of a biological event to an electronic signal. Over the past decades several sensing concepts and related devices have been developed. In this review, the most common traditional techniques, such as cyclic voltammetry, chronoamperometry, chronopotentiometry, impedance spectroscopy, and various field-effect transistor based methods are presented along with selected promising novel approaches, such as nanowire or magnetic nanoparticle-based biosensing. Additional measurement techniques, which have been shown useful in combination with electrochemical detection, are also summarized, such as the electrochemical versions of surface plasmon resonance, optical waveguide lightmode spectroscopy, ellipsometry, quartz crystal microbalance, and scanning probe microscopy. The signal transduction and the general performance of electrochemical sensors are often determined by the surface architectures that connect the sensing element to the biological sample at the nanometer scale. The most common surface modification techniques, the various electrochemical transduction mechanisms, and the choice of the recognition receptor molecules all influence the ultimate sensitivity of the sensor. New nanotechnology-based approaches, such as the use of engineered ion-channels in lipid bilayers, the encapsulation of enzymes into vesicles, polymersomes, or polyelectrolyte capsules provide additional possibilities for signal amplification. In particular, this review highlights the importance of the precise control over the delicate

A new application of scanning electrochemical microscopy for the label-free interrogation of antibody-antigen interactions

Energy Technology Data Exchange (ETDEWEB)

Holmes, Joanne L.; Davis, Frank; Collyer, Stuart D. [Cranfield Health, Cranfield University, Cranfield, MK43 0AL (United Kingdom); Higson, Seamus P.J., E-mail: s.p.j.higson@cranfield.ac.uk [Cranfield Health, Cranfield University, Cranfield, MK43 0AL (United Kingdom)

2011-03-18

Within this work we present a 'proof of principle' study for the use of scanning electrochemical microscopy (SECM) to detect and image biomolecular interactions in a label-free assay as a potential alternative to current fluorescence techniques. Screen-printed carbon electrodes were used as the substrate for the deposition of a dotted array, where the dots consist of biotinylated polyethyleneimine. These were then further derivatised, first with neutravidin and then with a biotinylated antibody to the protein neuron specific enolase (NSE). SECM using a ferrocene carboxylic acid mediator showed clear differences between the array and the surrounding unmodified carbon. Imaging of the arrays before and following exposure to various concentrations of the antigen showed clear evidence for specific binding of the NSE antigen to the antibody derivatised dots. Non-specific binding was quantified. Control experiments with other proteins showed only non-specific binding across the whole of the substrate, thereby confirming that specific binding does occur between the antibody and antigen at the surface of the dots. Binding of the antigen was accompanied by a measured increase in current response, which may be explained in terms of protein electrostatic interaction and hydrophobic interactions to the mediator, thereby increasing the localised mediator flux. A calibration curve was obtained between 500 fg mL{sup -1} to 200 pg mL{sup -1} NSE which demonstrated a logarithmic relationship between the current change upon binding and antigen concentration without the need for any labelling of the substrate.

Fabrication and characterization of electrochemically prepared bioanode (polyaniline/ferritin/glucose oxidase) for biofuel cell application

Science.gov (United States)

ul Haque, Sufia; Inamuddin; Nasar, Abu; Asiri, Abdullah M.

2018-01-01

Porous matrix of polyaniline (PANI) has been electrodeposited along with the entrapment of biocompatible redox mediator ferritin (Frt) and glucose oxidase (GOx) on the surface of glassy carbon (GC) electrode. The characterizations have been carried out by X-ray Diffraction (XRD) and Transmission electron microscopy (TEM). The enhanced electrochemical signal transfer rate from enzyme to the electrode surface was due to the intimate contact of the enzyme with the electrochemically polymerized conducting PANI matrix. The PANI/Frt/GOx modified GC bioanode was used to investigate the electrocatalytic activity as a function of the concentration of glucose in the range of 10-60 mM. It was confirmed by the electrochemical impedance spectroscopy (EIS), the thick deposition of PANI layer becomes more compact due to which the charge transfer resistance of PANI matrix becomes higher. All the electrochemical measurements of the electrode were carried out by using cyclic voltammetry (CV) and linear sweep voltammetry (LSV). CV curves were recorded at different scan rates (20-100 mV/s) at 50 mM of glucose in 0.3 M potassium ferrocyanide. A normalized saturation current density of 22.3 ± 2 mA/cm2 was observed for the oxidation of 50 mM glucose at a scan rate of 100 mV/s.

The Electrochemical Behavior of SnSb as an Anode for Li-ion Batteries Studied by Electrochemical Impedance Spectroscopy and Electron Microscopy

International Nuclear Information System (INIS)

Tesfaye, Alexander T.; Yücel, Yasemin D.; Barr, Maïssa K.S.; Santinacci, Lionel; Vacandio, Florence; Dumur, Frédéric; Maria, Sébastien; Monconduit, Laure; Djenizian, Thierry

2017-01-01

Highlights: •Electrochemical behavior of SnSb is investigated by EIS, SEM and TEM. •Formation of SEI and cracks occurs during cycling experiments. •The capacity fading as a result of the electrode modifications is discussed. -- Abstract: Evolution of the electrical and morphological properties of micron-sized SnSb has been investigated to understand the electrochemical behavior observed during cycling experiments. Electron microscopy techniques (scanning electron microscopy and transmission electron microscopy) and electrochemical impedance spectroscopy have been combined to evidence the electrode modifications and particularly the formation of a solid electrolyte interphase (SEI) layer. Evolution of the SEI resistance and the charge transfer resistance with the cell voltage can be explained by the electrolyte degradation and expansion/contraction of the electrode. Furthermore, we show that the SEI formation is not limited at the first discharge/charge of the battery. The continuous growth of the SEI layer up to 50 cycles associated to the electrode pulverization caused by the large volume variations are responsible for the capacity fading.

Electrochemical depth profiling of multilayer metallic structures: An aluminum brazing sheet

International Nuclear Information System (INIS)

Afshar, F. Norouzi; Ambat, R.; Kwakernaak, C.; Wit, J.H.W. de; Mol, J.M.C.; Terryn, H.

2012-01-01

Highlights: ► Localized electrochemical cell and glow discharge optical emission spectrometry were used. ► An electrochemical depth profile of an aluminum brazing sheet was obtained. ► The electrochemical responses were correlated to the microstructural features. - Abstract: Combinatory localized electrochemical cell and glow discharge optical emission spectrometry (GDOES) measurements were performed to obtain a thorough in depth electrochemical characterization of an aluminum brazing sheet. By defining electrochemical criteria i.e. breakdown potential, corrosion potential, cathodic and anodic reactivities, and tracking their changes as a function of depth, the evolution of electrochemical responses through out the material thickness were analyzed and correlated to the corresponding microstructural features. Polarization curves in 1 wt% NaCl solution at pH 2.8 were obtained at different depths from the surface using controlled sputtering in a glow discharge optical emission spectrometer as a sample preparation technique. The anodic and cathodic reactivity of the top surface areas were significantly higher than that of the bulk, thus indicating these areas to be more susceptible to localized attack. Consistent with this, optical microscopy and scanning electron microscope analysis revealed a relatively high density of fine intermetallic and silicon particles at these areas. The corrosion mechanism of the top layers was identified to be intergranular and pitting corrosion, while lower sensitivity to these localized attacks were detected toward the brazing sheet core. The results highlight the successful application of the electrochemical depth profiling approach in prediction of the corrosion behavior of the aluminum brazing sheet and the importance of the electrochemical activity of the outer 10 μm in controlling the corrosion performance of the aluminum brazing sheet.

Electrochemically pretreated zeolite-modified carbon-paste electrodes for determination of linuron in an agricultural formulation and water

International Nuclear Information System (INIS)

Siara, L.R.; Lima, F. de; Cardoso, C.A.L.; Arruda, G.J.

2015-01-01

Highlights: • Cyclic voltammetry, square-wave voltammetry, electrochemical impedance spectroscopic, and scanning electron microscopy were employed. • Kinetic parameters (n, α, k s , and Γ) were calculated. • High sensitivity was observed in the linear concentration range. • Excellent recovery rates were achieved for tap water samples. • The method proved applicable to the determination of linuron in the presence of potential organic and inorganic interferents, none of which affected the results. - Abstract: A simple and inexpensive, yet highly sensitive electrochemical method for quantifying linuron in tap and distilled water and in agricultural formulations was developed using electrochemically pretreated zeolite-modified carbon-paste electrodes (ZMCPEs). Compared with untreated ZMCPEs, the electrochemically pretreated electrodes showed significantly enhanced peak currents for linuron oxidation. Scanning electron microscopy and energy-dispersive x-ray spectroscopy were used to examine the structure of the zeolite-modified and unmodified carbon-paste electrodes (CPEs). ZMCPEs were electrochemically characterized using cyclic voltammetry, chronocoulometry, square-wave voltammetry, and electrochemical impedance spectroscopy. A mechanism for linuron oxidation on ZMCPE surfaces was proposed. The electrochemical variables taken into account were electrode area, number of transferred electrons, electron transfer coefficient, electrode reaction standard rate constant, surface coverage, and capacitance of the electric double layer. Zeolite was found to have a strong influence on these variables. The electrochemical procedure applied to linuron was developed using electrochemically pretreated ZMCPEs under optimal conditions. Linuron oxidation currents exhibited linear concentration in the 87.36 to 625.72 nmol L −1 range, with a limit of detection of 22.57 nmol L −1 . The proposed electrochemical method was employed to quantify linuron in tap and distilled

Composite Electrodes for Electrochemical Supercapacitors

Science.gov (United States)

Li, Jun; Yang, Quan Min; Zhitomirsky, Igor

2010-03-01

Manganese dioxide nanofibers with length ranged from 0.1 to 1 μm and a diameter of about 4-6 nm were prepared by a chemical precipitation method. Composite electrodes for electrochemical supercapacitors were fabricated by impregnation of the manganese dioxide nanofibers and multiwalled carbon nanotubes (MWCNT) into porous Ni plaque current collectors. Obtained composite electrodes, containing 85% of manganese dioxide and 15 mass% of MWCNT, as a conductive additive, with total mass loading of 7-15 mg cm-2, showed a capacitive behavior in 0.5-M Na2SO4 solutions. The decrease in stirring time during precipitation of the nanofibers resulted in reduced agglomeration and higher specific capacitance (SC). The highest SC of 185 F g-1 was obtained at a scan rate of 2 mV s-1 for mass loading of 7 mg cm-2. The SC decreased with increasing scan rate and increasing electrode mass.

Argon plasma treatment to enhance the electrochemical reactivity of screen-printed carbon surfaces

Energy Technology Data Exchange (ETDEWEB)

Ghamouss, F.; Luais, E. [Universite de Nantes, Faculte des Sciences et des Techniques, Chimie et Interdisciplinarite: Synthese, Analyse, Modelisation (CEISAM), UMR CNRS no 6230, 2, rue de la Houssiniere, BP 92208, 44322 NANTES Cedex 3 (France); Universite de Nantes, Institut des Materiaux Jean Rouxel IMN - CNRS, 2 rue de la Houssiniere, BP 32229, 44322 Nantes Cedex 3 (France); Thobie-Gautier, C. [Universite de Nantes, Faculte des Sciences et des Techniques, Chimie et Interdisciplinarite: Synthese, Analyse, Modelisation (CEISAM), UMR CNRS no 6230, 2, rue de la Houssiniere, BP 92208, 44322 NANTES Cedex 3 (France); Tessier, P.-Y. [Universite de Nantes, Faculte des Sciences et des Techniques, Chimie et Interdisciplinarite: Synthese, Analyse, Modelisation (CEISAM), UMR CNRS no 6230, 2, rue de la Houssiniere, BP 92208, 44322 NANTES Cedex 3 (France); Universite de Nantes, Institut des Materiaux Jean Rouxel IMN - CNRS, 2 rue de la Houssiniere, BP 32229, 44322 Nantes Cedex 3 (France); Boujtita, M. [Universite de Nantes, Faculte des Sciences et des Techniques, Chimie et Interdisciplinarite: Synthese, Analyse, Modelisation (CEISAM), UMR CNRS no 6230, 2, rue de la Houssiniere, BP 92208, 44322 NANTES Cedex 3 (France)], E-mail: mohammed.boujtita@univ-nantes.fr

2009-04-15

Radiofrequency argon plasma was used for screen-printed carbon electrodes (SPCE) surface treatment. The cyclic voltammetry of ferri/ferrocyanide as redox couple showed a remarkable improvement of the electrochemical reactivity of the SPCE after the plasma treatment. The effect of the plasma growth conditions on the efficiency of the treatment procedure was evaluated in term of electrochemical reactivity of the SPCE surface. The electrochemical study showed that the electrochemical reactivity of the treated electrodes was strongly dependant on radiofrequency power, treatment time and argon gas pressure. X-ray photoelectron spectroscopy (XPS) analysis showed a considerable evolution on the surface chemistry of the treated electrodes. Our results clearly showed that the argon plasma treatment induces a significant increase in the C{sub sp2}/C{sub sp3} ratio. The scanning electron micrograph (SEM) also showed a drastic change on the surface morphology of the treated SPCEs.

Study on the electrochemical of the metal deposition from ionic liquids for lithium, titanium and dysprosium

International Nuclear Information System (INIS)

Berger, Claudia A.

2017-01-01

The thesis was aimed to the characterization of electrochemically deposited film of lithium, titanium and dysprosium on Au(111) from different ionic liquids, finally dysprosium on neodymium-iron-boron magnate for industrial applications. The investigation of the deposits were performed using cyclic voltametry, in-situ scanning tunneling microscopy, electrochemical quartz microbalance, XPS and Auger electron spectroscopy. The sample preparation is described in detail. The deposition rate showed a significant temperature dependence.

Favoring the unfavored: Selective electrochemical nitrogen fixation using a reticular chemistry approach.

Science.gov (United States)

Lee, Hiang Kwee; Koh, Charlynn Sher Lin; Lee, Yih Hong; Liu, Chong; Phang, In Yee; Han, Xuemei; Tsung, Chia-Kuang; Ling, Xing Yi

2018-03-01

Electrochemical nitrogen-to-ammonia fixation is emerging as a sustainable strategy to tackle the hydrogen- and energy-intensive operations by Haber-Bosch process for ammonia production. However, current electrochemical nitrogen reduction reaction (NRR) progress is impeded by overwhelming competition from the hydrogen evolution reaction (HER) across all traditional NRR catalysts and the requirement for elevated temperature/pressure. We achieve both excellent NRR selectivity (~90%) and a significant boost to Faradic efficiency by 10 percentage points even at ambient operations by coating a superhydrophobic metal-organic framework (MOF) layer over the NRR electrocatalyst. Our reticular chemistry approach exploits MOF's water-repelling and molecular-concentrating effects to overcome HER-imposed bottlenecks, uncovering the unprecedented electrochemical features of NRR critical for future theoretical studies. By favoring the originally unfavored NRR, we envisage our electrocatalytic design as a starting point for high-performance nitrogen-to-ammonia electroconversion directly from water vapor-abundant air to address increasing global demand of ammonia in (bio)chemical and energy industries.

Competitive Dynamics in Micro: Analysis of Perception About Competition in Unitomo Street Food Business

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Bambang Raditya Purnomo

2017-09-01

Full Text Available The purpose of the study this is to explore small and micro businesses in their connections with competitors and the competitive force in the market. This study uses the information processing approach to examine three activities, scanning the competitive environment, the interpretation of competitive actions, and reactions based on that assessment. This research is motivated by the lack of competitiveness of micro businesses, especially those engaged in the culinary field. This study uses qualitative approach with phenomenological methods, in which researchers try to explain or reveal the meaning of a concept or phenomenon of experience based on the awareness that occurs in some individuals. In this study, researchers collect, summarize and interpret the data obtained, which is then processed back in order to obtain a clear, directed and thorough pictures of the problem which become the object of research. Phenomenological approach is used to analyze the original data collected from interview with the informant. Structural interpretation of the experience described by researchers in the description of the participants.

Chemical splitting of multiwalled carbon nanotubes to enhance electrochemical capacitance for supercapacitors

Science.gov (United States)

Li, Xinlu; Li, Tongtao; Zhang, Xinlin; Zhong, Qineng; Li, Hongyi; Huang, Jiamu

2014-06-01

Multiwalled carbon nanotubes (MWCNTs) were chemically split and self-assembled to a flexible porous paper made of graphene oxide nanoribbons (GONRs). The morphology and microstructure of the pristine MWCNTs and GONRs were analyzed by transmission electron microscopy, scanning electron microscopy, X-ray diffraction, Raman spectroscopy and Fourier transform infrared spectroscopy. And the specific surface area and porosity structure were measured by N2 adsorption-desorption. The longitudinally split MWCNTs show an enhancement in specific capacitance from 21 F g-1 to 156 F g-1 compared with the pristine counterpart at 0.1 A g-1 in a 6 M KOH aqueous electrolytes. The electrochemical experiments prove that the chemical splitting of MWCNTs will make inner carbon layers opened and exposed to electrochemical double layers, which can effectively improve the electrochemical capacitance for supercapacitors.

Nanoporous MnO{sub x} thin-film electrodes synthesized by electrochemical lithiation/delithiation for supercapacitors

Energy Technology Data Exchange (ETDEWEB)

Xia, Hui; Lai, Man On; Lu, Li [Department of Mechanical Engineering, National University of Singapore, 9 Engineering Drive 1, Singapore 117576 (Singapore)

2011-02-15

Nanoporous MnO{sub x} thin-film electrodes are synthesized using a combination of pulsed laser deposition (PLD) and electrochemical lithiation/delithiation methods. A dense Mn{sub 3}O{sub 4} thin-film deposited by PLD can transform into a nanoporous MnO{sub x} thin-film after electrochemical lithiation/delithiation. A nanoporous MnO{sub x} thin-film electrode exhibits significantly improved supercapacitive performance compared with an as-deposited Mn{sub 3}O{sub 4} thin-film electrode. A MnO{sub x} thin-film finally transforms into a MnO{sub 2} thin-film through an electrochemical oxidation process during continuous cyclic voltammetry scanning. (author)

A Review of Surface Analysis Techniques for the Investigation of the Phenomenon of Electrochemical Promotion of Catalysis with Alkaline Ionic Conductors

Directory of Open Access Journals (Sweden)

Jesús González-Cobos

2016-01-01

Full Text Available Electrochemical Promotion of Catalysis (EPOC with alkali ionic conductors has been widely studied in literature due to its operational advantages vs. alkali classical promotion. This phenomenon allows to electrochemically control the alkali promoter coverage on a catalyst surface in the course of the catalytic reaction. Along the study of this phenomenon, a large variety of in situ and ex situ surface analysis techniques have been used to investigate the origin and mechanism of this kind of promotion. In this review, we analyze the most important contributions made on this field which have clearly evidenced the presence of adsorbed alkali surface species on the catalyst films deposited on alkaline solid electrolyte materials during EPOC experiments. Hence, the use of different surface analysis techniques such as scanning electron microscopy (SEM, energy-dispersive X-ray spectroscopy (EDX, X-ray diffraction (XRD, X-ray photoelectron spectroscopy (XPS, scanning photoelectron microscopy (SPEM, or scanning tunneling microscopy (STM, led to a better understanding of the alkali promoting effect, and served to confirm the theory of electrochemical promotion on this kind of catalytic systems. Given the functional similarities between alkali electrochemical and chemical promotion, this review aims to bring closer this phenomenon to the catalysis scientific community.

Electrochemical preparation of uniform CuO/Cu2O heterojunction on β-cyclodextrin-modified carbon fibers

KAUST Repository

Chen, Fang-Ping; Jin, Guan-Ping; Su, Jing-Yu; Feng, Xiaoshuang

2016-01-01

materials were characterized by field emission scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and electrochemical techniques. The potential application in pollution treatment

Preparation of the electrochemically formed spinel-lithium manganese oxides

Energy Technology Data Exchange (ETDEWEB)

Katakura, Katsumi; Wada, Kohei; Kajiki, Yoshiyuki; Yamamoto, Akiko [Department of Chemical Engineering, Nara National College of Technology, 22 Yata-cho Yamotokoriyama, Nara 639-1080 (Japan); Ogumi, Zempachi [Graduate School of Engineering, Kyoto University, Nishikyo-ku, Kyoto 615-8510 (Japan)

2009-04-01

Electrochemically formed spinel-lithium manganese oxides were synthesized from manganese hydroxides prepared by a cathodic electrochemical precipitation from various concentrations of manganese nitrate solutions. Two types of manganese hydroxides were formed from diluted and concentrated Mn(NO{sub 3}){sub 2} aqueous solutions. Uniform and equi-sized disk shaped Mn(OH){sub 2} crystals of 0.2-5 {mu}m in diameter were obtained on a Pt substrate after the electrochemical precipitation from lower concentration of ranging from 2 mmol dm{sup -3} to 2 mol dm{sup -3} Mn(NO{sub 3}){sub 2} aq., while the grass blade-like precipitate which is ascribed to manganese hydroxide with 20-80 {mu}m long and 1-5 {mu}m wide were formed from concentrated Mn(NO{sub 3}){sub 2} aq. Both manganese hydroxides gave the electrochemically formed spinel-LiMn{sub 2}O{sub 4} onto a Pt sheet, which is ready for electrochemical measurement, after calcination of the Li incorporated precipitate at 750 C without any additives. While the shape and size of the secondary particle frameworks (aggregates) of the electrochemically formed spinel-LiMn{sub 2}O{sub 4} can be controlled by the electrolysis conditions, the nanostructured primary crystals of 200 nm in diameter were obtained in all cases except that the fiber-like nanostructured spinel-LiMn{sub 2}O{sub 4} crystals with 200 nm in diameter were obtained from concentrated Mn(NO{sub 3}){sub 2} aq. Though these two types of electrochemically formed spinel-LiMn{sub 2}O{sub 4} showed well-shaped CVs even in higher scan rates, it would be suitable for high power density battery applications. These behaviors are assumed to be ascribed to the crystal size and shape of the processed spinel-LiMn{sub 2}O{sub 4}. (author)

Material removal mechanisms in electrochemical-mechanical polishing of tantalum

International Nuclear Information System (INIS)

Gao, F.; Liang, H.

2009-01-01

Material removal mechanisms in tantalum chemical-mechanical polishing (CMP) and electrochemical-mechanical polishing (ECMP) were investigated using the single frequency electrochemical impedance spectroscopy (EIS). Through measuring the impedance of the tantalum surface, the single frequency EIS scan made it possible to observe the CMP and ECMP processes in situ. The impedance results presented competing mechanisms of removal and formation of a surface oxide layer of tantalum. Analysis indicated that the thickness of the oxide layer formed during polishing was related to the mechanical power correlated to the friction force and the rotating speed. Furthermore, the rate of growth and removal of the oxide film was a function of the mechanical power. This understanding is beneficial for optimization of CMP and ECMP processes.

Fabrication, characterization, and functionalization of dual carbon electrodes as probes for scanning electrochemical microscopy (SECM).

Science.gov (United States)

McKelvey, Kim; Nadappuram, Binoy Paulose; Actis, Paolo; Takahashi, Yasufumi; Korchev, Yuri E; Matsue, Tomokazu; Robinson, Colin; Unwin, Patrick R

2013-08-06

Dual carbon electrodes (DCEs) are quickly, easily, and cheaply fabricated by depositing pyrolytic carbon into a quartz theta nanopipet. The size of DCEs can be controlled by adjusting the pulling parameters used to make the nanopipet. When operated in generation/collection (G/C) mode, the small separation between the electrodes leads to reasonable collection efficiencies of ca. 30%. A three-dimensional finite element method (FEM) simulation is developed to predict the current response of these electrodes as a means of estimating the probe geometry. Voltammetric measurements at individual electrodes combined with generation/collection measurements provide a reasonable guide to the electrode size. DCEs are employed in a scanning electrochemical microscopy (SECM) configuration, and their use for both approach curves and imaging is considered. G/C approach curve measurements are shown to be particularly sensitive to the nature of the substrate, with insulating surfaces leading to enhanced collection efficiencies, whereas conducting surfaces lead to a decrease of collection efficiency. As a proof-of-concept, DCEs are further used to locally generate an artificial electron acceptor and to follow the flux of this species and its reduced form during photosynthesis at isolated thylakoid membranes. In addition, 2-dimensional images of a single thylakoid membrane are reported and analyzed to demonstrate the high sensitivity of G/C measurements to localized surface processes. It is finally shown that individual nanometer-size electrodes can be functionalized through the selective deposition of platinum on one of the two electrodes in a DCE while leaving the other one unmodified. This provides an indication of the future versatility of this type of probe for nanoscale measurements and imaging.

Electrochemical Quantification of Extracellular Local H2O2 Kinetics Originating from Single Cells.

Science.gov (United States)

Bozem, Monika; Knapp, Phillip; Mirčeski, Valentin; Slowik, Ewa J; Bogeski, Ivan; Kappl, Reinhard; Heinemann, Christian; Hoth, Markus

2017-05-15

H 2 O 2 is produced by all eukaryotic cells under physiological and pathological conditions. Due to its enormous relevance for cell signaling at low concentrations and antipathogenic function at high concentrations, precise quantification of extracellular local H 2 O 2 concentrations ([H 2 O 2 ]) originating from single cells is required. Using a scanning electrochemical microscope and bare platinum disk ultramicroelectrodes, we established sensitive long-term measurements of extracellular [H 2 O 2 ] kinetics originating from single primary human monocytes (MCs) ex vivo. For the electrochemical techniques square wave voltammetry, cyclic and linear scan voltammetry, and chronoamperometry, detection limits for [H 2 O 2 ] were determined to be 5, 50, and 500 nM, respectively. Following phorbol ester stimulation, local [H 2 O 2 ] 5-8 μm above a single MC increased by 3.4 nM/s within the first 10 min before reaching a plateau. After extracellular addition of H 2 O 2 to an unstimulated MC, the local [H 2 O 2 ] decreased on average by 4.2 nM/s due to degradation processes of the cell. Using the scanning mode of the setup, we found that H 2 O 2 is evenly distributed around the producing cell and can still be detected up to 30 μm away from the cell. The electrochemical single-cell measurements were validated in MC populations using electron spin resonance spectroscopy and the Amplex ® UltraRed assay. Innovation and Conclusion: We demonstrate a highly sensitive, spatially, and temporally resolved electrochemical approach to monitor dynamics of production and degradation processes for H 2 O 2 separately. Local extracellular [H 2 O 2 ] kinetics originating from single cells is quantified in real time. Antioxid. Redox Signal. 00, 000-000.

Carbon-fiber tips for scanning probe microscopes and molecular electronics experiments

NARCIS (Netherlands)

Rubio-Bollinger, G.; Castellanos-Gomez, A.; Bilan, S.; Zotti, L.A.; Arroyo, C.R.; Agraït, N.; Cuevas, J.

2012-01-01

We fabricate and characterize carbon-fiber tips for their use in combined scanning tunneling and force microscopy based on piezoelectric quartz tuning fork force sensors. An electrochemical fabrication procedure to etch the tips is used to yield reproducible sub-100-nm apex. We also study electron

Optical and electrochemical studies of polyaniline/SnO{sub 2} fibrous nanocomposites

Energy Technology Data Exchange (ETDEWEB)

Manivel, P. [Department of Nanoscience and Technology, Bharathiar University, Coimbatore 641 046, Tamil Nadu (India); Ramakrishnan, S.; Kothurkar, Nikhil K. [Department of Chemical Engineering and Material Science, Amrita Vishwa Vidyapeetham, Coimbatore 641 112, Tamil Nadu (India); Balamurugan, A.; Ponpandian, N.; Mangalaraj, D. [Department of Nanoscience and Technology, Bharathiar University, Coimbatore 641 046, Tamil Nadu (India); Viswanathan, C., E-mail: viswanathan@buc.edu.in [Department of Nanoscience and Technology, Bharathiar University, Coimbatore 641 046, Tamil Nadu (India)

2013-02-15

Graphical abstract: Fiber with porous like structure of PANI/SnO{sub 2} nanocomposites were prepared by simplest in situ chemical polymerization method. The PL emission spectra revealed that the band from 404 and 436 nm which is related with oxygen vacancies. The excellent electrochemical properties of composite electrode show the specific capacitance of 173 F/g at a scan rate of 25 m V/s. Display Omitted Highlights: ► Self assembled PANI/SnO{sub 2} nanocomposites were synthesized by simple polymerization method. ► Electrochemical behavior of PANI/SnO{sub 2} nanocomposites electrode was analyzed by CV. ► Nanocomposites exhibit a higher specific capacitance of 173 F/g, compared with pure SnO{sub 2}. -- Abstract: Polyaniline (PANI)/tin oxide (SnO{sub 2}) fibrous nanocomposites were successfully prepared by an in situ chemical polymerization method with suitable conditions. The obtained composites were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy, photoluminescence (PL), electrical conductivity and cyclic voltammetry studies (CV). The XRD pattern of the as-prepared sample shows the presence of tetragonal SnO{sub 2} and the crystalline structure of SnO{sub 2} was not affected with the incorporation of PANI. The FTIR analysis confirms the uniform attachment of PANI on the surface of SnO{sub 2} nanostructures. SEM images show a fibrous agglomerated structure of PANI/SnO{sub 2}. The PL emission spectra revealed that the band from 404 and 436 nm which is related with oxygen vacancies. The electrochemical behavior of the PANI/SnO{sub 2} composite electrode was evaluated in a H{sub 2}SO{sub 4} solution using cyclic voltammetry. The composite electrode exhibited a specific capacitance of 173 F/g at a scan rate 25 mV/s. Thus the as-prepared PANI/SnO{sub 2} composite shows excellent electrochemical properties, suggesting that this composite is a promising material for supercapacitors.

Dual responsive supramolecular hydrogel with electrochemical activity.

Science.gov (United States)

Du, Ping; Liu, Jianghua; Chen, Guosong; Jiang, Ming

2011-08-02

Supramolecular materials with reversible responsiveness to environmental changes are of particular research interest in recent years. Inclusion complexation between cyclodextrin (CD) and ferrocene (Fc) is well-known and extensively studied because of its reversible association-dissociation controlled by the redox state of Fc. Although there are quite a few reported nanoscale materials incorporating this host-guest pair, polymeric hydrogels with electrochemical activity based on this interactive pair are still rare. Taking advantage of our previous reported hybrid inclusion complex (HIC) hydrogel structure, a new Fc-HIC was designed and obtained with β-CD-modified quantum dots as the core and Fc-ended diblock co-polymer p(DMA-b-NIPAM) as the shell, to achieve an electrochemically active hydrogel at elevated temperatures. Considering the two independent cross-linking strategies in the network structure, i.e., the interchain aggregation of pNIPAM and inclusion complexation between CD and Fc on the surface of the quantum dots, the hydrogel was fully thermo-reversible and its gel-sol transition was achieved after the addition of either an oxidizing agent or a competitive guest to Fc.

Fabrication and electrochemical properties of free-standing single-walled carbon nanotube film electrodes

International Nuclear Information System (INIS)

Niu Zhi-Qiang; Ma Wen-Jun; Dong Hai-Bo; Li Jin-Zhu; Zhou Wei-Ya

2011-01-01

An easily manipulative approach was presented to fabricate electrodes using free-standing single-walled carbon nanotube (SWCNT) films grown directly by chemical vapor deposition. Electrochemical properties of the electrodes were investigated. In comparison with the post-deposited SWCNT papers, the directly grown SWCNT film electrodes manifested enhanced electrochemical properties and sensitivity of sensors as well as excellent electrocatalytic activities. A transition from macroelectrode to nanoelectrode behaviours was observed with the increase of scan rate. The heat treatment of the SWCNT film electrodes increased the current signals of electrochemical analyser and background current, because the heat-treatment of the SWCNTs in air could create more oxide defects on the walls of the SWCNTs and make the surfaces of SWCNTs more hydrophilic. The excellent electrochemical properties of the directly grown and heat-treated free-standing SWCNT film electrodes show the potentials in biological and electrocatalytic applications. (cross-disciplinary physics and related areas of science and technology)

Investigation on Electrochemical Properties of Polythiophene Nanocomposite with Graphite Derivatives as Supercapacitor Material on Breath Figure-Decorated PMMA Electrode

Science.gov (United States)

Azimi, Mona; Abbaspour, Mohsen; Fazli, Ali; Setoodeh, Hamideh; Pourabbas, Behzad

2018-03-01

Breath figures have been formed by the direct breath figure method on polymethyl methacrylate electrode sand hexagonal oriented holes with 0.5- to 10- μm2 surface area have been created. Deposition of materials on the electrodes has been performed by the spray-coating method. polythiophene (PTh) nanoparticles, polythiophene-graphene oxide (PTh-GO) and polythiophene-reduced graphene oxide (PTh-G) nanocomposites were synthesized by emulsion polymerization, while characterization of synthetic materials have been carried out by Fourier transform infrared, Χ-ray diffraction, transmission electron microscopy, UV-Vis spectroscopy and field emission scanning electron microscopy techniques. Also, the electrochemical properties of the designed electrodes were investigated by cyclic voltammetry, galvanostatic charge-discharge and electrochemical impedance spectroscopy techniques. Specific capacitance of porous electrodes coated by PTh nanoparticles, PTh-GO and PTh-G nanocomposites were calculated from cyclic voltammetry curves at 5 mV/s scan rate, andthe values are 3.5 F/g, 16.39 F/g, and 28.68 F/g, respectively. Also, the energy density of each electrode at 5 mV/s scan rate has been calculated and the results show that incorporation of GO and G nanolayers with PTh nanoparticles enhances the electrochemical properties of electrodes.

Electrochemical and Corrosion Properties of Aluminum Brass in Seawater Desalination Environments

Directory of Open Access Journals (Sweden)

Hong JU

2017-11-01

Full Text Available The corrosion behavior and mechanism of aluminum brass (HAl77-2 in seawater desalination plant were investigated using electrochemical measurement, Scanning Electronic Microscope (SEM and Energy Dispersive X-ray spectroscopy (EDX analysis. The electrochemical results revealed that the corrosion of HAl77-2 in the desalination artificial seawater depended on chloride ion concentrations, displaying a maximum with a chloride ion concentration of 2.3 wt.%. Corrosion rate of HAl77-2 initial increased and subsequently decreased with the increasing of chloride ion concentration. Moreover, corrosion of HAl77-2 becomes more severe when temperature rises. The above results obtained by electrochemical impedance spectroscopy and potentiodynamic polarization tests were in a good agreement. The results of SEM and EDX methods showed selective localized corrosion appeared remarkably on the surface of HAl77-2.DOI: http://dx.doi.org/10.5755/j01.ms.23.4.17170

Composite Electrodes for Electrochemical Supercapacitors

Directory of Open Access Journals (Sweden)

Yang QuanMin

2010-01-01

Full Text Available Abstract Manganese dioxide nanofibers with length ranged from 0.1 to 1 μm and a diameter of about 4–6 nm were prepared by a chemical precipitation method. Composite electrodes for electrochemical supercapacitors were fabricated by impregnation of the manganese dioxide nanofibers and multiwalled carbon nanotubes (MWCNT into porous Ni plaque current collectors. Obtained composite electrodes, containing 85% of manganese dioxide and 15 mass% of MWCNT, as a conductive additive, with total mass loading of 7–15 mg cm−2, showed a capacitive behavior in 0.5-M Na2SO4 solutions. The decrease in stirring time during precipitation of the nanofibers resulted in reduced agglomeration and higher specific capacitance (SC. The highest SC of 185 F g−1 was obtained at a scan rate of 2 mV s−1 for mass loading of 7 mg cm−2. The SC decreased with increasing scan rate and increasing electrode mass.

One-step electrochemical synthesis of a graphene–ZnO hybrid for improved photocatalytic activity

International Nuclear Information System (INIS)

Wei, Ang; Xiong, Li; Sun, Li; Liu, Yanjun; Li, Weiwei; Lai, Wenyong; Liu, Xiangmei; Wang, Lianhui; Huang, Wei; Dong, Xiaochen

2013-01-01

Graphical abstract: - Highlights: • Graphene–ZnO hybrid was synthesized by one-step electrochemical deposition. • Graphene–ZnO hybrid presents a special structure and wide UV–vis absorption spectra. • Graphene–ZnO hybrid exhibits an exceptionally higher photocatalytic activity for the degradation of dye methylene blue. - Abstract: A graphene–ZnO (G-ZnO) hybrid was synthesized by one-step electrochemical deposition. During the formation of ZnO nanostructure by cathodic electrochemical deposition, the graphene oxide was electrochemically reduced to graphene simultaneously. Scanning electron microscope images, X-ray photoelectron spectroscopy, X-ray diffraction, Raman spectra, and UV–vis absorption spectra indicate the resulting G-ZnO hybrid presents a special structure and wide UV–vis absorption spectra. More importantly, it exhibits an exceptionally higher photocatalytic activity for the degradation of dye methylene blue than that of pure ZnO nanostructure under both ultraviolet and sunlight irradiation

Electrochemical capacitance performance of titanium nitride nanoarray

Energy Technology Data Exchange (ETDEWEB)

Xie, Yibing, E-mail: ybxie@seu.edu.cn [School of Chemistry and Chemical Engineering, Southeast University, Nanjing 211189 (China); Suzhou Research Institute of Southeast University, Suzhou 215123 (China); Wang, Yong [School of Chemistry and Chemical Engineering, Southeast University, Nanjing 211189 (China); Du, Hongxiu [School of Chemistry and Chemical Engineering, Southeast University, Nanjing 211189 (China); Suzhou Research Institute of Southeast University, Suzhou 215123 (China)

2013-12-01

Highlights: • TiN nanoarray is formed by a nitridation process of TiO{sub 2} in ammonia atmosphere. • TiN nanoarray exhibits much higher EDLC capacitance than TiO{sub 2} nanoarray. • The specific capacitance of TiN nanoarray achieves a high level of 99.7 mF cm{sup −2}. • A flexible solid-state supercapacitor is constructed by TiN nanoarray and PVA gel. -- Abstract: In this study, titanium nitride (TiN) nanoarrays with a short nanotube and long nanopore structure have been prepared by an anodization process of ultra thin titanium foil in ethylene glycol (EG) solution containing ammonium fluoride, subsequent calcination process in an air atmosphere, and final nitridation process in an ammonia atmosphere. The morphology and microstructure characterization has been conducted using field emission scanning electron microscope and X-ray diffraction. The electrochemical properties have been investigated through cyclic voltammetry and electrochemical impedance spectrum measurements. The electrochemical capacitance performance has been investigated by galvanostatic charge–discharge measurements in the acidic, neural and alkali electrolyte solution. Well-defined TiN nanoarrays contribute a much higher capacitance performance than titania (TiO{sub 2}) in the supercapacitor application due to the extraordinarily improved electrical conductivity. Such an electrochemical capacitance can be further enhanced by increasing aspect ratio of TiN nanoarray from short nanotubes to long nanopores. A flexible supercapacitor has been constructed using two symmetrical TiN nanoarray electrodes and a polyvinyl alcohol (PVA) gel electrolyte with H{sub 2}SO{sub 4}–KCl–H{sub 2}O–EG. Such a supercapacitor has a highly improved potential window and still keeps good electrochemical energy storage. TiN nanoarray with a high aspect ratio can act well as an ultra thin film electrode material of flexible supercapacitor to contribute a superior capacitance performance.

Electrochemical Biosensors - Sensor Principles and Architectures

Directory of Open Access Journals (Sweden)

Erik Reimhult

2008-03-01

Full Text Available Quantification of biological or biochemical processes are of utmost importancefor medical, biological and biotechnological applications. However, converting the biologicalinformation to an easily processed electronic signal is challenging due to the complexity ofconnecting an electronic device directly to a biological environment. Electrochemical biosensorsprovide an attractive means to analyze the content of a biological sample due to thedirect conversion of a biological event to an electronic signal. Over the past decades severalsensing concepts and related devices have been developed. In this review, the most commontraditional techniques, such as cyclic voltammetry, chronoamperometry, chronopotentiometry,impedance spectroscopy, and various field-effect transistor based methods are presented alongwith selected promising novel approaches, such as nanowire or magnetic nanoparticle-basedbiosensing. Additional measurement techniques, which have been shown useful in combinationwith electrochemical detection, are also summarized, such as the electrochemical versionsof surface plasmon resonance, optical waveguide lightmode spectroscopy, ellipsometry,quartz crystal microbalance, and scanning probe microscopy.The signal transduction and the general performance of electrochemical sensors are often determinedby the surface architectures that connect the sensing element to the biological sampleat the nanometer scale. The most common surface modification techniques, the various electrochemicaltransduction mechanisms, and the choice of the recognition receptor moleculesall influence the ultimate sensitivity of the sensor. New nanotechnology-based approaches,such as the use of engineered ion-channels in lipid bilayers, the encapsulation of enzymesinto vesicles, polymersomes, or polyelectrolyte capsules provide additional possibilities forsignal amplification.In particular, this review highlights the importance of the precise control over the

In-situ electrochemical coating of Ag nanoparticles onto graphite electrode with enhanced performance for Li-ion batteries

International Nuclear Information System (INIS)

Yun, Jiaojiao; Wang, Yan; Gao, Tian; Zheng, Huiyuan; Shen, Ming; Qu, Qunting; Zheng, Honghe

2015-01-01

The effects of silver hexafluorophosphate (AgPF 6 ) as an electrolyte additive on the electrochemical behaviors of graphite anode are systematically studied by cyclic voltammetry, galvanostatic charge-discharge, and electrochemical impedance spectroscopy. The surface structure and composition of graphite electrode after electrochemical cycles are investigated through scanning electron microscopy, X-ray diffraction, energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy. It is found that Ag nanoparticles derived from electrochemical reduction of Ag + are homogenously distributed on the graphite surface. Significant improvements on the discharge capacity, rate behavior, and low-temperature performance of graphite electrode are obtained. The reasons are associated with the decreased resistances of solid-electrolyte interface and charge-transfer process, which improve the electrode kinetics for Li + intercalation/deintercalation

Electrochemical Dissolution of Iridium and Iridium Oxide Particles in Acidic Media: Transmission Electron Microscopy, Electrochemical Flow Cell Coupled to Inductively Coupled Plasma Mass Spectrometry, and X-ray Absorption Spectroscopy Study.

Science.gov (United States)

Jovanovič, Primož; Hodnik, Nejc; Ruiz-Zepeda, Francisco; Arčon, Iztok; Jozinović, Barbara; Zorko, Milena; Bele, Marjan; Šala, Martin; Šelih, Vid Simon; Hočevar, Samo; Gaberšček, Miran

2017-09-13

Iridium-based particles, regarded as the most promising proton exchange membrane electrolyzer electrocatalysts, were investigated by transmission electron microscopy and by coupling of an electrochemical flow cell (EFC) with online inductively coupled plasma mass spectrometry. Additionally, studies using a thin-film rotating disc electrode, identical location transmission and scanning electron microscopy, as well as X-ray absorption spectroscopy have been performed. Extremely sensitive online time-and potential-resolved electrochemical dissolution profiles revealed that Ir particles dissolve well below oxygen evolution reaction (OER) potentials, presumably induced by Ir surface oxidation and reduction processes, also referred to as transient dissolution. Overall, thermally prepared rutile-type IrO 2 particles are substantially more stable and less active in comparison to as-prepared metallic and electrochemically pretreated (E-Ir) analogues. Interestingly, under OER-relevant conditions, E-Ir particles exhibit superior stability and activity owing to the altered corrosion mechanism, where the formation of unstable Ir(>IV) species is hindered. Due to the enhanced and lasting OER performance, electrochemically pre-oxidized E-Ir particles may be considered as the electrocatalyst of choice for an improved low-temperature electrochemical hydrogen production device, namely a proton exchange membrane electrolyzer.

Electrochemical extraction of samarium from molten chlorides in pyrochemical processes

International Nuclear Information System (INIS)

Castrillejo, Y.; Fernandez, P.; Medina, J.; Hernandez, P.; Barrado, E.

2011-01-01

This work concerns the electrochemical extraction of samarium from molten chlorides. In this way, the electrochemical behaviour of samarium ions has been investigated in the eutectic LiCl-KCl at the surface of tungsten, aluminium and aluminium coated tungsten electrodes. On a W inert electrode the electro-reduction of Sm(III) takes place in only one soluble-soluble electrochemical step Sm(III)/Sm(II). The electrochemical system Sm(II)/Sm(0) has not been observed within the electrochemical window, because of the prior reduction of Li(I) ions from the solvent, which inhibits the electro-extraction of Sm species from the salt on such a substrate. Sm metal in contact with the melt react to give Li(0) according to the reaction: Sm(0) + 2Li(I) ↔ Sm(II) + 2Li(0). On the contrary, on reactive Al electrodes the electrochemical system Sm(II)/Sm(0) was observed within the electroactive range. The potential shift of the redox couple is caused by the decrease of Sm activity in the metal phase due to the formation of Sm-Al alloys at the interface. The formation mechanism of the intermetallic compounds was studied in a melt containing: (i) both Sm(III) and Al(III) ions, using W and Al coated tungsten electrodes, and (ii) Sm(III) ions using an Al electrode. Analysis of the samples after potentiostatic electrolysis by X-ray diffraction and scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDS), allowed the identification of Al 3 Sm and Al 2 Sm.

Electrochemical extraction of samarium from molten chlorides in pyrochemical processes

Energy Technology Data Exchange (ETDEWEB)

Castrillejo, Y., E-mail: ycastril@qa.uva.es [QUIANE/Dept Quimica Analitica, F. de Ciencias, Universidad de Valladolid, Prado de la Magdalena s/n, 47005 Valladolid (Spain); Fernandez, P. [QUIANE/Dept Quimica Analitica, F. de Ciencias, Universidad de Valladolid, Prado de la Magdalena s/n, 47005 Valladolid (Spain); Medina, J. [Dept Fisica Materia Condensada Cristalografia y Mineralogia, F. de Ciencias, Universidad de Valladolid, Prado de la Magdalena s/n, 47005 Valladolid (Spain); Hernandez, P. [Centro de Investigaciones Quimicas, Universidad Autonoma del Estado de Hidalgo, Carr. Pachuca-Tulancingo Km. 4.5, C.P. 42076 Pachuca, Hidalgo (Mexico); Barrado, E. [QUIANE/Dept Quimica Analitica, F. de Ciencias, Universidad de Valladolid, Prado de la Magdalena s/n, 47005 Valladolid (Spain)

2011-10-01

This work concerns the electrochemical extraction of samarium from molten chlorides. In this way, the electrochemical behaviour of samarium ions has been investigated in the eutectic LiCl-KCl at the surface of tungsten, aluminium and aluminium coated tungsten electrodes. On a W inert electrode the electro-reduction of Sm(III) takes place in only one soluble-soluble electrochemical step Sm(III)/Sm(II). The electrochemical system Sm(II)/Sm(0) has not been observed within the electrochemical window, because of the prior reduction of Li(I) ions from the solvent, which inhibits the electro-extraction of Sm species from the salt on such a substrate. Sm metal in contact with the melt react to give Li(0) according to the reaction: Sm(0) + 2Li(I) {r_reversible} Sm(II) + 2Li(0). On the contrary, on reactive Al electrodes the electrochemical system Sm(II)/Sm(0) was observed within the electroactive range. The potential shift of the redox couple is caused by the decrease of Sm activity in the metal phase due to the formation of Sm-Al alloys at the interface. The formation mechanism of the intermetallic compounds was studied in a melt containing: (i) both Sm(III) and Al(III) ions, using W and Al coated tungsten electrodes, and (ii) Sm(III) ions using an Al electrode. Analysis of the samples after potentiostatic electrolysis by X-ray diffraction and scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDS), allowed the identification of Al{sub 3}Sm and Al{sub 2}Sm.

Influence of fabrication procedure on the electrochemical performance of Ag/AgCl reference electrodes

Energy Technology Data Exchange (ETDEWEB)

Stoica, Daniela [Department of Biomedical and Inorganic Chemistry, Laboratoire National de Metrologie et d' Essais, 1 Rue Gaston Boissier, 75015 Paris (France); Brewer, Paul J., E-mail: paul.brewer@npl.co.uk [Analytical Science Division, National Physical Laboratory, Teddington, Middlesex TW11 0LW (United Kingdom); Brown, Richard J.C. [Analytical Science Division, National Physical Laboratory, Teddington, Middlesex TW11 0LW (United Kingdom); Fisicaro, Paola [Department of Biomedical and Inorganic Chemistry, Laboratoire National de Metrologie et d' Essais, 1 Rue Gaston Boissier, 75015 Paris (France)

2011-11-30

The influence of several parameters in the preparation procedure of thermal-electrolytic Ag/AgCl electrodes on the resulting electrode performance has been studied. In particular, we report the effect on electrode performance of subtle variations in the preparation of silver oxide paste used for electrode manufacture, in thermal annealing conditions employed and in the procedure for electrochemically converting a fraction of the electrode from silver to silver chloride. Scanning electron microscopy and electrochemical impedance spectroscopy have been used to study the characteristics of the electrodes produced. This work reveals a correlation between the electrochemical behaviour and surface physical characteristics - in particular electrode porosity. The outputs of this study have positive implications for improving the accuracy and comparability of primary pH measurement.

Zn2+-Doped Polyaniline/Graphene Oxide as Electrode Material for Electrochemical Supercapacitors

Science.gov (United States)

Xu, Hui; Tang, Jing; Chen, Yong; Liu, Jian; Pu, Jinjuan; Li, Qi

2017-10-01

Electrodes based on Zn2+-doped polyaniline/graphene oxide (Zn2+/PANI/GO) were synthesized on stainless steel mesh substrates in H2SO4 solution via electrochemical codeposition. Different concentrations of graphene oxide (GO) were incorporated into the films to improve the electrochemical performance of the electrodes. Electrochemical properties of the films were tested by cyclic voltammetry, galvanostatic charge-discharge tests, and electrochemical impedance spectroscopy, in a three-electrode system. The maximum specific capacitance of the Zn2+/PANI/GO film with a GO concentration of 15 mg L-1 was found to be 1266 F g-1 at a scan rate of 3 mV s-1. This value was higher than that of a Zn2+ doped polyaniline (Zn2+/PANI) film (814 F g-1). The Zn2+/PANI/GO film also showed good cycling stability, retaining over 86% of its initial capacitance after 1000 cycles. These results indicate that the Zn2+/PANI/GO composites can be applied as high performance supercapacitor electrodes.

Degradation of all-vanadium redox flow batteries (VRFB) investigated by electrochemical impedance and X-ray photoelectron spectroscopy: Part 2 electrochemical degradation

Science.gov (United States)

Derr, Igor; Bruns, Michael; Langner, Joachim; Fetyan, Abdulmonem; Melke, Julia; Roth, Christina

2016-09-01

Electrochemical degradation (ED) of carbon felt electrodes was investigated by cycling of a flow through all-vanadium redox flow battery (VRFB) and conducting half-cell measurements with two reference electrodes inside the test bench. ED was detected using half-cell and full-cell electrochemical impedance spectroscopy (EIS) at different states of charge (SOC). Reversing the polarity of the battery to recover cell performance was performed with little success. Renewing the electrolyte after a certain amount of cycles restored the capacity of the battery. X-ray photoelectron spectroscopy (XPS) reveals that the amount of surface functional increases by more than a factor of 3 for the negative side as well as for the positive side. Scanning electron microscope (SEM) images show a peeling of the fiber surface after cycling the felts, which leads to a loss of electrochemically active surface area (ECSA). Long term cycling shows that ED has a stronger impact on the negative half-cell [V(II)/V(III)] than the positive half-cell [V(IV)/V(V)] and that the negative half-cell is the rate-determining half-cell for the VRFB.

Quasi-steady-state voltammetry of rapid electron transfer reactions at the macroscopic substrate of the scanning electrochemical microscope.

Science.gov (United States)

Nioradze, Nikoloz; Kim, Jiyeon; Amemiya, Shigeru

2011-02-01

We report on a novel theory and experiment for scanning electrochemical microscopy (SECM) to enable quasi-steady-state voltammetry of rapid electron transfer (ET) reactions at macroscopic substrates. With this powerful approach, the substrate potential is cycled widely across the formal potential of a redox couple while the reactant or product of a substrate reaction is amperometrically detected at the tip in the feedback or substrate generation/tip collection mode, respectively. The plot of tip current versus substrate potential features the retraceable sigmoidal shape of a quasi-steady-state voltammogram although a transient voltammogram is obtained at the macroscopic substrate. Finite element simulations reveal that a short tip-substrate distance and a reversible substrate reaction (except under the tip) are required for quasi-steady-state voltammetry. Advantageously, a pair of quasi-steady-state voltammograms is obtained by employing both operation modes to reliably determine all transport, thermodynamic, and kinetic parameters as confirmed experimentally for rapid ET reactions of ferrocenemethanol and 7,7,8,8-tetracyanoquinodimethane at a Pt substrate with ∼0.5 μm-radius Pt tips positioned at 90 nm-1 μm distances. Standard ET rate constants of ∼7 cm/s were obtained for the latter mediator as the largest determined for a substrate reaction by SECM. Various potential applications of quasi-steady-state voltammetry are also proposed.

Evaluation of toughness deterioration by an electrochemical method in an isothermally-aged N-containing austenitic stainless steel

International Nuclear Information System (INIS)

Saucedo-Munoz, Maribel L.; Lopez-Hirata, Victor M.; Avila-Davila, Erika O.; Melo-Maximo, Dulce V.

2009-01-01

This work presents the results of an evaluation of the deterioration of cryogenic toughness by means of an electrochemical method in a N-containing austenitic stainless steel (JK2) aged at temperatures of 700, 800 and 900 deg. C for times from 10 to 1000 min. The aging process at 700 and 800 deg. C caused the decrease in the Charpy V-Notch impact energy at - 196 deg. C because of the intergranular precipitation of carbides. Scanning electron micrographs of the Charpy V-Notch test specimens showed the presence of intergranular brittle fracture. The degree of sensitization was determined by the ratio of the maximum current density generated by the reactivation scan to that of the anodic scan, I r /I a , using the double-loop electrochemical potentiokinetic reactivation test. The Charpy V-Notch impact energy decreased with increase in the I r /I a ratio. This relation permits an estimate of the deterioration of cryogenic toughness due to thermal aging in this type of steel

Electrochemical Oxidation of Glycerol Using Gold Electrode

International Nuclear Information System (INIS)

Mohamed Rozali Othman; Amirah Ahmad

2015-01-01

Cyclic voltammetry, potential linear V and chronocuolometry methods were carried out to gain electrochemical behavior of glycerol at a gold electrode. Potassium hydroxide and sulfuric acid were chosen to be the electrolyte for the electro-oxidation of this organic compound. Besides gold plate electrode, gold composite electrode (Au-PVC) was also used as the working electrode. The Au-PVC composite electrode was characterized by Scanning Electron Microscopy (SEM) to determine its morphological aspects before and after used in electrochemical oxidation of glycerol. In alkaline solution, the adsorption of hydroxide species onto the surface of both gold plate and composite Au-PVC electrodes occurs at potential around 500 mV vs SCE. However, at gold plate electrode, there was a small, broad peak before the drastic escalation of current densities which indicates the charge transfer of the chemisorbed OH - anion. In acidic media, the gold oxide was formed after potential 1.0 V. From the cyclic voltammogram glycerol undergo oxidation twice in potassium hydroxide at gold plate and Au-PVC composite electrodes, while in sulfuric acid, oxidation reaction happened once for glycerol on the gold plate electrode. Overall, electrochemical oxidation of glycerol was more effective in alkaline media. Tafel graph which plotted from potential linear V method shows that Au-PVC composite electrode is better than gold plate electrode for the electro-oxidation of glycerol in alkaline solution. Electrochemical oxidation of glycerol products as analyzed by Gas Chromatography-Mass Spectrometry (GC-MS) produced several carboxylic acids and phenolic compounds. (author)

Characterization of electrochemically modified polycrystalline platinum surfaces

Energy Technology Data Exchange (ETDEWEB)

Krebs, L.C.; Ishida, Takanobu.

1991-12-01

The characterization of electrochemically modified polycrystalline platinum surfaces has been accomplished through the use of four major electrochemical techniques. These were chronoamperometry, chronopotentiommetry, cyclic voltammetry, and linear sweep voltammetry. A systematic study on the under-potential deposition of several transition metals has been performed. The most interesting of these were: Ag, Cu, Cd, and Pb. It was determined, by subjecting the platinum electrode surface to a single potential scan between {minus}0.24 and +1.25 V{sub SCE} while stirring the solution, that the electrocatalytic activity would be regenerated. As a consequence of this study, a much simpler method for producing ultra high purity water from acidic permanganate has been developed. This method results in water that surpasses the water produced by pyrocatalytic distillation. It has also been seen that the wettability of polycrystalline platinum surfaces is greatly dependent on the quantity of oxide present. Oxide-free platinum is hydrophobic and gives a contact angle in the range of 55 to 62 degrees. We have also modified polycrystalline platinum surface with the electrically conducting polymer poly-{rho}-phenylene. This polymer is very stable in dilute sulfuric acid solutions, even under applied oxidative potentials. It is also highly resistant to electrochemical hydrogenation. The wettability of the polymer modified platinum surface is severely dependent on the choice of supporting electrolyte chosen for the electrochemical polymerization. Tetraethylammonium tetrafluoroborate produces a film that is as hydrophobic as Teflon, whereas tetraethylammonium perchlorate produces a film that is more hydrophilic than oxide-free platinum.

Characterization of electrochemically modified polycrystalline platinum surfaces

Energy Technology Data Exchange (ETDEWEB)

Krebs, Leonard C. [State Univ. of New York (SUNY), Stony Brook, NY (United States); Ishida, Takanobu [State Univ. of New York (SUNY), Stony Brook, NY (United States)

1991-12-01

The characterization of electrochemically modified polycrystalline platinum surfaces has been accomplished through the use of four major electrochemical techniques. These were chronoamperometry, chronopotentiommetry, cyclic voltammetry, and linear sweep voltammetry. A systematic study on the under-potential deposition of several transition metals has been performed. The most interesting of these were: Ag, Cu, Cd, and Pb. It was determined, by subjecting the platinum electrode surface to a single potential scan between -0.24 and +1.25 V_SCE while stirring the solution, that the electrocatalytic activity would be regenerated. As a consequence of this study, a much simpler method for producing ultra high purity water from acidic permanganate has been developed. This method results in water that surpasses the water produced by pyrocatalytic distillation. It has also been seen that the wettability of polycrystalline platinum surfaces is greatly dependent on the quantity of oxide present. Oxide-free platinum is hydrophobic and gives a contact angle in the range of 55 to 62 degrees. We have also modified polycrystalline platinum surface with the electrically conducting polymer poly-ρ-phenylene. This polymer is very stable in dilute sulfuric acid solutions, even under applied oxidative potentials. It is also highly resistant to electrochemical hydrogenation. The wettability of the polymer modified platinum surface is severely dependent on the choice of supporting electrolyte chosen for the electrochemical polymerization. Tetraethylammonium tetrafluoroborate produces a film that is as hydrophobic as Teflon, whereas tetraethylammonium perchlorate produces a film that is more hydrophilic than oxide-free platinum.

Flexible Pillared Graphene-Paper Electrodes for High-Performance Electrochemical Supercapacitors

Energy Technology Data Exchange (ETDEWEB)

Wang, Gongkai; Sun, Xiang; Lu, Fengyuan; Sun, Hongtao; Yu, Mingpeng; Jiang, Weilin; Liu, Changsheng; Lian, Jie

2011-12-08

Flexible graphene paper (GP) pillared by carbon black (CB) nanoparticles using a simple vacuum filtration method is developed as a high-performance electrode material for supercapacitors. Through the introduction of CB nanoparticles as spacers, the self-restacking of graphene sheets during the filtration process is mitigated to a great extent. The pillared GP-based supercapacitors exhibit excellent electrochemical performances and cyclic stabilities compared with GP without the addition of CB nanoparticles. At a scan rate of 10 mV s^-1, the specific capacitance of the pillared GP is 138 F g^-1 and 83.2 F g^-1 with negligible 3.85% and 4.35% capacitance degradation after 2000 cycles in aqueous and organic electrolytes, respectively. At an extremely fast scan rate of 500 mV s^-1, the specific capacitance can reach 80 F g^-1 in aqueous electrolyte. No binder is needed for assembling the supercapacitor cells and the pillared GP itself may serve as a current collector due to its intrinsic high electrical conductivity. Finally, the pillared GP has great potential in the development of promising flexible and ultralight-weight supercapacitors for electrochemical energy storage.

Submolecular Electronic Mapping of Single Cysteine Molecules by in Situ Scanning Tunneling Imaging

DEFF Research Database (Denmark)

Zhang, Jingdong; Chi, Qijin; Nazmutdinov, R. R.

2009-01-01

We have used L-Cysteine (Cys) as a model system to study the surface electronic structures of single molecules at the submolecular level in aqueous buffer solution by a combination of electrochemical scanning tunneling microscopy (in situ STM), electrochemistry including voltammetry and chronocou...

Electrochemical Preparation of Polyaniline Nanowires with the Used Electrolyte Solution Treated with the Extraction Process and Their Electrochemical Performance

Directory of Open Access Journals (Sweden)

Ying Wu

2018-02-01

Full Text Available Electrochemical polymerization of aniline is one of the most promising methods to prepare polyaniline (PANI materials. However, during this process, the electrolyte solution must be replaced after electropolymerization of a certain time because of the generation and the accumulation of the by-products, which have significant effects on the morphology, purity and properties of PANI products. Treatment and recycling of the used electrolyte solution are worthwhile to study to reduce the high treatment cost of the used electrolyte solution containing aniline and its polymerization by-products. Here, the composition of the used electrolyte solution was separated and determined by high performance liquid chromatography coupled with diode array detection (HPLC-DAD in the range of ultraviolet and visible (UV-Vis light. The analysis results revealed that the used electrolyte solution consisted of aniline, p-hydroquinone (HQ, p-benzoquinone (BQ, co-oligomers of aniline and p-benzoquinone (CAB and acid. Then, n-octanol and 2-octanone were selected as extracts to remove HQ, BQ and CAB from the used electrolyte solution. Following that, the recycled electrolyte solution was prepared by adjusting the concentration of aniline and acid of the aqueous phase, and the electrochemical polymerization process was conducted. Finally, the obtained PANI was characterized by scanning electron microscope (SEM and electrochemical methods. The experimental results clearly demonstrate that the morphology and specific capacitance of PANI produced from the recycled electrolyte solution can be recovered completely. This research paves the way for reusing the used electrolyte solution for aniline electrochemical polymerization.

Electrochemical Preparation of Polyaniline Nanowires with the Used Electrolyte Solution Treated with the Extraction Process and Their Electrochemical Performance.

Science.gov (United States)

Wu, Ying; Wang, Jixiao; Ou, Bin; Zhao, Song; Wang, Zhi; Wang, Shichang

2018-02-12

Electrochemical polymerization of aniline is one of the most promising methods to prepare polyaniline (PANI) materials. However, during this process, the electrolyte solution must be replaced after electropolymerization of a certain time because of the generation and the accumulation of the by-products, which have significant effects on the morphology, purity and properties of PANI products. Treatment and recycling of the used electrolyte solution are worthwhile to study to reduce the high treatment cost of the used electrolyte solution containing aniline and its polymerization by-products. Here, the composition of the used electrolyte solution was separated and determined by high performance liquid chromatography coupled with diode array detection (HPLC-DAD) in the range of ultraviolet and visible (UV-Vis) light. The analysis results revealed that the used electrolyte solution consisted of aniline, p-hydroquinone (HQ), p-benzoquinone (BQ), co-oligomers of aniline and p-benzoquinone (CAB) and acid. Then, n-octanol and 2-octanone were selected as extracts to remove HQ, BQ and CAB from the used electrolyte solution. Following that, the recycled electrolyte solution was prepared by adjusting the concentration of aniline and acid of the aqueous phase, and the electrochemical polymerization process was conducted. Finally, the obtained PANI was characterized by scanning electron microscope (SEM) and electrochemical methods. The experimental results clearly demonstrate that the morphology and specific capacitance of PANI produced from the recycled electrolyte solution can be recovered completely. This research paves the way for reusing the used electrolyte solution for aniline electrochemical polymerization.

A dual amplified electrochemical immunosensor for ofloxacin: Polypyrrole film-Au nanocluster as the matrix and multi-enzyme-antibody functionalized gold nanorod as the label

International Nuclear Information System (INIS)

Zang, Shuai; Liu, Yingju; Lin, Mouhong; Kang, Jianli; Sun, Yuanming; Lei, Hongtao

2013-01-01

Graphical abstract: Schematic representation of the OFL electrochemical immunosensor using Au nanoclusters/PPy/GCE as the substrate and multi-HRP-GNR-Ab2 bioconjugates as the label. Highlights: ► Gold nanorod was used to load HRP and Ab 2 to form multi-HRP-GNR-Ab 2 . ► A sensitive immunosensor for ofloxacin was constructed using the homemade antibody. ► A dual signal amplified strategy was based on the PPy-Au and multi-HRP-GNR-Ab 2 . -- Abstract: In this work, an electrochemical immunosensor, basing on a dual signal amplified strategy by employing a biocompatible polypyrrole film-Au nanocluster matrix as a sensor platform and multi-enzyme-antibody functionalized gold nanorod as an electrochemical detection label, is established for sensitive detection of ofloxacin (OFL). Firstly, polypyrrole film and Au nanoclusters were progressively fabricated onto the surface of a glassy carbon electrode via electropolymerization and electrochemical deposition, respectively. Such PPy-Au nanocomposite modified electrode was used to immobilize OFL-OVA, blocked with the blocking reagent, and then associated with the corresponding antibody. Secondly, gold nanorod (GNR) was synthesized to load horseradish peroxidase (HRP) and horseradish peroxidase-secondary antibody (HRP-Ab 2 ), and the resulting nanostructure (multi-HRP-GNR-Ab 2 ) was applied as the detection label. The fabrication process of the ordered multilayer structure and immunosensor were characterized by scanning electron microscopy (SEM) and electrochemical measurements, respectively. Finally, based on a competitive immunoassay, i.e., the association ability with the corresponding antibody between the captured antigen and free OFL in the solution, the fabricated immunosensor exhibited a sensitive response to OFL in the range from 0.08 to 410 ng/mL with a detection limit of 0.03 ng/mL. The current immunosensor exhibited good sensitivity, selectivity and long-term stability. This amplification strategy shows excellent

Electrochemical performance of potentiodynamically deposited polyaniline electrodes in ionic liquid

Energy Technology Data Exchange (ETDEWEB)

Patil, Dipali S., E-mail: dipali.patilphy@gmail.com [Department of Physics, Yeungnam University, Gyeonbuk 712-749 (Korea, Republic of); Thin Film Materials Laboratory, Department of Physics, Shivaji University, Kolhapur 416 004 (India); Pawar, S.A. [Thin Film Materials Laboratory, Department of Physics, Shivaji University, Kolhapur 416 004 (India); Department of Materials Science and Engineering, Chonnam National University, Gwangju 500 757 (Korea, Republic of); Patil, S.K.; Salavi, P.P.; Kolekar, S.S. [Department of Chemistry, Shivaji University, Kolhapur 416 004 (India); Devan, R.S.; Ma, Y.R. [Department of Physics, National Dong Hwa University, Hualien 97401, Taiwan (China); Kim, J.H. [Department of Materials Science and Engineering, Chonnam National University, Gwangju 500 757 (Korea, Republic of); Shin, J.C. [Department of Physics, Yeungnam University, Gyeonbuk 712-749 (Korea, Republic of); Patil, P.S., E-mail: patilps_2000@yahoo.com [Thin Film Materials Laboratory, Department of Physics, Shivaji University, Kolhapur 416 004 (India)

2015-10-15

Present work reports electropolymerization of aniline onto stainless steel substrate using room temperature ionic liquid N-methyl-2-pyrrolidonium hydrogensulfate [NMP][HSO{sub 4}] by potentiodynamic electrodeposition method. To study the effect of electropolymerization cycle number on the electrochemical performance, the number of scans is varied from 1{sup st} to 5{sup th} cycle. X-ray photoelectron spectroscopy is used for the phase identification of polyaniline (PANI) films. Scanning electrochemical microscopy (SECM) was used to study the electrochemical activity of PANI films. The highest specific capacitance of 581 Fg{sup −1} and energy density of 96.6 whkg{sup −1} are obtained for the sample, deposited using four cycle. - Graphical abstract: We have synthesized PANI samples with different thickness (or deposited mass) on stainless steel as a function of deposition cycles by potentiodynamic electrodeposition in room temperature IL [NMP][HSO{sub 4}]. A globular nanostructural growth of PANI is observed over the compact background of PANI for sample P{sub 2}. The sample P{sub 4} revealed a globular structure with spongy porous morphology. This nanostructure and porous structure is useful for supercapacitor, because it reduces the diffusion resistance of the electrolyte into electrode matrix. - Highlights: • Electropolymerization of aniline using room temperature ionic liquid N-methyl-2-pyrrolidonium hydrogensulfate [NMP][HSO4]. • The highest specific capacitance of 581 Fg{sup −1} and energy density of 96.60 Whkg{sup −1} is observed for the optimized sample. • The improved specific capacitance of PANI electrode material can be used to develop high performance supercapacitor.

Electrochemical performance of potentiodynamically deposited polyaniline electrodes in ionic liquid

International Nuclear Information System (INIS)

Patil, Dipali S.; Pawar, S.A.; Patil, S.K.; Salavi, P.P.; Kolekar, S.S.; Devan, R.S.; Ma, Y.R.; Kim, J.H.; Shin, J.C.; Patil, P.S.

2015-01-01

Present work reports electropolymerization of aniline onto stainless steel substrate using room temperature ionic liquid N-methyl-2-pyrrolidonium hydrogensulfate [NMP][HSO 4 ] by potentiodynamic electrodeposition method. To study the effect of electropolymerization cycle number on the electrochemical performance, the number of scans is varied from 1 st to 5 th cycle. X-ray photoelectron spectroscopy is used for the phase identification of polyaniline (PANI) films. Scanning electrochemical microscopy (SECM) was used to study the electrochemical activity of PANI films. The highest specific capacitance of 581 Fg −1 and energy density of 96.6 whkg −1 are obtained for the sample, deposited using four cycle. - Graphical abstract: We have synthesized PANI samples with different thickness (or deposited mass) on stainless steel as a function of deposition cycles by potentiodynamic electrodeposition in room temperature IL [NMP][HSO 4 ]. A globular nanostructural growth of PANI is observed over the compact background of PANI for sample P 2 . The sample P 4 revealed a globular structure with spongy porous morphology. This nanostructure and porous structure is useful for supercapacitor, because it reduces the diffusion resistance of the electrolyte into electrode matrix. - Highlights: • Electropolymerization of aniline using room temperature ionic liquid N-methyl-2-pyrrolidonium hydrogensulfate [NMP][HSO4]. • The highest specific capacitance of 581 Fg −1 and energy density of 96.60 Whkg −1 is observed for the optimized sample. • The improved specific capacitance of PANI electrode material can be used to develop high performance supercapacitor

Field emission response from multi-walled carbon nanotubes grown on electrochemically engineered copper foil

Energy Technology Data Exchange (ETDEWEB)

Tripathi, Amit Kumar; Jain, Vaibhav [Nanomaterials and Applications Lab., Department of Metallurgical and Materials Engineering, Indian Institute of Technology Roorkee, Roorkee, 247667, Uttarakhand (India); Saini, Krishna [Nanomaterials and Applications Lab., Department of Metallurgical and Materials Engineering, Indian Institute of Technology Roorkee, Roorkee, 247667, Uttarakhand (India); Centre of Excellence: Nanotechnology, Indian Institute of Technology Roorkee, Roorkee, 247667, Uttarakhand (India); Lahiri, Indranil, E-mail: indrafmt@iitr.ac.in [Nanomaterials and Applications Lab., Department of Metallurgical and Materials Engineering, Indian Institute of Technology Roorkee, Roorkee, 247667, Uttarakhand (India); Centre of Excellence: Nanotechnology, Indian Institute of Technology Roorkee, Roorkee, 247667, Uttarakhand (India)

2017-02-01

Exciting properties of carbon nanotube has proven it to be a promising candidate for field emission applications, if its processing cost can be reduced effectively. In this research, a new electrochemical technique is proposed for growing carbon nanotubes in selective areas by thermal chemical vapour deposition. In this process, electrochemical processing is used to create localized pits and deposition of catalysts, which act as roots to support growth and alignment of the CNTs on copper substrate. CNTs grown thus were characterized and studied using scanning electron microscope, transmission electron microscope and Raman spectroscopy, elucidating presence of multiwall carbon nanotubes (MWCNT). These CNT emitters have comparatively lower turn-on field and higher field enhancement factor. - Highlights: • Electrochemical pitting for localized carbon nanotube growth is proposed. • Electrochemical pitting method shows patterning effect on the substrate. • Size and density of pits depend on voltage, pH and temperature. • CNTs thus grown shows good field emission response.

Polypyrrole Composite Film for Highly Sensitive and Selective Electrochemical Determination Sensors

International Nuclear Information System (INIS)

Zheng, Xiangli; Tian, Dong; Duan, Shuo; Wei, Maochao; Liu, Shan; Zhou, Changli; Li, Qing; Wu, Gang

2014-01-01

In this paper, polypyrrole (PPy) and benz[a]anthracene-7,12-dione (BaD) were electro-polymerized onto a pyrolytic graphite electrode (PGE), constructing a novel BaD/PPy/PGE platform for electrochemical sensoring. The morphology and electrochemical properties of the fabricated BaD/PPy/PGE were characterized by scanning electron microscopy, cyclic voltammetry and electrochemical impedance spectroscopy. Furthermore, the electrochemical behavior of benzo[k]fluoranthene (BkF) at the BaD/PPy/PGE was investigated. Due to the specific interactions between BkF and BaD, a wide linear range of BkF detection from 1.0 × 10 −12 to 1.0 × 10 −9 M with good linearity (R 2 = 0.9962) and a low detection limit (1.0 × 10 −13 M, S/N = 3) were demonstrated. Importantly, other similar aromatics which had one ring or more than two rings, such as benzo[a]anthracene, benzo[a]pyrene, pyrene, benzo[ghi]peryle, anthracene, phenanthrene, naphthalene and parachlorophenol, showed insignificant interference on BkF detection. Consequently, this novel BaD/PPy/PGE with excellent stability and selectivity holds promise as an effective BkF electrochemical sensor in aqueous solution. As an example for its practical application, the newly developed sensor was applied to quantitative determination of BkF in waste water samples obtained from a coking plant with satisfactory sensitivity, selectivity, and reversibility

Influence of the polymeric coating thickness on the electrochemical performance of Carbon Fiber/PAni composites

Directory of Open Access Journals (Sweden)

Carla Polo Fonseca

2015-10-01

Full Text Available Abstract Carbon fiber/polyaniline composites (CF/PAni were synthesized at three different deposition time of 30, 60 and 90 min by oxidative polymerization. The composite materials were morphologically and physically characterized by scanning electron microscopy and by Raman spectroscopy, respectively. Their electrochemical responses were analyzed by cyclic voltammetry, by galvanostatic test, and by electrochemical impedance spectroscopy. The influence of the PAni layer thickness deposited on carbon fibers for the composite formation as well as for their electrochemical properties was discussed. The CF/PAni-30 showed a nanometric thickness with more homogeneous morphology compared to those formed in deposition times of 60 and 90 min. It also showed, from the electrochemical impedance spectroscopy measurements, the lowest charge transfer resistance value associated to the its highest value for the double-layer capacitance of 180 Fg-1 making it a very strong candidate as a supercapacitor electrode.

Light-Regulated Electrochemical Sensor Array for Efficiently Discriminating Hazardous Gases.

Science.gov (United States)

Liang, Hongqiu; Zhang, Xin; Sun, Huihui; Jin, Han; Zhang, Xiaowei; Jin, Qinghui; Zou, Jie; Haick, Hossam; Jian, Jiawen

2017-10-27

Inadequate detection limit and unsatisfactory discrimination features remain the challenging issues for the widely applied electrochemical gas sensors. Quite recently, we confirmed that light-regulated electrochemical reaction significantly enhanced the electrocatalytic activity, and thereby can potentially extend the detection limit to the parts per billion (ppb) level. Nevertheless, impact of the light-regulated electrochemical reaction on response selectivity has been discussed less. Herein, we systematically report on the effect of illumination on discrimination features via design and fabrication of a light-regulated electrochemical sensor array. Upon illumination (light on), response signal to the examined gases (C 3 H 6 , NO, and CO) is selectively enhanced, resulting in the sensor array demonstrating disparate response patterns when compared with that of the sensor array operated at light off. Through processing all the response patterns derived from both light on and light off with a pattern recognition algorithm, a satisfactory discrimination feature is observed. In contrast, apparent mutual interference between NO and CO is found when the sensor array is solely operated without illumination. The impact mechanism of the illumination is studied and it is deduced that the effect of the illumination on the discriminating features can be mainly attributed to the competition of electrocatalytic activity and gas-phase reactivity. If the enhanced electrocatalytic activity (to specific gas) dominates the whole sensing progress, enhancements in the corresponding response signal would be observed upon illumination. Otherwise, illumination gives a negligible impact. Hence, the response signal to part of the examined gases is selectively enhanced by illumination. Conclusively, light-regulated electrochemical reaction would provide an efficient approach to designing future smart sensing devices.

Electrochemically reduced graphene oxide-based electrochemical sensor for the sensitive determination of ferulic acid in A. sinensis and biological samples

Energy Technology Data Exchange (ETDEWEB)

Liu, Linjie [School of Pharmacy, Lanzhou University, Lanzhou 730000 (China); Gou, Yuqiang [Lanzhou Military Command Center for Disease Prevention and Control, Lanzhou 730000 (China); Gao, Xia; Zhang, Pei; Chen, Wenxia; Feng, Shilan [School of Pharmacy, Lanzhou University, Lanzhou 730000 (China); Hu, Fangdi, E-mail: hufd@lzu.edu.cn [School of Pharmacy, Lanzhou University, Lanzhou 730000 (China); Li, Yingdong, E-mail: lydj412@163.com [Gansu College of Tradition Chinese Medicine, Lanzhou 730000 (China)

2014-09-01

An electrochemically reduced graphene oxide (ERGO) modified glassy carbon electrode (GCE) was used as a new voltammetric sensor for the determination of ferulic acid (FA). The morphology and microstructure of the modified electrodes were characterized by scanning electron microscopy (SEM) and Raman spectroscopy analysis, and the electrochemical effective surface areas of the modified electrodes were also calculated by chronocoulometry method. Sensing properties of the electrochemical sensor were investigated by means of cyclic voltammetry (CV) and differential pulse voltammetry (DPV). It was found that ERGO was electrodeposited on the surface of GCE by using potentiostatic method. The proposed electrode exhibited electrocatalytic activity to the redox of FA because of excellent electrochemical properties of ERGO. The transfer electron number (n), electrode reaction rate constant (k{sub s}) and electron-transfer coefficient (α) were calculated as 1.12, 1.24 s{sup −1}, and 0.40, respectively. Under the optimized conditions, the oxidation peak current was proportional to FA concentration at 8.49 × 10{sup −8} mol L{sup −1} to 3.89 × 10{sup −5} mol L{sup −1} with detection limit of 2.06 × 10{sup −8} mol L{sup −1}. This fabricated sensor also displayed acceptable reproducibility, long-term stability, and high selectivity with negligible interferences from common interfering species. The voltammetric sensor was successfully applied to detect FA in A. sinensis and biological samples with recovery values in the range of 99.91%-101.91%. - Highlights: • A novel ERGO–based electrochemical sensor of FA was successfully fabricated by using one-step electrodeposition method. • The electrode reaction was an adsorption–diffusion mixed controlled process. • The low detection limit with good selectivity and sensitivity were obtained. • This method was applied for the determination of FA in A. sinensis and biological samples.

Fabrication of an electrically conductive mixed self-assembled monolayer and its application in an electrochemical immunosensor

International Nuclear Information System (INIS)

Lee, Jung Bae; Namgung, Miok; Lee, Sang-Baek; Oh, Se Young

2008-01-01

Oligophenylethynylene thiol containing carboxylic acid in the tail group as a conducting wire bioreceptor was synthesized, and then its electrical property was investigated from the measurement of scanning tunneling microscopy (STM). Mixed self-assembled monolayer (SAM) consisting of 4-(2-(4-acetylthio)phenyl)ethynyl) benzoic acid (APBA) and butanethiol was fabricated in order to improve the electrical conductivity owing to the molecular orientation. We have examined the molecular orientation and the electrochemical activity of mixed SAM via X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). Especially, the prepared mixed SAM used as a bioreceptor in electrochemical prostate specific antigen (PSA) immunosensor showed higher electrochemical activity than that of the other SAMs

Electrochemical behavior of cysteine at a CuGeO3 nanowires modified glassy carbon electrode

International Nuclear Information System (INIS)

Dong Yongping; Pei Lizhai; Chu Xiangfeng; Zhang Wangbing; Zhang Qianfeng

2010-01-01

A CuGeO 3 nanowire modified glassy carbon electrode was fabricated and characterized by scanning electron microscopy. The results of electrochemical impedance spectroscopy reveal that electron transfer through nanowire film is facile compared with that of bare glassy carbon electrode. The modified electrode exhibited a novel electrocatalytic behavior to the electrochemical reactions of L-cysteine in neutral solution, which was not reported previously. Two pairs of semi-reversible electrochemical peaks were observed and assigned to the processes of oxidation/reduction and adsorption/desorption of cysteine at the modified electrode, respectively. The electrochemical response of cysteine is poor in alkaline condition and is enhanced greatly in acidic solution, suggesting that hydrogen ions participate in the electrochemical oxidation process of cysteine. The intensities of two anodic peaks varied linearly with the concentration of cysteine in the range of 1 x 10 -6 to 1 x 10 -3 mol L -1 , which make it possible to sensitive detection of cysteine with the CuGeO 3 nanowire modified electrode. Furthermore, the modified electrode exhibited good reproducibility and stability.

Conductive polymer/reduced graphene oxide/Au nano particles as efficient composite materials in electrochemical supercapacitors

Energy Technology Data Exchange (ETDEWEB)

Shabani Shayeh, J. [Center of Excellence in Electrochemistry, University of Tehran, Tehran (Iran, Islamic Republic of); Ehsani, A., E-mail: a.ehsani@qom.ac.ir [Department of Chemistry, Faculty of Science, University of Qom, P.O. Box 37185-359, Qom (Iran, Islamic Republic of); Ganjali, M.R.; Norouzi, P. [Center of Excellence in Electrochemistry, University of Tehran, Tehran (Iran, Islamic Republic of); Endocrinology & Metabolism Research Center, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Jaleh, B. [Physics Department, Bu-Ali Sina University, Hamedan 65174 (Iran, Islamic Republic of)

2015-10-30

Graphical abstract: - Highlights: • PANI/rGO/AuNPs as a ternary composite synthesized by electrodeposition. • Presence of rGO/AuNPs caused increasing the stability of electrodes. • Composite represented high specific capacitance, specific power and specific energy values than PANI. - Abstract: Polyaniline/reduced graphene oxide/Au nano particles (PANI/rGO/AuNPs) as a hybrid supercapacitor were deposited on a glassy carbon electrode (GCE) by cyclic voltammetry (CV) method as ternary composites and their electrochemical performance was evaluated in acidic medium. Scanning electron micrographs clearly revealed the formation of nanocomposites on the surface of the working electrode. Scanning electron micrographs (SEM) clearly revealed the formation of nanocomposites on the surface of working electrode. Different electrochemical methods including galvanostatic charge–discharge (CD) experiments, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were carried out in order to investigate the applicability of the system as a supercapacitor. Based on the cyclic voltammogram results obtained, PANI/rGO/AuNPs gave higher specific capacitance, power and energy values than PANI at a current density of 1 mA cm{sup −2}. Specific capacitance (SC) of PANI and PANI/rGO/AuNPs electrodes calculated using CV method are 190 and 303 F g{sup −1}, respectively. The present study introduces new nanocomposite materials for electrochemical redox capacitors with advantages including long life cycle and stability due to synergistic effects of each component.

Conductive polymer/reduced graphene oxide/Au nano particles as efficient composite materials in electrochemical supercapacitors

International Nuclear Information System (INIS)

Shabani Shayeh, J.; Ehsani, A.; Ganjali, M.R.; Norouzi, P.; Jaleh, B.

2015-01-01

Graphical abstract: - Highlights: • PANI/rGO/AuNPs as a ternary composite synthesized by electrodeposition. • Presence of rGO/AuNPs caused increasing the stability of electrodes. • Composite represented high specific capacitance, specific power and specific energy values than PANI. - Abstract: Polyaniline/reduced graphene oxide/Au nano particles (PANI/rGO/AuNPs) as a hybrid supercapacitor were deposited on a glassy carbon electrode (GCE) by cyclic voltammetry (CV) method as ternary composites and their electrochemical performance was evaluated in acidic medium. Scanning electron micrographs clearly revealed the formation of nanocomposites on the surface of the working electrode. Scanning electron micrographs (SEM) clearly revealed the formation of nanocomposites on the surface of working electrode. Different electrochemical methods including galvanostatic charge–discharge (CD) experiments, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were carried out in order to investigate the applicability of the system as a supercapacitor. Based on the cyclic voltammogram results obtained, PANI/rGO/AuNPs gave higher specific capacitance, power and energy values than PANI at a current density of 1 mA cm"−"2. Specific capacitance (SC) of PANI and PANI/rGO/AuNPs electrodes calculated using CV method are 190 and 303 F g"−"1, respectively. The present study introduces new nanocomposite materials for electrochemical redox capacitors with advantages including long life cycle and stability due to synergistic effects of each component.

Gold nanocone probes for near-field scanning optical microscopy

Energy Technology Data Exchange (ETDEWEB)

Zeeb, Bastian; Schaefer, Christian; Nill, Peter; Fleischer, Monika; Kern, Dieter P. [Institute of Applied Physics, University of Tuebingen, Auf der Morgenstelle 10, 72076 Tuebingen (Germany)

2010-07-01

Apertureless near-field scanning optical microscopy (ANSOM) provides the possibility to collect simultaneously high-resolution topographical and sub-diffraction limited optical information from a surface. When optically excited, the scanning probes act as optical antennae with a strong near-field enhancement near the tip apex. Spatial resolution and optical near-field enhancement depend strongly on the properties and geometry of the scanning probe - in particular on very sharp tip radii. Various possibilities for fabricating good antennae have been pursued. Most commonly, scanning probes consist of electrochemically etched gold wires which are sharp but not well-defined in geometry. We present two different approaches for ultra sharp and well-defined antennae based upon fabricating gold nanocones with a tip radius smaller than 10 nm which can be used in ANSOM. A transfer process is presented that can be used to attach single gold nanocones to non-metallic probes such as sharp glass fiber tips. Alternatively, new processes are presented to fabricate cones directly on pillars of different materials such as silicon or bismuth, which can be applied to cantilever tips for ANSOM scanning applications.

An Electrochemical Investigation of Nano Cerium Oxide/Graphene as an Electrode Material for Supercapacitors

Directory of Open Access Journals (Sweden)

Mohammadreza Shishesaz

2015-01-01

In this paper, the effect of cationic and anionic ion sizes on the charge storage capability of graphene nanosheets, is investigated. Electrochemical properties of produced electrode are studied using cyclic voltammetry (CV and electrochemical impedance spectroscopy (EIS techniques, in 3M NaCl, NaOH and KOH electrolytes. Scanning electron microscopy (SEM is used to characterize the microstructure and nature of prepared electrode. SEM images and XRD patterns confirm the layered structure (12 nm thickness of the used graphene with an interlayer distance of 3.36 (Å. The electrochemical results and the ratio of q*O/q*T confirm a good charge storage and charge delivering capability of prepared electrode in 3M NaCl electrolyte. Charge/discharge cycling test shows a good reversibility and confirms that solution resistance will increase after 500 cycles.

Electrochemical reduction of NO{sub x}

Energy Technology Data Exchange (ETDEWEB)

Lund Traulsen, M.

2012-04-15

NO and NO{sub 2} (collectively referred to as NO{sub x}) are air pollutants, and the largest single contributor to NO{sub x} pollution is automotive exhaust. This study investigates electrochemical deNO{sub x}, a technology which aims to remove NO{sub x} from automotive diesel exhaust by electrochemical reduction of NO{sub x} to N{sub 2} and O{sub 2}. The focus in this study is on improving the activity and selectivity of solid oxide electrodes for electrochemical deNO{sub x} by addition of NO{sub x} storage compounds to the electrodes. Two different composite electrodes, La{sub 0.85}Sr{sub 0.15}MnO{sub 3-{delta}-}Ce{sub 0.9}Gd{sub 0.1}O{sub 1.95} (LSM15-CGO10) and La{sub 0.85}Sr{sub 0.15}FeO{sub 3-{delta}-}Ce{sub 0.9}Gd{sub 0.1}O{sub 1.95} (LSF15-CGO10), have been investigated in combination with three different NO{sub x} storage compounds: BaO, K{sub 2}O and MnO{sub x}. The main focus in the investigation has been on conversion measurements and electrochemical characterization, the latter by means of electrochemical impedance spectroscopy and cyclic voltammetry. In addition, infrared spectroscopy has been performed to study how NO{sub x} adsorption on the electrodes is affected by the presence of the aforementioned NO{sub x} storage compounds. Furthermore, non-tested and tested electrode microstructures have been thoroughly evaluated by scanning electron microscopy. The studies reveal addition of MnO{sub x} or K{sub 2}O to the electrodes cause severe degradation problems, and addition of these compounds is thus unsuitable for electrode improvement. In contrast, addition of BaO to LSM15-CGO10 electrodes is shown to have a very positive impact on the NO{sub x} conversion. The increased NO{sub x} conversion, following the BaO addition, is attributed to a combination of 1) a decreased electrode polarisation resistance and 2) an altered NO{sub x} adsorption. The NO{sub x} conversion is observed to increase strongly with polarisation, and during 9 V polarisation of an

Electrochemical Properties of Graphene Oxide/Resol Composites as Electrode Materials for Supercapacitor Applications.

Science.gov (United States)

Park, Geon Woo; Jeon, Sang Kwon; Yang, Jin Yong; Choi, Sung Dae; Kim, Geon Joong

2016-05-01

RGO/Resol carbon composites were prepared from a mixture of reduced GO and a low-molecular-weight phenolic resin (Resol) solution. The effects of the calcination temperature, amount of Resol added and KOH treatment on the electrochemical performance of the RGO/Resol composites were investigated. The physical and electrochemical properties of the composite materials were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Brunauer, Emmett and Teller (BET) surface areas measurements, and cyclic voltammetry (CV). The relationships between their physical properties and their electrochemical performance were examined for use as super-capacitors (SCs). The RGO/Resol composite calcined at 400 degrees C after the KOH loading showed dramatically improved electrochemical properties, showing a high BET surface and capacitance of 2190 m2/g and 220 F/g, respectively. The RGO/Resol composites calcined after the KOH treatment showed much better capacitor performance than those treated only thermally at the same temperature without KOH impregnation. The fabrication of high surface electrodes was essential for improving the SCs properties.

Electrochemical behaviours of lanthanide fluorides in the electrolysis system with LiF-NaF-Kf salt

International Nuclear Information System (INIS)

Joon-Bo, Shim; Sung-Chan, Hwang; Eung-Ho, Kim; Young-Ho, Kang; Byung-Jik, Lee; Jae-Hyung, Yoo

2003-01-01

As a part of partitioning studies, the experiments of cyclic voltammetry and electrolytic reduction with the liquid bismuth cathode were conducted to investigate electrochemical behaviours of lanthanide elements in the electrorefining system employing LiF-NaF-KF eutectic salt as the electrolyte. The cyclic voltammograms for NdF 3 and GdF 3 were obtained at various potential scan rates, respectively. The cathodic and anodic peak currents of the elements increased in proportion to the square root of the potential scan rate. According to changes of the potential difference between the coupled cathodic and anodic peaks, reversibilities of the reduction-oxidation reactions in this system were evaluated. In addition, further behaviours of electrochemical reaction of the elements were examined through electrolytic tests of the system using liquid bismuth as the cathode at fixed current densities. (author)

An electrochemical sensor based on carboxymethylated dextran modified gold surface for ochratoxin A analysis

OpenAIRE

Heurich, Meike; Kadir, Mohamad Kamal Abdul; Tothill, Ibtisam E.

2011-01-01

A disposable electrochemical immunosensor method was developed for ochratoxin A analysis to be applied for wine samples by using a screen-printed gold working electrode with carbon counter and silver/silver chloride pseudo-reference electrode. An indirect competitive enzyme-linked immunosorbent assay (ELISA) format was constructed by immobilising ochratoxin A conjugate using passive adsorption or covalent immobilisation via amine coupling to a carboxymethylated dextran (CMD)...

MnO{sub 2} nanotube and nanowire arrays by electrochemical deposition for supercapacitors

Energy Technology Data Exchange (ETDEWEB)

Xia, Hui; Feng, Jinkui; Wang, Hailong; Lai, Man On; Lu, Li [Department of Mechanical Engineering, National University of Singapore, 9 Engineering Drive 1, Singapore 117576 (Singapore)

2010-07-01

Highly ordered MnO{sub 2} nanotube and nanowire arrays are successfully synthesized via a electrochemical deposition technique using porous alumina templates. The morphologies and microstructures of the MnO{sub 2} nanotube and nanowire arrays are investigated by field emission scanning electron microscopy and transmission electron microscopy. Electrochemical characterization demonstrates that the MnO{sub 2} nanotube array electrode has superior capacitive behaviour to that of the MnO{sub 2} nanowire array electrode. In addition to high specific capacitance, the MnO{sub 2} nanotube array electrode also exhibits good rate capability and good cycling stability, which makes it promising candidate for supercapacitors. (author)

Characterization of immobilization methods of antiviral antibodies in serum for electrochemical biosensors

Energy Technology Data Exchange (ETDEWEB)

Huy, Tran Quang, E-mail: huytq@nihe.org.vn [National Institute of Hygiene and Epidemiology (NIHE), No1 Yersin St., Hanoi (Viet Nam); International Training Institute for Materials Science (ITIMS), Hanoi University of Science and Technology (HUST), No1 Dai Co Viet, Hanoi (Viet Nam); Hanh, Nguyen Thi Hong; Van Chung, Pham; Anh, Dang Duc; Nga, Phan Thi [National Institute of Hygiene and Epidemiology (NIHE), No1 Yersin St., Hanoi (Viet Nam); Tuan, Mai Anh, E-mail: tuanma-itims@mail.hut.edu.vn [International Training Institute for Materials Science (ITIMS), Hanoi University of Science and Technology (HUST), No1 Dai Co Viet, Hanoi (Viet Nam)

2011-06-01

In this paper, we describes different methods to immobilize Japanese encephalitis virus (JEV) antibodies in human serum onto the interdigitated surface of a microelectrode sensor for optimizing electrochemical detection: (1) direct covalent binding to the silanized surface, (2) binding to the silanized surface via a cross-linker of glutaraldehyde (GA), (3) binding to glutaraldehyde/silanized surface via goat anti-human IgG polyclonal antibody and (4) binding to glutaraldehyde/silanized surface via protein A (PrA). Field emission scanning electron microscopy, Fourier transform infrared spectrometry, and fluorescence microscopy are used to verify the characteristics of antibodies on the interdigitated surface after the serum antibodies immobilization. The analyzed results indicate that the use of protein A is an effective choice for immobilization and orientation of antibodies in serum for electrochemical biosensors. This study provides an advantageous immobilization method of serum containing antiviral antibodies to develop electrochemical biosensors for preliminary screening of viruses in clinical samples from outbreaks.

Chitosan/graphene oxide nanocomposite films with enhanced interfacial interaction and their electrochemical applications

International Nuclear Information System (INIS)

He, Linghao; Wang, Hongfang; Xia, Guangmei; Sun, Jing; Song, Rui

2014-01-01

Graphical abstract: Nanocomposites by introducing graphene oxide (GO) into chitosan (CS) matrix were prepared and the effect of GO on the crystallization, thermal stability and mechanical properties of the films were investigated. In addition, the electrochemical behavior of the CS/GO modified electrode was comparatively studied with that of the neat CS-modified electrode. - Highlights: • Graphene oxide (GO) with well dispersion in the biopolymer chitosan (CS) matrix. • Detectable interactions do exist between the GO nanosheets and CS segments. • The addition of minor GO can improve the electrochemical activity of the neat CS. - Abstract: A series of chitosan (CS) nanocomposites incorporated with graphene oxide (GO) nanosheets were facilely prepared by sonochemical method. Characterized by scanning electron microscopy, the obtained nanocomposites showed fine dispersion of GO in the CS matrix. Meanwhile, a marked interfacial interaction was also revealed as the values of glass transition temperature, the decomposition temperature and the storage modulus were significantly increased with the addition of GO. Furthermore, the well dispersed GO nanosheets could significantly improve the electrochemical activity of the CS as demonstrated by the electrochemical behaviors of pure CS and the GO/CS composite electrodes. Hence, the GO/CS nanocomposites film could be a promising candidate in the fabrication of electrochemical biosensors

Reaction of Br2 with adsorbed CO on Pt, studied by the surface interrogation mode of scanning electrochemical microscopy.

Science.gov (United States)

Wang, Qian; Rodríguez-López, Joaquín; Bard, Allen J

2009-12-02

Scanning electrochemical microscopy surface interrogation (SI-SECM) in the cyclic voltammetry mode was successfully used to detect and quantify adsorbed CO on a Pt electrode by reaction with electrogenerated Br(2). The two-electrode setup used in this new technique allowed the production of Br(2) on an interrogator tip, which reported a transient positive feedback above a Pt substrate at open circuit as an indication of the reactivity of this halogen with CO((ads)). Br(-) and CO(2) are shown to be the main products of the reaction (in the absence of O(2)), which may involve the formation of bromophosgene as a hydrolyzable intermediate. Under saturation conditions, CO((ads)) was reproducibly quantified at the polycrystalline Pt surface with theta(CO) approximately = 0.5. The reaction is shown to be blocked by the action of pre-adsorbed cyanide, which demonstrates the surface character of the process. The formation of CO(2) as an end product was further tested in a bulk experiment: addition of Pt black to a mixture of Br(2) in 0.5 M H(2)SO(4) through which CO was bubbled gave a precipitate of BaCO(3) in a saturated solution of Ba(OH)(2). The use of SI-SECM allowed access to a reaction that would otherwise be difficult to prove through conventional electrochemistry on a single electrode.

Effect of antimony, bismuth and calcium addition on corrosion and electrochemical behaviour of AZ91 magnesium alloy

International Nuclear Information System (INIS)

Zhou Wei; Aung, Naing Naing; Sun Yangshan

2009-01-01

This study investigated the effect of antimony, bismuth and calcium addition on the corrosion and electrochemical behaviour of AZ91 magnesium alloy in 3.5% NaCl solution. Techniques including constant immersion, electrochemical potentiodynamic polarisation, scanning electron microscopy (SEM), energy dispersed spectroscopy (EDS) and X-ray diffraction (XRD) were used to characterise electrochemical and corrosion properties and surface topography. It was found that corrosion attack occurred preferentially on Mg 3 Bi 2 and Mg 3 Sb 2 particles while Mg 17 Al 8 Ca 0.5 and Mg 2 Ca phases showed no detrimental effect on corrosion. Combined addition of small amounts of bismuth and antimony to the AZ91 alloy resulted in significant increase in corrosion rate

Technological study of electrochemical uranium fuel reprocessing in fused chloride bath

International Nuclear Information System (INIS)

Fernandes, Damaris

2002-01-01

This study is applied to metallic fuels recycling, concerning advanced reactor concept, which was proposed and tested in LMR type reactors. Conditions for electrochemical non-irradiated uranium fuel reprocessing in fused chloride bath in laboratory scale were established. Experimental procedures and parameters for dehydration treatment of LiCl-KCl eutectic mixture and for electrochemical study of U 3+ /U system in LiCl-KCl were developed and optimized. In the voltammetric studies many working electrodes were tested. As auxiliary electrodes, graphite and stainless steels crucibles were verified, with no significant impurities inclusions in the system. Ag/AgCl in Al 2 O 3 with 1 w% in AgCl were used as reference electrode. The experimental set up developed for electrolyte treatment as well as for the study of the system U 3+ /U in LiCl-KCl showed to be adequate and efficient. Thermogravimetric Techniques, Scanning Electron Microscopy with Energy Dispersive X-Ray Spectrometry and cyclic voltametry showed an efficient dehydration method by using HCl gas and than argon flux for 12 h. Scanning Electron Microscopy, with Energy Dispersive X-Ray Spectrometry and Inductively Coupled Plasma Emission Spectrometry and DC Arc Emission Spectrometry detected the presence of uranium in the cadmium phase. X-ray Diffraction and also Inductively Coupled Plasma Emission Spectrometry and DC Arc Emission Spectrometry were used for uranium detection in the salt phase. The obtained results for the system U 3+ /U in LiCl-KCl showed the viability of the electrochemical reprocessing process based on the IFR advanced fuel cycle. (author)

On the Electrochemical Behavior of PVD Ti-Coated AISI 304 Stainless Steel in Borate Buffer Solution

Science.gov (United States)

Fattah-alhosseini, Arash; Elmkhah, Hassan; Attarzadeh, Farid Reza

2017-04-01

This work aims at studying the electrochemical behavior of annealed pure titanium (Ti) and nano-structured (NS) Ti coating in borate buffer solutions. Cathodic arc evaporation was successfully applied to deposit NS Ti coating. Samples were characterized by means of scanning electron microscope and x-ray diffraction. Potentiodynamic polarization tests, electrochemical impedance spectroscopy, and Mott-Schottky analysis were employed to discuss the electrochemical behavior of samples thoroughly. Electrochemical measurements showed that the deposited NS Ti coating offers a superior passivity in borate buffer solutions of pH 9.0 and 9.5. Mott-Schottky analysis revealed that all passive films are of n-type semiconducting nature in these alkaline solutions and the deposition process did not alter the semiconducting type of passive films formed on samples. Additionally, this analysis showed that the NS Ti coating possessed lower levels of donor densities. Finally, all electrochemical tests showed that passive behavior of the NS Ti samples was superior, mainly due to the formation of thicker and less defective passive films.

Hydroxyapatite formation on biomedical Ti–Ta–Zr alloys by magnetron sputtering and electrochemical deposition

Energy Technology Data Exchange (ETDEWEB)

Kim, Hyun-Ju [Department of Dental Materials, Research Center of Nano-Interface Activation for Biomaterials, and Research Center for Oral Disease Regulation of the Aged, School of Dentistry, Chosun University, Gwangju (Korea, Republic of); Jeong, Yong-Hoon [Biomechanics and Tissue Engineering Laboratory, Division of Orthodontics, College of Dentistry, The Ohio State University, Columbus, OH (United States); Choe, Han-Cheol, E-mail: hcchoe@chosun.ac.kr [Department of Dental Materials, Research Center of Nano-Interface Activation for Biomaterials, and Research Center for Oral Disease Regulation of the Aged, School of Dentistry, Chosun University, Gwangju (Korea, Republic of); Brantley, William A. [Division of Prosthodontics and Restorative Science, College of Dentistry, The Ohio State University, Columbus, OH (United States)

2014-12-01

The purpose of this study was to investigate hydroxyapatite formation on Ti-25Ta-xZr titanium alloys resulting from radio-frequency magnetron sputtering and electrochemical deposition. Electrochemical deposition of hydroxyapatite (HA) was first carried out using a cyclic voltammetry (CV) method at 80 °C in 5 mM Ca (NO{sub 3}){sub 2} + 3 mM NH{sub 4}H{sub 2}PO{sub 4}. Then a physical vapor deposition (PVD) coating was obtained by a radio-frequency (RF) magnetron sputtering technique. The microstructures, phase transformations, and morphologies of the hydroxyapatite films deposited on the titanium alloys were analyzed by optical microscopy (OM), X-ray diffractometer (XRD), energy dispersive X-ray spectroscopy (EDS) and field-emission scanning electron microscopy (FE-SEM). The morphologies of electrochemically deposited HA showed plate-like shapes on the titanium alloys, and the morphologies of the RF-sputtered HA coating had the appearance droplet particles on the plate-like precipitates that had formed by electrochemical deposition. For the RF-sputtered HA coatings, the Ca/P ratio was increased, compared to that for the electrochemically deposited HA surface. Moreover, the RF-sputtered HA coating, consisting of agglomerated droplet particles on the electrochemically deposited HA surface, had better wettability compared to the bulk titanium alloy surface. - Highlights: • Hydroxyapatite (HA) was deposited on Ti–Ta–Zr alloys by radio-frequency (RF) magnetron sputtering and a cyclic voltammetry. • The morphologies of the RF-sputtered HA coating on electrochemical deposits presented plate-like shapes with a droplet particle. • The Ca/P ratio for RF-sputtered HA coatings was greater than that for electrochemical deposited HA coatings. • The RF-sputtered and electrochemical HA coatings had superior wettability compared to the electrochemically deposited coatings.

Hydroxyapatite formation on biomedical Ti–Ta–Zr alloys by magnetron sputtering and electrochemical deposition

International Nuclear Information System (INIS)

Kim, Hyun-Ju; Jeong, Yong-Hoon; Choe, Han-Cheol; Brantley, William A.

2014-01-01

The purpose of this study was to investigate hydroxyapatite formation on Ti-25Ta-xZr titanium alloys resulting from radio-frequency magnetron sputtering and electrochemical deposition. Electrochemical deposition of hydroxyapatite (HA) was first carried out using a cyclic voltammetry (CV) method at 80 °C in 5 mM Ca (NO 3 ) 2 + 3 mM NH 4 H 2 PO 4 . Then a physical vapor deposition (PVD) coating was obtained by a radio-frequency (RF) magnetron sputtering technique. The microstructures, phase transformations, and morphologies of the hydroxyapatite films deposited on the titanium alloys were analyzed by optical microscopy (OM), X-ray diffractometer (XRD), energy dispersive X-ray spectroscopy (EDS) and field-emission scanning electron microscopy (FE-SEM). The morphologies of electrochemically deposited HA showed plate-like shapes on the titanium alloys, and the morphologies of the RF-sputtered HA coating had the appearance droplet particles on the plate-like precipitates that had formed by electrochemical deposition. For the RF-sputtered HA coatings, the Ca/P ratio was increased, compared to that for the electrochemically deposited HA surface. Moreover, the RF-sputtered HA coating, consisting of agglomerated droplet particles on the electrochemically deposited HA surface, had better wettability compared to the bulk titanium alloy surface. - Highlights: • Hydroxyapatite (HA) was deposited on Ti–Ta–Zr alloys by radio-frequency (RF) magnetron sputtering and a cyclic voltammetry. • The morphologies of the RF-sputtered HA coating on electrochemical deposits presented plate-like shapes with a droplet particle. • The Ca/P ratio for RF-sputtered HA coatings was greater than that for electrochemical deposited HA coatings. • The RF-sputtered and electrochemical HA coatings had superior wettability compared to the electrochemically deposited coatings

Addition of nitrite enhances the electrochemical defluorination of 2-fluoroaniline

International Nuclear Information System (INIS)

Feng, Huajun; Liang, Yuxiang; Guo, Kun; Long, Yuyang; Cong, Yanqing; Shen, Dongsheng

2015-01-01

Highlights: • A method for improving defluorination performance by in situ self-assembly of pollutants was developed. • The mechanisms of 2-FA modification and defluorination are discussed. • Positively-charged diazonium salt is used to weaken the C–F bond. - Abstract: This study introduces a novel approach that uses the interaction of pollutants with added nitrite to produce diazonium salts, which cause in situ self-assembly of the pollutants on carbon electrodes, to improve their 2-fluoroaniline (2-FA) defluorination and removal performance. The 2-FA degradation performance, electrode properties, electrochemical properties and degradation pathway were investigated. The reactor containing NO_2"− achieved a 2-FA removal efficiency of 90.1% and a defluorination efficiency of 38% within 48 h, 1.4 and 2.3 times higher than the corresponding results achieved without NO_2"−, respectively. The residual NO_2"− was less than 0.5 mg/L in the reactor containing added NO_2"−, which would not cause serious secondary pollution. Scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) results proved that the carbon anode surface was successfully modified with benzene polymer, and electrochemical tests confirmed that the electrochemical activity of the modified anode was enhanced significantly. The C–F bond was weakened by the effect of the positive charge of the benzenediazonium groups, and the high electrochemical activity of the carbon anode enhanced the electrochemical performance of the system to accelerate defluorination. Thus, the present electrical method involving nitrite nitrogen is very promising for the treatment of wastewater containing fluoroaniline compounds.

Static and Dynamic Measurement of Dopamine Adsorption in Carbon Fiber Microelectrodes Using Electrochemical Impedance Spectroscopy.

Science.gov (United States)

Rivera-Serrano, Nilka; Pagan, Miraida; Colón-Rodríguez, Joanisse; Fuster, Christian; Vélez, Román; Almodovar-Faria, Jose; Jiménez-Rivera, Carlos; Cunci, Lisandro

2018-02-06

In this study, electrochemical impedance spectroscopy was used for the first time to study the adsorption of dopamine in carbon fiber microelectrodes. In order to show a proof-of-concept, static and dynamic measurements were taken at potentials ranging from -0.4 to 0.8 V versus Ag|AgCl to demonstrate the versatility of this technique to study dopamine without the need of its oxidation. We used electrochemical impedance spectroscopy and single frequency electrochemical impedance to measure different concentrations of dopamine as low as 1 nM. Moreover, the capacitance of the microelectrodes surface was found to decrease due to dopamine adsorption, which is dependent on its concentration. The effect of dissolved oxygen and electrochemical oxidation of the surface in the detection of dopamine was also studied. Nonoxidized and oxidized carbon fiber microelectrodes were prepared and characterized by optical microscopy, scanning electron microscopy, cyclic voltammetry, and electrochemical impedance spectroscopy. Optimum working parameters of the electrodes, such as frequency and voltage, were obtained for better measurement. Electrochemical impedance of dopamine was determined at different concentration, voltages, and frequencies. Finally, dynamic experiments were conducted using a flow cell and single frequency impedance in order to study continuous and real-time measurements of dopamine.

Electrochemical Impedance Spectroscopic Analysis of RuO2 Based Thick Film pH Sensors

International Nuclear Information System (INIS)

Manjakkal, Libu; Djurdjic, Elvira; Cvejin, Katarina; Kulawik, Jan; Zaraska, Krzysztof; Szwagierczak, Dorota

2015-01-01

The conductimetric interdigitated thick film pH sensors based on RuO 2 were fabricated and their electrochemical reactions with solutions of different pH values were studied by electrochemical impedance spectroscopy (EIS) technique. The microstructural properties and composition of the sensitive films were examined by scanning electron microscopy, X-ray energy dispersive spectroscopy and Raman spectroscopy. The EIS analysis of the sensor was carried out in the frequency range 10 mHz–2 MHz for pH values of test solutions 2–12. The electrical parameters of the sensor were found to vary with changing pH. The conductance and capacitance of the film were distinctly dependent on pH in the low frequency range. The Nyquist and Bode plots derived from the impedance data for the metal oxide thick film pH sensor provided information about the underlying electrochemical reactions

Flexible pillared graphene-paper electrodes for high-performance electrochemical supercapacitors.

Science.gov (United States)

Wang, Gongkai; Sun, Xiang; Lu, Fengyuan; Sun, Hongtao; Yu, Mingpeng; Jiang, Weilin; Liu, Changsheng; Lian, Jie

2012-02-06

Flexible graphene paper (GP) pillared by carbon black (CB) nanoparticles using a simple vacuum filtration method is developed as a high-performance electrode material for supercapacitors. Through the introduction of CB nanoparticles as spacers, the self-restacking of graphene sheets during the filtration process is mitigated to a great extent. The pillared GP-based supercapacitors exhibit excellent electrochemical performances and cyclic stabilities compared with GP without the addition of CB nanoparticles. At a scan rate of 10 mV s(-1) , the specific capacitance of the pillared GP is 138 F g(-1) and 83.2 F g(-1) with negligible 3.85% and 4.35% capacitance degradation after 2000 cycles in aqueous and organic electrolytes, respectively. At an extremely fast scan rate of 500 mV s (-1) , the specific capacitance can reach 80 F g(-1) in aqueous electrolyte. No binder is needed for assembling the supercapacitor cells and the pillared GP itself may serve as a current collector due to its intrinsic high electrical conductivity. The pillared GP has great potential in the development of promising flexible and ultralight-weight supercapacitors for electrochemical energy storage. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Electrochemical biosensors

CERN Document Server

Cosnier, Serge

2015-01-01

"This is an excellent book on modern electrochemical biosensors, edited by Professor Cosnier and written by leading international experts. It covers state-of-the-art topics of this important field in a clear and timely manner."-Prof. Joseph Wang, UC San Diego, USA 　"This book covers, in 13 well-illustrated chapters, the potential of electrochemical methods intimately combined with a biological component for the assay of various analytes of biological and environmental interest. Particular attention is devoted to the description of electrochemical microtools in close contact with a biological cell for exocytosis monitoring and to the use of nanomaterials in the electrochemical biosensor architecture for signal improvement. Interestingly, one chapter describes the concept and design of self-powered biosensors derived from biofuel cells. Each topic is reviewed by experts very active in the field. This timely book is well suited for providing a good overview of current research trends devoted to electrochemical...

Electrochemical H2O2 biosensor composed of myoglobin on MoS2 nanoparticle-graphene oxide hybrid structure.

Science.gov (United States)

Yoon, Jinho; Lee, Taek; Bapurao G, Bharate; Jo, Jinhee; Oh, Byung-Keun; Choi, Jeong-Woo

2017-07-15

In this research, the electrochemical biosensor composed of myoglobin (Mb) on molybdenum disulfide nanoparticles (MoS 2 NP) encapsulated with graphene oxide (GO) was fabricated for the detection of hydrogen peroxide (H 2 O 2 ). Hybrid structure composed of MoS 2 NP and GO (GO@MoS 2 ) was fabricated for the first time to enhance the electrochemical signal of the biosensor. As a sensing material, Mb was introduced to fabricate the biosensor for H 2 O 2 detection. Formation and immobilization of GO@MoS 2 was confirmed by transmission electron microscopy, ultraviolet-visible spectroscopy, scanning electron microscopy, and scanning tunneling microscopy. Immobilization of Mb, and electrochemical property of biosensor were investigated by cyclic voltammetry and amperometric i-t measurements. Fabricated biosensor showed the electrochemical signal enhanced redox current as -1.86μA at an oxidation potential and 1.95μA at a reduction potential that were enhanced relative to those of electrode prepared without GO@MoS 2 . Also, this biosensor showed the reproducibility of electrochemical signal, and retained the property until 9 days from fabrication. Upon addition of H 2 O 2 , the biosensor showed enhanced amperometric response current with selectivity relative to that of the biosensor prepared without GO@MoS 2 . This novel hybrid material-based biosensor can suggest a milestone in the development of a highly sensitive detecting platform for biosensor fabrication with highly sensitive detection of target molecules other than H 2 O 2 . Copyright © 2016 Elsevier B.V. All rights reserved.

Undoped CVD diamond films for electrochemical applications

International Nuclear Information System (INIS)

Mosinska, Lidia; Fabisiak, Kazimierz; Paprocki, Kazimierz; Kowalska, Magdalena; Popielarski, Pawel; Szybowicz, Miroslaw

2013-01-01

By using different deposition conditions, the CVD diamond films with different qualities and orientation were grown by the hot-filament CVD technique. The object of this article is to summarize and discuss relation between structural, physical and electrochemical properties of different diamond electrodes. The physical properties of the Hot Filament CVD microcrystalline diamond films are analyzed by scanning electron microscopy and Raman spectroscopy. In presented studies two different electrodes were used of the diamond grain sizes around 200 nm and 10 μm, as it was estimated from SEM picture. The diamond layers quality was checked on basis of FWHM (Full width at Half Maximum) of 1332 cm −1 diamond Raman peak. The ratio of sp 3 /sp 2 carbon bonds was determined by 1550 cm −1 G band and 1350 cm −1 D band in the Raman spectrum. The electrochemical properties were analyzed using (CV) cyclic voltammetry measurements in aqueous solutions. The sensitivity of undoped diamond electrodes depends strongly on diamond film quality and concentration of amorphous carbon phase in the diamond layer

Zinc oxide nanostructures for electrochemical cortisol biosensing

Science.gov (United States)

Vabbina, Phani Kiran; Kaushik, Ajeet; Tracy, Kathryn; Bhansali, Shekhar; Pala, Nezih

2014-05-01

In this paper, we report on fabrication of a label free, highly sensitive and selective electrochemical cortisol immunosensors using one dimensional (1D) ZnO nanorods (ZnO-NRs) and two dimensional nanoflakes (ZnO-NFs) as immobilizing matrix. The synthesized ZnO nanostructures (NSs) were characterized using scanning electron microscopy (SEM), selective area diffraction (SAED) and photoluminescence spectra (PL) which showed that both ZnO-NRs and ZnO-NFs are single crystalline and oriented in [0001] direction. Anti-cortisol antibody (Anti-Cab) are used as primary capture antibodies to detect cortisol using electrochemical impedance spectroscopy (EIS). The charge transfer resistance increases linearly with increase in cortisol concentration and exhibits a sensitivity of 3.078 KΩ. M-1 for ZnO-NRs and 540 Ω. M -1 for ZnO-NFs. The developed ZnO-NSs based immunosensor is capable of detecting cortisol at 1 pM. The observed sensing parameters are in physiological range. The developed sensors can be integrated with microfluidic system and miniaturized potentiostat to detect cortisol at point-of-care.

Scanning Tunneling Spectroscope Use in Electrocatalysis Testing

Science.gov (United States)

Knutsen, Turid

2010-01-01

The relationship between the electrocatalytic properties of an electrode and its ability to transfer electrons between the electrode and a metallic tip in a scanning tunneling microscope (STM) is investigated. The alkaline oxygen evolution reaction (OER) was used as a test reaction with four different metallic glasses, Ni78Si8B14, Ni70Mo20Si5B5, Ni58Co20Si10B12, and Ni25Co50Si15B10, as electrodes. The electrocatalytic properties of the electrodes were determined. The electrode surfaces were then investigated with an STM. A clear relationship between the catalytic activity of an electrode toward the OER and its tunneling characteristics was found. The use of a scanning tunneling spectroscope (STS) in electrocatalytic testing may increase the efficiency of the optimization of electrochemical processes.

Scanning Tunneling Spectroscope Use in Electrocatalysis Testing

Directory of Open Access Journals (Sweden)

Turid Knutsen

2010-06-01

Full Text Available The relationship between the electrocatalytic properties of an electrode and its ability to transfer electrons between the electrode and a metallic tip in a scanning tunneling microscope (STM is investigated. The alkaline oxygen evolution reaction (OER was used as a test reaction with four different metallic glasses, Ni78Si8B14, Ni70Mo20Si5B5, Ni58Co20Si10B12, and Ni25Co50Si15B10, as electrodes. The electrocatalytic properties of the electrodes were determined. The electrode surfaces were then investigated with an STM. A clear relationship between the catalytic activity of an electrode toward the OER and its tunneling characteristics was found. The use of a scanning tunneling spectroscope (STS in electrocatalytic testing may increase the efficiency of the optimization of electrochemical processes.

Surface x-ray scattering and scanning tunneling microscopy studies at the Au(111) electrode

International Nuclear Information System (INIS)

Ocko, B.M.; Magnussen, O.M.; Wang, J.X.; Adzic, R.R.

1993-01-01

This chapter reviews Surface X-ray Scattering and Scanning Tunneling Microscopy results carried out at the Au(111) surface under electrochemical conditions. Results are presented for the reconstructed surface, and for bromide and thallium monolayers. These examples are used to illustrate the complementary nature of the techniques

Imprinted electrochemical sensor for dopamine recognition and determination based on a carbon nanotube/polypyrrole film

International Nuclear Information System (INIS)

Kan Xianwen; Zhou Hong; Li Chen; Zhu Anhong; Xing Zonglan; Zhao Zhe

2012-01-01

An electrochemical sensor combining a molecular imprinted technique and an electropolymerization method was developed in this work. A molecular imprinted polymer (MIP) film was fabricated by electropolymerizing pyrrole in the presence of dopamine (DA) after electrodepositing carboxyl-functionalized multi-walled carbon nanotubes (MWNTs-COOH) onto a glassy carbon electrode (GCE) surface. Scanning electron microscopy (SEM), differential pulse voltammetry (DPV), and electrochemical impedance spectroscopy (EIS) were employed to characterize the constructed sensor. The effects of pH, the monomer concentration, the number of cycles for the electropolymerization, and the scan rate for the sensor preparation were optimized. The MIP-based sensor displayed an excellent recognition capacity toward DA compared with other structurally similar molecules. Additionally, the DPV peak current was linear to the DA concentration in the range from 6.25 × 10 −7 to 1 × 10 −4 mol/L, with a detection limit of 6 × 10 −8 mol/L. The prepared sensor also showed stable reproducibility and regeneration capacity.

Electrochemical behavior of thin anodic oxide films on Zircaloy-4: Role of the mobile defects

International Nuclear Information System (INIS)

Salot, R.; Lefebvre-Joud, F.; Baroux, B.

1996-01-01

The first stages of the electrochemical oxidation of Zircaloy-4 are investigated using simple electrochemical tests and modeling the passive film modifications occurring as a result of contact with the electrolyte. Variations in electrode potential (open-circuit conditions) or current density (potentiodynamic scans) can be simply explained by a high field (F ∼ 10 6 V/cm) assisted passive film growth. Under open-circuit conditions, this field does not vary with exposure time (in the 2 h to 48 h range). The minimum electric field for the onset of high-field behavior is also evaluated and found smaller than the theoretical value which can be explained by a variation in the concentration of mobile defects throughout the film. Measurements of the electrode potential decay after a potentiodynamic scan confirm this model, allowing interpretation of the film modification as a combination of two separate phenomena: film growth under a high electric field and point defect annihilation

Improvement in tribological properties of atmospheric plasma-sprayed WC-Co coating followed by Cu electrochemical impregnation

International Nuclear Information System (INIS)

Yuan Jianhui; Zhu Yingchun; Zheng Xuebing; Ruan Qichao; Ji Heng

2009-01-01

The WC-Co coating obtained by atmospheric plasma spraying (APS) was modified by Cu electrochemical impregnation. The copper has infiltrated into and filled up the pores in WC-Co coating. The tribological properties of the coating against the stainless steel ball as sliding pairs were investigated with a ball-on-disc (BOD) configuration in air at room temperature. The as-prepared samples were characterized by means of optical microscope, scanning electron microscope and X-ray diffraction. It was found that the frictional behavior of the WC-Co coating followed by Cu electrochemical impregnation was superior to that of WC-Co coating. The wear mechanism of the WC-Co coating followed by Cu electrochemical impregnation was microcutting, whilst that of a WC-Co coating was the fatigue wear. The improvement in tribological properties of the WC-Co coating followed by Cu electrochemical impregnation was attributed to the formation of self-lubricating Cu film on the wear surface which induces the transformation of wear mechanism.

Preparation of iron-deposited graphite surface for application as cathode material during electrochemical vat-dyeing process

International Nuclear Information System (INIS)

Anbu Kulandainathan, M.; Kiruthika, K.; Christopher, G.; Babu, K. Firoz; Muthukumaran, A.; Noel, M.

2008-01-01

Iron-deposited graphite surfaces were prepared, characterized and employed as cathode materials for electrochemical vat-dyeing process containing very low concentration of sodium dithionite. The electrodeposition, in presence of ammonium thiocyanate and gelatin or animal glue as binding additives, were found to give finer iron deposits for improved electrochemical dyeing application. The electrodeposits were characterized using scanning electron microscopy, electron-dispersive X-ray spectroscopy and X-ray diffraction methods, before and after electrochemical dyeing process. The electrochemical activity of the iron-deposited graphite electrodes always stored in water seems to depend on the surface-bound Fe 3+ /Fe 2+ redox species. Vat dyes like C.I. Vat Violet 1, C.I. Vat Green 1 and C.I. Vat Blue 4 could be efficiently dyed employing these above electrode materials. The colour intensity and washing fastness of the dyed fabrics were found to be equal with conventionally dyed fabrics. The electrodes could also be reused for the dyeing process

Electrochemical Deposition and Dissolution of Thallium from Sulfate Solutions

Directory of Open Access Journals (Sweden)

Ye. Zh. Ussipbekova

2015-01-01

Full Text Available The electrochemical behavior of thallium was studied on glassy carbon electrodes in sulfate solutions. Cyclic voltammetry was used to study the kinetics of the electrode processes and to determine the nature of the limiting step of the cathodic reduction of thallium ions. According to the dependence of current on stirring rate and scan rate, this process is diffusion limited. Chronocoulometry showed that the electrodeposition can be performed with a current efficiency of up to 96% in the absence of oxygen.

Electrochemical corrosion behavior of Ni-containing hypoeutectic Al-Si alloy

Directory of Open Access Journals (Sweden)

Abul Hossain

2015-12-01

Full Text Available Electrochemical corrosion characteristics of the thermally treated 2 wt % Ni-containing Al-6Si-0.5Mg alloy were studied in NaCl solutions. The corrosion behavior of thermally treated (T6 Al-6Si-0.5Mg (-2Ni alloys in 0.1 M NaCl solution was investigated by electrochemical potentiodynamic polarization technique consisting of linear polarization method using the fit of Tafel plot and electrochemical impedance spectroscopy (EIS techniques. Generally, linear polarization experiments revealed a decrease of the corrosion rate at thermal treated Al-6Si-0.5Mg-2Ni alloy. The EIS test results showed that there is no significant change in charge transfer resistance (Rct after addition of Ni to Al-6Si-0.5Mg alloy. The magnitude of the positive shift in the open circuit potential (OCP, corrosion potential (Ecorr and pitting corrosion potential (Epit increased with the addition of Ni to Al-6Si-0.5Mg alloy. The forms of corrosion in the studied Al-6Si-0.5Mg alloy (except Al-6Si-0.5Mg-2Ni alloy are pitting corrosion as obtained from the scanning electron microscopy (SEM study.

Molecularly imprinted electrochemical sensor based on nickel nanoparticle-modified electrodes for phenobarbital determination

International Nuclear Information System (INIS)

Yu, Hui Cheng; Huang, Xue Yi; Lei, Fu Hou; Tan, Xue Cai; Wei, Yi Chun; Li, Hao

2014-01-01

Highlights: • Uniform Ni nanoparticles were synthesized. • A Ni nanoparticle-modified imprinted sensor was developed to detect phenobarbital. • The modified sensor exhibited high sensitivity for phenobarbital. • The electrochemical properties of the modified sensor were investigated. • The prepared sensor was applied to detect phenobarbital in fish samples. - Abstract: Uniform nickel nanoparticles were applied to improve the sensitivity of sensors for phenobarbital (PB) determination. A Ni nanoparticle-modified imprinted electrochemical sensor was developed by thermal polymerization with the use of methacrylic acid as the functional monomer and ethylene glycol maleic rosinate acrylate as the crosslinking agent. The chemical structures and morphologies of the imprinted films were characterized using Fourier transform infrared spectroscopy and scanning electron microscopy. The success of the fabrication of Ni nanoparticles, as well as the Ni nanoparticle-modified imprinted electrochemical sensor, was confirmed by the analytical results. The electrochemical properties of the modified molecularly imprinted and non-imprinted polymer sensors were investigated by cyclic voltammetry, differential pulse voltammetry, electrochemical impedance spectroscopy, and chronoamperometry. Results showed that the electrochemical properties of the molecularly imprinted sensor were remarkably different from those of the non-imprinted sensor. Linear responses of the imprinted sensor to PB were observed for concentrations ranging from 1.4 × 10 −7 mol L −1 to 1.3 × 10 −4 mol L −1 (r 2 = 0.9976), with a detection limit of 8.2 × 10 −9 mol L −1 (S/N = 3). The imprinted electrochemical sensor was used to determine PB in actual fish samples, in which average recoveries between 95.60% and 104.67% were achieved. The developed Ni nanoparticle-modified electrochemical sensor exhibited high sensitivity, high selectivity, and good recovery

Electrochemical energy generation

International Nuclear Information System (INIS)

Kreysa, G.; Juettner, K.

1993-01-01

The proceedings encompass 40 conference papers belonging to the following subject areas: Baseline and review papers; electrochemical fuel cells; batteries: Primary and secondary cells; electrochemical, regenerative systems for energy conversion; electrochemical hydrogen generation; electrochemistry for nuclear power plant; electrochemistry for spent nuclear fuel reprocessing; energy efficiency in electrochemical processes. There is an annex listing the authors and titles of the poster session, and compacts of the posters can be obtained from the office of the Gesellschaft Deutscher Chemiker, Abteilung Tagungen. (MM) [de

Development of three-electrode type micro-electrochemical reactor on anodized aluminum with photon rupture and electrochemistry

International Nuclear Information System (INIS)

Sakairi, Masatoshi; Yamada, Masashi; Kikuchi, Tastuya; Takahashi, Hideaki

2007-01-01

Photon rupture with a focused single pulse of pulsed YAG-laser irradiation was used to fabricate an aluminum electrochemical micro-reactor. Porous type anodic oxide film formed on aluminum specimens was irradiated in solutions with a pulsed Nd-YAG laser beam through a convex lens to fabricate micro-channels, micro-electrode, and through holes (for reference electrode, solution inlet, and outlet). During irradiation, specimens were moved by a computer controlled XYZ stage. After irradiation, the surface of the micro-channel and through hole were again treated to form anodic oxide film and the surface of the micro-electrode was treated electrochemically to provide an Au layer. The calculated volume of the micro-reactor including micro-channel and through holes is about 1.5 μl. The cyclic voltammogram of the micro-electrochemical cell was measured in K 3 Fe(CN) 6 /K 4 Fe(CN) 6 with both static and flowing solution at different scanning rates. The anodic and cathodic peak currents were measured and the values depended on scanning rate and ion concentration when the solution was static. With the flowing solution, limiting currents were observed and the anodic limiting current was increased with the cubic root of the solution flow rate

Optical and structural properties of porous zinc oxide fabricated via electrochemical etching method

International Nuclear Information System (INIS)

Ching, C.G.; Lee, S.C.; Ooi, P.K.; Ng, S.S.; Hassan, Z.; Hassan, H. Abu; Abdullah, M.J.

2013-01-01

Highlights: • Hillock like porous structure zinc oxide was obtained via electrochemical etching. • Anisotropic dominance etching process by KOH etchant. • Reststrahlen features are sensitive to multilayer porous structure. • Determination of porosity from IR reflectance spectrum. -- Abstract: We investigated the optical and structural properties of porous zinc oxide (ZnO) thin film fabricated by ultraviolet light-assisted electrochemical etching. This fabrication process used 10 wt% potassium hydroxide solution as an electrolyte. Hillock-like porous ZnO films were successfully fabricated according to the field emission scanning electron microscopy results. The cross-sectional study of the sample indicated that anisotropic-dominated etching process occurred. However, the atomic force microscopic results showed an increase in surface roughness of the sample after electrochemical etching. A resonance hump induced by the porous structure was observed in the infrared reflectance spectrum. Using theoretical modeling technique, ZnO porosification was verified, and the porosity of the sample was determined

Improved electrochemical performance of hierarchical porous carbon/polyaniline composites

International Nuclear Information System (INIS)

Hu Juan; Wang Huanlei; Huang Xiao

2012-01-01

Highlights: ► Polyaniline-coated hierarchical porous carbon (HPC) composites have been synthesized by in situ polymerization. ► The HPC/polyaniline composite has significantly better electrochemical capacitance performance than pure HPC and polyaniline. ► The amount of polyaniline loading has a significant effect on the composites’ electrochemical performances. - Abstract: Polyaniline (PANI)-coated hierarchical porous carbon (HPC) composites (HPC/PANI) for use as supercapacitor electrodes were prepared by in situ chemical oxidation polymerization at 273 K of an aniline solution containing well-dispersed HPC particles. After polymerization, a thin layer of PANI was coated on the surface of the HPC particles, which was confirmed by Fourier transform infrared spectroscopy (FT-IR), transmission electron microscope (TEM) and scanning electron microscopy (SEM). Compared to pure PANI and HPC, the electrochemical capacitance performance of the composites was significantly improved. The highest specific capacitance of the composites obtained is 478 F g −1 at 1 mV s −1 , which is more than twice as that of pure PANI and three times as that of pure HPC. Because of the influence from the hierarchical pore structure of the carbon material, the calculated specific capacitance of PANI in the composite (pseudocapacitance contribution from PANI) is almost one magnitude higher than that of pure PANI.

Synthesis, Characterization, and Electrochemical Properties of Polyaniline Thin Films

Science.gov (United States)

Rami, Soukaina

Conjugated polymers have been used in various applications (battery, supercapacitor, electromagnetic shielding, chemical sensor, biosensor, nanocomposite, light-emitting-diode, electrochromic display etc.) due to their excellent conductivity, electrochemical and optical properties, and low cost. Polyaniline has attracted the researchers from all disciplines of science, engineering, and industry due to its redox properties, environmental stability, conductivity, and optical properties. Moreover, it is a polymer with fast electroactive switching and reversible properties displayed at low potential, which is an important feature in many applications. The thin oriented polyaniline films have been fabricated using self-assembly, Langmuir-Blodgett, in-situ self-assembly, layer-by-layer, and electrochemical technique. The focus of this thesis is to synthesize and characterize polyaniline thin films with and without dyes. Also, the purpose of this thesis is to find the fastest electroactive switching PANI electrode in different electrolytic medium by studying their electrochemical properties. These films were fabricated using two deposition techniques: in-situ self-assembly and electrochemical deposition. The characterization of these films was done using techniques such as Fourier Transform Infrared Spectroscopy (FTIR), UV-spectroscopy, Scanning Electron Microscope (SEM), and X-Ray Diffraction (XRD). FTIR and UV-spectroscopy showed similar results in the structure of the polyaniline films. However, for the dye incorporated films, since there was an addition in the synthesis of the material, peak locations shifted, and new peaks corresponding to these materials appeared. The 1 layer PANI showed compact film morphology, comparing to other PANI films, which displayed a fiber-like structure. Finally, the electrochemical properties of these thin films were studied using cyclic voltammetry (CV), chronoamperometry (CA), and electrochemical impedance spectroscopy (EIS) in

Electrochemical assisted photocatalytic degradation of salicylic acid with highly ordered TiO{sub 2} nanotube electrodes

Energy Technology Data Exchange (ETDEWEB)

Zhang, Qian [The State Key Laboratory of Multiphase Flow in Power Engineering, Xi’an Jiaotong University, Xi’an 710049 (China); Zhu, Jinwei [China Aerospace Science and Technology Corporation Fourty-fourth Research Institution (China); Wang, Ying; Feng, Jiangtao [Department of Environmental Science and Engineering, Xi’an Jiaotong University, Xi’an 710049 (China); Yan, Wei, E-mail: yanwei@mail.xjtu.edu.cn [The State Key Laboratory of Multiphase Flow in Power Engineering, Xi’an Jiaotong University, Xi’an 710049 (China); Department of Environmental Science and Engineering, Xi’an Jiaotong University, Xi’an 710049 (China); Xu, Hao, E-mail: xuhao@mail.xjtu.edu.cn [Department of Environmental Science and Engineering, Xi’an Jiaotong University, Xi’an 710049 (China)

2014-07-01

To explore the kinetics of photoelectrocatalytic degradation of salicylic acid, one of the important PPCPs, highly ordered TiO{sub 2} nanotube arrays (NTs) were prepared by the electrochemical anodization and characterized with scanning electron microscopy and X-ray diffraction techniques. The effect of TiO{sub 2} NTs properties, bias potential, initial salicylic acid concentration and solution pH on the degradation efficiency was studied and carefully analyzed. The results revealed that the salicylic acid degradation follows quasi-first order kinetics in the photoelectrocatalytic process, and the fastest decay kinetics was achieved in acidic environment (pH 2). The result was further interpreted through the electrochemical impedance spectroscopy. It is confirmed that the electrochemical assisted photocatalysis is a synergetic approach to combat stable organic substances with improved efficiency.

Quasi-reference electrodes in confined electrochemical cells can result in in situ production of metallic nanoparticles.

Science.gov (United States)

Perera, Rukshan T; Rosenstein, Jacob K

2018-01-31

Nanoscale working electrodes and miniaturized electroanalytical devices are valuable platforms to probe molecular phenomena and perform chemical analyses. However, the inherent close distance of metallic electrodes integrated into a small volume of electrolyte can complicate classical electroanalytical techniques. In this study, we use a scanning nanopipette contact probe as a model miniaturized electrochemical cell to demonstrate measurable side effects of the reaction occurring at a quasi-reference electrode. We provide evidence for in situ generation of nanoparticles in the absence of any electroactive species and we critically analyze the origin, nucleation, dissolution and dynamic behavior of these nanoparticles as they appear at the working electrode. It is crucial to recognize the implications of using quasi-reference electrodes in confined electrochemical cells, in order to accurately interpret the results of nanoscale electrochemical experiments.

The role of alternating current in photo-assisted electrochemical porosification of GaN

International Nuclear Information System (INIS)

Ainorkhilah, Mahmood; Naser, M. Ahmed; Yushamdan, Yusof; Kwong, Yam Fong; Zainuriah, Hassan; Tiginyanu, Ion; Siang, Chuah Lee

2013-01-01

In this paper, we report the formation of porous GaN films under a novel alternating current (sine-wave a.c. (50 Hz)) photo-assisted electrochemical (ACPEC) etching conditions. The ACPEC formed porous GaN with excellent structural and surface morphology. Field emission scanning electron microscope (FESEM), atomic force microscopy (AFM) and high resolution X-ray diffraction (HR-XRD) phi-scan and rocking curves measurements evidenced important features of the pore morphology and nanostructures. According to the FESEM micrographs, the spatial nano architecture of the porous structures exhibits pores with perfect hexagonal shape. The AFM measurements revealed an increase in the surface roughness induced by porosification. X-ray diffraction phi-scan showed that porous GaN sample maintained the epitaxial. (authors)

Characterization of manganese dioxide electrodeposited by pulse and direct current for electrochemical capacitor

International Nuclear Information System (INIS)

Adelkhani, H.; Ghaemi, M.

2010-01-01

This paper describes the electrochemical capacitor behavior of manganese dioxide (MD, MnO 2 ) samples that were prepared by direct current (DCMD) and pulse current (PCMD) electrodeposition. The capacitive characteristics of the samples were studied in 0.5 M aqueous Na 2 SO 4 solution using the cyclic voltammetry (CV) method. Scanning electron microscopy (SEM), X-ray diffraction (XRD), chemical composition analyses and the Barrett-Joyner-Halenda (BJH) method were employed to characterize the samples. In the study of the effect of scan rate on capacitance, it was revealed that PCMD displayed higher capacities than DCMD for all scan rates. The higher capacitive performance of PCMD was attributed to its porosity (specific surface area, pore volume, and pore-size distribution), chemical composition and structural properties.

Addition of nitrite enhances the electrochemical defluorination of 2-fluoroaniline

Energy Technology Data Exchange (ETDEWEB)

Feng, Huajun [School of Environmental Science and Engineering, Zhejiang Gongshang University, Hangzhou 310012 (China); Zhejiang Provincial Key Laboratory of Solid Waste Treatment and Recycling, Hangzhou 310012 (China); Laboratory of Microbial Ecology and Technology, Ghent University, Coupure Links 653, B-9000 Ghent (Belgium); Liang, Yuxiang [School of Environmental Science and Engineering, Zhejiang Gongshang University, Hangzhou 310012 (China); Zhejiang Provincial Key Laboratory of Solid Waste Treatment and Recycling, Hangzhou 310012 (China); Guo, Kun [Laboratory of Microbial Ecology and Technology, Ghent University, Coupure Links 653, B-9000 Ghent (Belgium); Long, Yuyang [School of Environmental Science and Engineering, Zhejiang Gongshang University, Hangzhou 310012 (China); Zhejiang Provincial Key Laboratory of Solid Waste Treatment and Recycling, Hangzhou 310012 (China); Cong, Yanqing, E-mail: yqcong@hotmail.com [School of Environmental Science and Engineering, Zhejiang Gongshang University, Hangzhou 310012 (China); Shen, Dongsheng [School of Environmental Science and Engineering, Zhejiang Gongshang University, Hangzhou 310012 (China); Zhejiang Provincial Key Laboratory of Solid Waste Treatment and Recycling, Hangzhou 310012 (China)

2015-12-30

Highlights: • A method for improving defluorination performance by in situ self-assembly of pollutants was developed. • The mechanisms of 2-FA modification and defluorination are discussed. • Positively-charged diazonium salt is used to weaken the C–F bond. - Abstract: This study introduces a novel approach that uses the interaction of pollutants with added nitrite to produce diazonium salts, which cause in situ self-assembly of the pollutants on carbon electrodes, to improve their 2-fluoroaniline (2-FA) defluorination and removal performance. The 2-FA degradation performance, electrode properties, electrochemical properties and degradation pathway were investigated. The reactor containing NO{sub 2}{sup −} achieved a 2-FA removal efficiency of 90.1% and a defluorination efficiency of 38% within 48 h, 1.4 and 2.3 times higher than the corresponding results achieved without NO{sub 2}{sup −}, respectively. The residual NO{sub 2}{sup −} was less than 0.5 mg/L in the reactor containing added NO{sub 2}{sup −}, which would not cause serious secondary pollution. Scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) results proved that the carbon anode surface was successfully modified with benzene polymer, and electrochemical tests confirmed that the electrochemical activity of the modified anode was enhanced significantly. The C–F bond was weakened by the effect of the positive charge of the benzenediazonium groups, and the high electrochemical activity of the carbon anode enhanced the electrochemical performance of the system to accelerate defluorination. Thus, the present electrical method involving nitrite nitrogen is very promising for the treatment of wastewater containing fluoroaniline compounds.

Electrochemical corrosion behavior of a Ti-35Nb alloy for medical prostheses

International Nuclear Information System (INIS)

Cremasco, Alessandra; Osorio, Wislei R.; Freire, Celia M.A.; Garcia, Amauri; Caram, Rubens

2008-01-01

Since the 1980s, the titanium alloys show attractive properties for biomedical applications where the most important factors are, firstly, biocompatibility, corrosion and mechanical resistances, low modulus of elasticity, very good strength to weight ratio, reasonable formability and osseointegration. The aim of this study was to investigate the effects of two different heat treatments; furnace cooling and water quenching, on the general electrochemical corrosion resistance of Ti-35 wt%Nb alloy samples immersed in a 0.9% NaCl (0.15 mol L -1 ) solution at 25 deg. C and neutral pH range. The samples were obtained using a non-consumable tungsten electrode furnace with a water-cooled copper hearth under argon atmosphere. The microstructural pattern was examined by scanning electron microscopy (SEM) and X-ray diffractometry (XRD). In order to evaluate the electrochemical corrosion behavior of such Ti-Nb alloy samples, corrosion tests were performed by using electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization curves. Analyses of an equivalent circuit have also been used to provide quantitative support for the discussions and understanding of the corrosion behavior. It was found that water quenching provides a microstructural pattern consisting of an alpha-martensite acicular phase which decreases the material electrochemical performance due to the stress-induced martensitic transformation

Electrochemical corrosion behavior of a Ti-35Nb alloy for medical prostheses

Energy Technology Data Exchange (ETDEWEB)

Cremasco, Alessandra [Department of Materials Engineering, State University of Campinas, UNICAMP, P.O. Box 6122, 13083-970 Campinas, SP (Brazil); Osorio, Wislei R. [Department of Materials Engineering, State University of Campinas, UNICAMP, P.O. Box 6122, 13083-970 Campinas, SP (Brazil)], E-mail: wislei@fem.unicamp.br; Freire, Celia M.A.; Garcia, Amauri; Caram, Rubens [Department of Materials Engineering, State University of Campinas, UNICAMP, P.O. Box 6122, 13083-970 Campinas, SP (Brazil)

2008-05-30

Since the 1980s, the titanium alloys show attractive properties for biomedical applications where the most important factors are, firstly, biocompatibility, corrosion and mechanical resistances, low modulus of elasticity, very good strength to weight ratio, reasonable formability and osseointegration. The aim of this study was to investigate the effects of two different heat treatments; furnace cooling and water quenching, on the general electrochemical corrosion resistance of Ti-35 wt%Nb alloy samples immersed in a 0.9% NaCl (0.15 mol L{sup -1}) solution at 25 deg. C and neutral pH range. The samples were obtained using a non-consumable tungsten electrode furnace with a water-cooled copper hearth under argon atmosphere. The microstructural pattern was examined by scanning electron microscopy (SEM) and X-ray diffractometry (XRD). In order to evaluate the electrochemical corrosion behavior of such Ti-Nb alloy samples, corrosion tests were performed by using electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization curves. Analyses of an equivalent circuit have also been used to provide quantitative support for the discussions and understanding of the corrosion behavior. It was found that water quenching provides a microstructural pattern consisting of an alpha-martensite acicular phase which decreases the material electrochemical performance due to the stress-induced martensitic transformation.

Electrochemical characterization of pulsed layer deposited hydroxyapatite-zirconia layers on Ti-21Nb-15Ta-6Zr alloy for biomedical application

Energy Technology Data Exchange (ETDEWEB)

Izquierdo, Javier [Department of Chemistry, Universidad de La Laguna, P.O. Box 456, E-38200 La Laguna, Tenerife (Spain); Bolat, Georgiana [“Gheorghe Asachi” Technical University of Iasi, Faculty of Chemical Engineering and Environmental Protection, 73 Prof. Dr. Doc. D. Mangeron Street, 700050 Iasi (Romania); Cimpoesu, Nicanor [“Gheorghe Asachi” Technical University of Iasi, Faculty of Materials Science, 61-63 Prof. Dr. Doc. D. Mangeron Street, 700050 Iasi (Romania); Trinca, Lucia Carmen [Science Department, University of Agricultural Sciences and Veterinary Medicine, M. Sadoveanu Alley 3, 700490 Iasi (Romania); Mareci, Daniel, E-mail: danmareci@yahoo.com [“Gheorghe Asachi” Technical University of Iasi, Faculty of Chemical Engineering and Environmental Protection, 73 Prof. Dr. Doc. D. Mangeron Street, 700050 Iasi (Romania); Souto, Ricardo Manuel, E-mail: rsouto@ull.es [Department of Chemistry, Universidad de La Laguna, P.O. Box 456, E-38200 La Laguna, Tenerife (Spain); Institute of Material Science and Nanotechnology, Universidad de La Laguna, E-38200 La Laguna, Tenerife (Spain)

2016-11-01

Highlights: • New quarternary Ti-based alloy for biomaterial application. • Combined hydroxyapatite-zirconia coating produced by pulsed laser deposition. • Porous layer formed on the coated alloy blocks electron transfer reactions. • Electrochemical behaviour consistent with passive film with duplex structure. • HA–ZrO{sub 2} coated Ti-21Nb-15Ta-6Zr exhibits high potential for osseointegration. - Abstract: A new titanium base Ti-21Nb-15Ta-6Zr alloy covered with hydroxyapatite-zirconia (HA–ZrO{sub 2}) by pulsed laser deposition (PLD) technique was characterized regarding its corrosion resistance in simulated physiological Ringer’s solution at 37 °C. For the sake of comparison, Ti-6Al-4V standard implant alloy, with and without hydroxyapatite-zirconia coating, was also characterized. Multiscale electrochemical analysis using both conventional averaging electrochemical techniques, namely electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization, and spatially-resolved microelectrochemical techniques (scanning electrochemical microscopy, SECM) were used to investigate the electrochemical behaviour of the materials. In addition, scanning electron microscopy evidenced that no relevant surface morphology changes occurred on the materials upon immersion in the simulated physiological solution, despite variations in their electrochemical behaviour. Although uncoated metals appear to show better performances during conventional corrosion tests, the response is still quite similar for the HA–ZrO{sub 2} coated materials while providing superior resistance towards electron transfer due to the formation of a more dense film on the surface, thus effectively behaving as a passive material. It is believed corrosion of the HA–ZrO{sub 2} coated Ti-21Nb-15Ta-6Zr alloy will have negligible effect upon biochemical and cellular events at the bone-implant interface and could facilitate osseointegration.

Asymmetric electrochemical supercapacitor, based on polypyrrole coated carbon nanotube electrodes

International Nuclear Information System (INIS)

Su, Y.; Zhitomirsky, I.

2015-01-01

Highlights: • Polypyrrole (PPy) coated multiwalled carbon nanotubes (MWCNT) were prepared. • New method is based on the use of new electrochemically active dopants for PPy. • The dopans provided dispersion of MWCNT and promoted PPy coating formation. • Symmetric PPy–MWCNT supercapacitors showed high capacitance and low resistance. • Asymmetric PPy–MWCNT/VN–MWCNT devices and modules allowed larger voltage window. - Abstract: Conductive polypyrrole (PPy) polymer – multiwalled carbon nanotubes (MWCNT) composites were synthesized using sulfanilic acid azochromotrop (SPADNS) and sulfonazo III sodium salt (CHR-BS) as anionic dopants for chemical polymerization of PPy. The composites were tested for application in electrodes of electrochemical supercapacitors (ES). Sedimentation tests, electrophoretic deposition experiments and Fourier transform infrared spectroscopy (FTIR) investigations showed that strong adsorption of anionic CHR-BS on MWCNT provided MWCNT dispersion. The analysis of scanning and transmission electron microscopy data demonstrated that the use of CHR-BS allowed the formation of PPy coatings on MWCNT. As a result, the composites, prepared using CHR-BS, showed higher capacitance, compared to the composites, prepared using SPADNS. The electrodes, containing MWCNT, coated with PPy showed a capacitance of 179 F g −1 for active mass loading of 10 mg cm −2 , good capacitance retention at scan rates in the range of 2–100 mV s −1 and excellent cyclic stability. Asymmetric ES devices, containing positive PPy–MWCNT electrodes and negative vanadium nitride (VN)–MWCNT electrodes showed significant improvement in energy storage performance, compared to the symmetric ES due to the larger voltage window. The low impedance and high capacitance of the individual cells paved the way to the development of modules with higher voltage, which showed good electrochemical performance

Fabrication of silver tips for scanning tunneling microscope induced luminescence.

Science.gov (United States)

Zhang, C; Gao, B; Chen, L G; Meng, Q S; Yang, H; Zhang, R; Tao, X; Gao, H Y; Liao, Y; Dong, Z C

2011-08-01

We describe a reliable fabrication procedure of silver tips for scanning tunneling microscope (STM) induced luminescence experiments. The tip was first etched electrochemically to yield a sharp cone shape using selected electrolyte solutions and then sputter cleaned in ultrahigh vacuum to remove surface oxidation. The tip status, in particular the tip induced plasmon mode and its emission intensity, can be further tuned through field emission and voltage pulse. The quality of silver tips thus fabricated not only offers atomically resolved STM imaging, but more importantly, also allows us to perform challenging "color" photon mapping with emission spectra taken at each pixel simultaneously during the STM scan under relatively small tunnel currents and relatively short exposure time.

CONCEPTUAL APPROACH OF COMPETITIVENESS AND INTERDEPENDENCE BETWEEN COMPETITION AND COMPETITIVENESS

Directory of Open Access Journals (Sweden)

Tatiana GUTIUM

2017-11-01

Full Text Available This article is devoted to analysis of interdependence and correlation between competition and competitiveness, and competition’s consequences. The author analysed some authors’ visions on competitiveness, and common features between theories of competition and competitiveness. Using the synthetic indicator elaborated by author has been evaluated the competitiveness of domestic goods on the internal and external market. At the end of this article, the author has developed proposals to increase competitiveness.

Morphology and electrical properties of electrochemically synthesized pyrrole–formyl pyrrole copolymer

Energy Technology Data Exchange (ETDEWEB)

Gholami, Mehrdad, E-mail: mehrdad897@um.edu.my [Department of Chemistry, University of Malaya, Kuala Lumpur 50603 (Malaysia); Department of Chemistry, Marvdasht Branch, Islamic Azad University, P.O. Box 465, Marvdasht (Iran, Islamic Republic of); Nia, Pooria Moozarm, E-mail: pooriamn@yahoo.com [Department of Chemistry, University of Malaya, Kuala Lumpur 50603 (Malaysia); Alias, Yatimah, E-mail: yatimah70@um.edu.my [Department of Chemistry, University of Malaya, Kuala Lumpur 50603 (Malaysia)

2015-12-01

Graphical abstract: - Highlights: • The (Py–co-FPy) copolymer was synthesized electrochemically. • This copolymer has 1.6 times higher surface coverage compared to polypyrrole. • This copolymer showed 2.5 times lower resistance compared to polypyrrole. • The conjugated structure between Py and FPy causes enhancement of conductivity. • This conducting copolymer has a strong potential to be used in various applications. - Abstract: A direct electrochemical copolymerization of pyrrole–formyl pyrrole (Py–co-FPy) was carried out by oxidative copolymerization of formyl pyrrole and pyrrole in LiClO{sub 4} aqueous solution through galvanostatic method. The (Py–co-FPy) copolymer was characterized using Fourier-transform infrared spectroscopy (FT-IR), field emission scanning electron microscope (FESEM), energy-filtering transmission electron microscope (EFTEM), thermal gravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The FESEM images showed that the synthesized copolymer had a hollow whelk-like helixes structure, which justifies the enhancement of charge transportation through the copolymer film. Cyclic voltammetry studies revealed that the electrocatalytic activity of synthesized copolymer has improved and the surface coverage in copolymer enhanced 1.6 times compared to polypyrrole alone. Besides, (Py–co-FPy) copolymer showed 2.5 times lower electrochemical charge transfer resistance (R{sub ct}) value in impedance spectroscopy. Therefore, this copolymer has a strong potential to be used in several applications such as sensor applications.

Observation of a Ag protrusion on a Ag2S island using a scanning tunneling microscope

Directory of Open Access Journals (Sweden)

Takeo Ohno

2015-01-01

Full Text Available A silver sulfide (Ag2S island as an ionic conductor in resistive switching memories was formed and a protrusion of silver from the Ag2S formed by an electrochemical reaction was observed using a scanning tunneling microscope.

Surface treatment influences electrochemical stability of cpTi exposed to mouthwashes

International Nuclear Information System (INIS)

Beline, Thamara; Garcia, Camila S.; Ogawa, Erika S.; Marques, Isabella S.V.; Matos, Adaias O.; Sukotjo, Cortino; Mathew, Mathew T.

2016-01-01

The role of surface treatment on the electrochemical behavior of commercially pure titanium (cpTi) exposed to mouthwashes was tested. Seventy-five disks were divided into 15 groups according to surface treatment (machined, sandblasted with Al 2 O 3 , and acid etched) and electrolyte solution (artificial saliva — control, 0.12% chlorhexidine digluconate, 0.05% cetylpyridinium chloride, 0.2% sodium fluoride, and 1.5% hydrogen peroxide) (n = 5). Open-circuit-potential and electrochemical impedance spectroscopy were conducted at baseline and after 7 and 14 days of immersion in each solution. Potentiodynamic test and total weight loss of disks were performed after 14 days of immersion. Scanning electron microscopy, energy dispersive spectroscopy, white light interferometry and profilometry were conducted for surface characterization before and after the electrochemical tests. Sandblasting promoted the lowest polarization resistance (R p ) (P < .0001) and the highest capacitance (CPE) (P < .006), corrosion current density (I corr ) and corrosion rate (P < .0001). In contrast, acid etching increased R p and reduced CPE, independent to the mouthwash; while hydrogen peroxide reduced R p (P < .008) and increased I corr and corrosion rate (P < .0001). The highest CPE values were found for hydrogen peroxide and 0.2% sodium fluoride. Immersion for longer period improved the electrochemical stability of cpTi (P < .05). In conclusion, acid etching enhanced the electrochemical stability of cpTi. Hydrogen peroxide and sodium fluoride reduced the resistance to corrosion of cpTi, independent to the surface treatment. Chlorhexidine gluconate and cetylpyridinium chloride did not alter the corrosive behavior of cpTi. - Highlights: • Acid etching enhanced the electrochemical stability of cpTi. • Hydrogen peroxide and sodium fluoride reduced the corrosion resistance of cpTi. • Chlorhexidine gluconate and cetylpyridinium chloride can be safely used.

Surface treatment influences electrochemical stability of cpTi exposed to mouthwashes

Energy Technology Data Exchange (ETDEWEB)

Beline, Thamara [Department of Prosthodontics and Periodontology, Piracicaba Dental School, University of Campinas (UNICAMP), Av Limeira, 901, Piracicaba, São Paulo 13414-903 (Brazil); IBTN/Br — Institute of Biomaterials, Tribocorrosion and Nanomedicine, Brazilian Branch (Brazil); Garcia, Camila S. [Department of Prosthodontics and Periodontology, Piracicaba Dental School, University of Campinas (UNICAMP), Av Limeira, 901, Piracicaba, São Paulo 13414-903 (Brazil); Ogawa, Erika S. [Department of Prosthodontics and Periodontology, Piracicaba Dental School, University of Campinas (UNICAMP), Av Limeira, 901, Piracicaba, São Paulo 13414-903 (Brazil); IBTN/Br — Institute of Biomaterials, Tribocorrosion and Nanomedicine, Brazilian Branch (Brazil); Marques, Isabella S.V. [Department of Prosthodontics and Periodontology, Piracicaba Dental School, University of Campinas (UNICAMP), Av Limeira, 901, Piracicaba, São Paulo 13414-903 (Brazil); Matos, Adaias O. [Department of Prosthodontics and Periodontology, Piracicaba Dental School, University of Campinas (UNICAMP), Av Limeira, 901, Piracicaba, São Paulo 13414-903 (Brazil); IBTN/Br — Institute of Biomaterials, Tribocorrosion and Nanomedicine, Brazilian Branch (Brazil); Sukotjo, Cortino [Department of Restorative Dentistry, University of Illinois at Chicago, College of Dentistry, 801 S Paulina, Chicago, IL 60612 (United States); IBTN — Institute of Biomaterials, Tribocorrosion and Nanomedicine (United States); Mathew, Mathew T. [IBTN — Institute of Biomaterials, Tribocorrosion and Nanomedicine (United States); Department of Orthopedic Surgery, Rush University Medical Center, 1611 W Harrison, Chicago, IL 60612 (United States); and others

2016-02-01

The role of surface treatment on the electrochemical behavior of commercially pure titanium (cpTi) exposed to mouthwashes was tested. Seventy-five disks were divided into 15 groups according to surface treatment (machined, sandblasted with Al{sub 2}O{sub 3}, and acid etched) and electrolyte solution (artificial saliva — control, 0.12% chlorhexidine digluconate, 0.05% cetylpyridinium chloride, 0.2% sodium fluoride, and 1.5% hydrogen peroxide) (n = 5). Open-circuit-potential and electrochemical impedance spectroscopy were conducted at baseline and after 7 and 14 days of immersion in each solution. Potentiodynamic test and total weight loss of disks were performed after 14 days of immersion. Scanning electron microscopy, energy dispersive spectroscopy, white light interferometry and profilometry were conducted for surface characterization before and after the electrochemical tests. Sandblasting promoted the lowest polarization resistance (R{sub p}) (P < .0001) and the highest capacitance (CPE) (P < .006), corrosion current density (I{sub corr}) and corrosion rate (P < .0001). In contrast, acid etching increased R{sub p} and reduced CPE, independent to the mouthwash; while hydrogen peroxide reduced R{sub p} (P < .008) and increased I{sub corr} and corrosion rate (P < .0001). The highest CPE values were found for hydrogen peroxide and 0.2% sodium fluoride. Immersion for longer period improved the electrochemical stability of cpTi (P < .05). In conclusion, acid etching enhanced the electrochemical stability of cpTi. Hydrogen peroxide and sodium fluoride reduced the resistance to corrosion of cpTi, independent to the surface treatment. Chlorhexidine gluconate and cetylpyridinium chloride did not alter the corrosive behavior of cpTi. - Highlights: • Acid etching enhanced the electrochemical stability of cpTi. • Hydrogen peroxide and sodium fluoride reduced the corrosion resistance of cpTi. • Chlorhexidine gluconate and cetylpyridinium chloride can be safely used.

Electrochemical characterization of azo dye (E)-1-(4-((4-(phenylamino)phenyl)diazenyl)phenyl)ethanone (DPA)

International Nuclear Information System (INIS)

Surucu, Ozge; Abaci, Serdar; Seferoğlu, Zeynel

2016-01-01

Highlights: • Electrochemical characterization of azo dye DPA was performed. • Pencil graphite electrode was used as working electrode. • Cyclic voltammetry was used to determine the effect of scan rate and pH. • Chronoamperometry was used to determine diffusion constant. • Square wave voltammetry verified the results of cyclic voltammetry. - Abstract: An enormous range of possible dyes are available, especially as the starting molecules are readily available and cheap. As other dye classes become less viable from either an environmental or economic reasons, azo dyes come to the forefront. Therefore, electrochemical characterization of a novel synthesized azo dye (E)-1-(4-((4-(phenylamino) phenyl)diazenyl)phenyl)ethanone was achieved for the first time. Cyclic voltammetry, chronoamperometry and square wave voltammetry techniques were used to investigate the electrochemical behavior and electrocatalytic effect of azo dye (E)-1-(4-((4-(phenylamino) phenyl)diazenyl)phenyl)ethanone at pencil graphite electrode. Cyclic voltammograms were utilized to determine the effect of scan rate and pH on the peak current and peak potential. Chronoamperometry technique was used to determine diffusion constant, D and the type of adsorption isotherms. The kinetics parameters which were the apparent electron transfer rate constant, k s and charge transfer coefficient, α were calculated. Square wave voltammetry was used to verify responses of cyclic voltammetry technique.

Fabrication of hematite (α-Fe{sub 2}O{sub 3}) nanoparticles using electrochemical deposition

Energy Technology Data Exchange (ETDEWEB)

Meng, Qingling; Wang, Zuobin, E-mail: wangz@cust.edu.cn; Chai, Xiangyu; Weng, Zhankun; Ding, Ran; Dong, Litong

2016-04-15

Graphical abstract: - Highlights: • Cathodic electrochemical deposition proposed to fabricate hematite nanoparticles. • Hematite nanoparticles were fabricated on indium-tin-oxide coated glass substrates. • The size and shape of nanoparticles were determined by deposition conditions. • The nanoparticles were well decentralized for different potential applications. • Electrochemical deposition is a useful approach in fabricating nanoparticles. - Abstract: In this work, cathodic electrochemical deposition was proposed to fabricate reproducible and homogeneous hematite (α-Fe{sub 2}O{sub 3}) nanoparticles on indium-tin-oxide (ITO) films. The α-Fe{sub 2}O{sub 3} nanoparticles, which were quasi-hexagonally shaped, were deposited in an aqueous mixture of FeCl{sub 2} and FeCl{sub 3} at the temperatures 16.5 °C, 40 °C and 60 °C. The electrochemically deposited α-Fe{sub 2}O{sub 3} nanoparticles showed excellent stability and good crystallinity. The α-Fe{sub 2}O{sub 3} nanoparticles were characterized by Raman spectroscope and X-ray diffractometer (XRD). A scanning electron microscope (SEM) was used to measure the size and shape of the nanoparticles. The experiment results have shown that the size and shape of nanoparticles were determined by electrochemical deposition conditions including the deposition time, current density, reaction temperature and solution concentration. The proposed electrochemical deposition method has been proven to be a cost-effective, environment friendly and highly efficient approach in fabricating well decentralized α-Fe{sub 2}O{sub 3} nanoparticles for different potential applications.

Self-assembled hierarchical graphene/polyaniline hybrid aerogels for electrochemical capacitive energy storage

International Nuclear Information System (INIS)

Yang, Fan; Xu, Maowen; Bao, Shu-Juan; Wei, Hua; Chai, Hui

2014-01-01

In this work, polyaniline nanowires (PANI-NWs) act as spacers, incorporated with graphene oxide and self-assembled into graphene/PANI hybrid aerogels through a facile hydrothermal route. The as-synthesized samples have been characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectra, X-ray photoelectron spectroscopy (XPS), contact angle measurement, field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) for their microstructure, morphology and relative affinities toward water. Cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) measurements have been used to study the effects of composition, microstructure and morphology of the samples on their capacitive performance. The experimental results indicate that the PANI can effectively tailor the microstructures and electrochemical performances of the products. The as-prepared materials with an appropriate proportion of PANI nanowires can efficiently prevent the adjacent graphene sheets from aggregation and provide fast ionic channels for electrochemical energy storage. A specific capacitance of 520.3 F g −1 has been achieved from graphene/PANI hybrid aerogel, which also exhibits excellent cycling stability

Polycarbonate-based ordered arrays of electrochemical nanoelectrodes obtained by e-beam lithography

Energy Technology Data Exchange (ETDEWEB)

Moretto, L M; De Leo, M; Ugo, P [Department of Molecular Sciences and Nanosystems, University Ca' Foscari of Venice, Santa Marta 2137, 30123 Venice (Italy); Tormen, M; Carpentiero, A, E-mail: ugo@unive.it [CNR-IOM, TASC Laboratory, Basovizza S S 14 km 163.5, 34149 Trieste (Italy)

2011-05-06

Ordered arrays of nanoelectrodes for electrochemical use are prepared by electron beam lithography (EBL) using polycarbonate as a novel e-beam resist. The nanoelectrodes are fabricated by patterning arrays of holes in a thin film of polycarbonate spin-coated on a gold layer on Si/Si{sub 3}N{sub 4} substrate. Experimental parameters for the successful use of polycarbonate as high resolution EBL resist are optimized. The holes can be filled partially or completely by electrochemical deposition of gold. This enables the preparation of arrays of nanoelectrodes with different recession degree and geometrical characteristics. The polycarbonate is kept on-site and used as the insulator that separates the nanoelectrodes. The obtained nanoelectrode arrays (NEAs) exhibit steady state current controlled by pure radial diffusion in cyclic voltammetry for scan rates up to approximately 50 mV s{sup -1}. Electrochemical results showed satisfactory agreement between experimental voltammograms and suitable theoretical models. Finally, the peculiarities of NEAs versus ensembles of nanoelectrodes, obtained by membrane template synthesis, are critically evaluated.

Electrochemical fabrication of a novel conducting metallopolymer nanoparticles and its electrocatalytic application

International Nuclear Information System (INIS)

Kazemi, Sayed Habib; Mohamadi, Rahim

2013-01-01

Graphical abstract: Nanoparticles of nickel-curcumin conducting polymer (Ni-Curc-NPs) were fabricated by a two steps electrochemical method. In the first step, nickel source was immobilized at the electrode surface in the form of nickel nanoparticles (NiNPs). Then, electropolymerization of Ni-curcumin was performed at the NiNPs modified electrode. These nanostructures were successfully employed for electrooxidative determination of glucose and significant increase in the electrochemical sensitivity and lower limit of detection were observed. -- Highlights: • A novel two steps method for fabrication of nickel-curcumin conducting polymer was described. • Nickel-curcumine nanoparticles were easily prepared instead of thin film. • Ni-Curc-NPs modified electrode was successfully employed for electrooxidation of glucose. • Significant improvement in the sensitivity and limit of detection was observed. -- Abstract: Present article is the first example of a novel two step electrochemical route for fabrication of nanoparticles of conducting metallopolymer of Ni-curcumin (Ni-Curc-NPs). Firstly, nickel nanoparticles (Ni-NPs) were electrochemically deposited on the electrode surface. Then, electropolymerization of Ni-Curc-NPs were performed at the electrode modified with Ni-NPs. These nanostructures were characterized using electrochemical methods including cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and hydrodynamic amperometry, also surface analysis methods and electron microscopy including energy dispersive analysis of X-ray (EDAX), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). Additionally, application of the Ni-Curc-NPs modified electrode toward glucose electrooxidation was examined. A lower limit of detection and enhanced dynamic linear range for determination of glucose were observed at Ni-Curc-NPs modified electrode compared to Ni-NPs modified electrode

Electrochemically Deposited Polypyrrole for Dye-Sensitized Solar Cell Counter Electrodes

Directory of Open Access Journals (Sweden)

Khamsone Keothongkham

2012-01-01

Full Text Available Polypyrrole films were coated on conductive glass by electrochemical deposition (alternative current or direct current process. They were then used as the dye-sensitized solar cell counter electrodes. Scanning electron microscopy revealed that polypyrrole forms a nanoparticle-like structure on the conductive glass. The amount of deposited polypyrrole (or film thickness increased with the deposition duration, and the performance of polypyrrole based-dye-sensitized solar cells is dependant upon polymer thickness. The highest efficiency of alternative current and direct current polypyrrole based-dye-sensitized solar cells (DSSCs is 4.72% and 4.02%, respectively. Electrochemical impedance spectroscopy suggests that the superior performance of alternative current polypyrrole solar cells is due to their lower charge-transfer resistance between counter electrode and electrolyte. The large charge-transfer resistance of direct current solar cells is attributed to the formation of unbounded polypyrrole chains minimizing the I3 − reduction rate.

Metabolic lung scanning with N-isopropyl-I-123-p-iodoamphetamine

International Nuclear Information System (INIS)

Touya, J.; Akber, S.F.; Rashimian, J.; Bennett, L.R.

1982-01-01

The mechanisms of uptake of N-Isopropyl-I-123-p-Iodoamphetamine (IMP) in the lung was studied in dogs. It has been concluded that this amine is taken in low specificity - high capacity endothelial receptors. Competitive effect of propranolol guanethidine, amphetamine and ketanine for the binding sites of IMP in the pulmonary endothelial cells was observed. These results show that IMP can be an agent for nonparticulate lung perfusion scans as well as for metabolic lung scans

NEW INSIGTHS ON THE KINETICS AND MECHANISM OF THE ELECTROCHEMICAL OXIDATION OF DICLOFENAC IN NEUTRAL AQUEOUS MEDIUM

International Nuclear Information System (INIS)

Cid-Cerón, M.M.; Guzmán-Hernández, D.S.; Ramírez-Silva, M.T.; Galano, A.; Romero-Romo, M.; Palomar-Pardavé, M.

2016-01-01

Highlights: • DCF electrochemical oxidation was studied from aqueous solution with a CPE. • Both stagnant and forced convection conditions were considered. • We found DCF electrochemical oxidation is a mass transfer-controlled process. • An EC mechanism was found where the electrodic is quasi-reversible. • C reaction provokes the breaking up the DCF through the nitrogen atom. • DCF diffusion coefficient was experimental and theoretically calculated. - Abstract: The diclofenac (DCF) electrochemical oxidation mechanism was studied through: linear voltammetry (LV), chronoamperometry (CA) sampled-current voltammetry (SCV), potentiostatic coulometry (PC) cyclic voltammetry (CV) under stagnant conditions and linear voltammetry under forced convection conditions (FCLV) over a carbon paste electrode (CPE) from an aqueous medium containing 0.1 M phosphate buffer at pH 7. It was found that the DCF electrochemical oxidation involves an EC mechanism, where the electrochemical reaction is carried out through a one electron-exchange while the chemical reaction involves breaking up the DCF through the nitrogen atom, thereby generating the fragments 2,6 dichloroaniline and 2-(2hydroxyprop-2-enyl)phenol. Reverting the potential scan in the cathodic direction at different scan rates and regardless of its rate, after the oxidation peak, it was found that it was possible to reduce only 38% of the DCF oxidized. The spectrophotometric study carried out during different macro-electrolysis periods allowed observing that the current decrease of the oxidation peak coupled to the DCF absorption (at 270 nm), together with the development of a new spectrophotometric absorption maximum (450 nm), all confirm the EC mechanism proposed. With the use of several experimental techniques (CA, LV and FCLV) and theoretical ones using the Stokes–Einstein approach, the DCF diffusion coefficient was determined, this being in average 8.1 × 10"−"6 cm"2 s"−"1.

Lamellar-crossing-structured Ni(OH){sub 2}/CNTs/Ni(OH){sub 2} nanocomposite for electrochemical supercapacitor materials

Energy Technology Data Exchange (ETDEWEB)

Wu, Qingnan [Department of Chemistry, State Key Laboratory of Pollution Control and Resource Reuse, Tongji University, Shanghai 200092 (China); Wen, Ming, E-mail: m_wen@tongji.edu.cn [Department of Chemistry, State Key Laboratory of Pollution Control and Resource Reuse, Tongji University, Shanghai 200092 (China); Shanghai Key Lab of Chemical Assessment and Sustainability, Tongji University, Shanghai 200092 (China); Chen, Shipei [Department of Chemistry, State Key Laboratory of Pollution Control and Resource Reuse, Tongji University, Shanghai 200092 (China); Wu, Qingsheng [Department of Chemistry, State Key Laboratory of Pollution Control and Resource Reuse, Tongji University, Shanghai 200092 (China); Shanghai Key Lab of Chemical Assessment and Sustainability, Tongji University, Shanghai 200092 (China)

2015-10-15

Ni(OH){sub 2}/CNTs/Ni(OH){sub 2} lamellar-crossing-nanostructure with a single lamellar spacing of ∼5 nm was effectively constructed through two-phase-interface reaction process followed by the CNTs crossed among the lamellar-nanostructured Ni(OH){sub 2}. The resultant nanocomposite can offer large active surface areas and short diffusion paths for electrons and ions, and is investigated as a potential pseudocapacitor electrode material for electrochemical energy storage applications. Electrochemical data demonstrate that the as-prepared nanocomposite exhibits a high specific capacitance of ∼1600 F g{sup −1} at the scan rate of 1 mV s{sup −1} in 6 M KOH solution at normal pressure and temperature, which is great higher than Ni(OH){sub 2} (∼1200 F g{sup −1}). Furthermore, Ni(OH){sub 2}/CNTs/Ni(OH){sub 2} nanocomposite shows a higher energy density (∼125 Wh kg{sup −1}, 2 A g{sup −1}) and has a slightly decrease of 5% in specific capacitance after 1000 continuous charge/discharge cycles. - Graphical abstract: As-constructed Ni(OH){sub 2}/CNTs/Ni(OH){sub 2} lamellar-crossing-nanostructure exhibits remarkable enhancement in electrochemical stability and high specific capacity of ∼1600 F g{sup −1} at a scan rate of 1 mV s{sup −1}, suggesting promising potential for supercapacitor applications. - Highlights: • New designed lamellar-crossing-structured Ni(OH){sub 2}/CNTs/Ni(OH){sub 2} nanocomposites have been firstly reported in this work. • Ni(OH){sub 2}/CNTs/Ni(OH){sub 2} lamellar-crossing-nanostructures show firm nanostructure and excellent electrochemical stability. • Ni(OH){sub 2}/CNTs/Ni(OH){sub 2} nanocomposites exhibit excellent specific capacitance. • Ni(OH){sub 2}/CNTs/Ni(OH){sub 2} nanocomposites have the potential application in electrochemical energy storage applications.

In situ anodization of aluminum surfaces studied by x-ray reflectivity and electrochemical impedance spectroscopy

International Nuclear Information System (INIS)

Bertram, F.; Evertsson, J.; Messing, M. E.; Mikkelsen, A.; Lundgren, E.; Zhang, F.; Pan, J.; Carlà, F.; Nilsson, J.-O.

2014-01-01

We present results from the anodization of an aluminum single crystal [Al(111)] and an aluminum alloy [Al 6060] studied by in situ x-ray reflectivity, in situ electrochemical impedance spectroscopy and ex situ scanning electron microscopy. For both samples, a linear increase of oxide film thickness with increasing anodization voltage was found. However, the slope is much higher in the single crystal case, and the break-up of the oxide film grown on the alloy occurs at a lower anodization potential than on the single crystal. The reasons for these observations are discussed as are the measured differences observed for x-ray reflectivity and electrochemical impedance spectroscopy.

Structural and electrochemical properties of single crystalline MoV 2O8 nanowires for energy storage devices

KAUST Repository

Shahid, Muhammad; Liu, Jingling; Ali, Zahid; Shakir, Imran; Warsi, Muhammad Farooq

2013-01-01

We report the synthesis of MoV2O8 nanowires of high quality using spin coating followed by the thermal annealing process. Transmission electron microscopy (TEM) reveals the average diameter of synthesized nanowire about 100 nm, and average length ranges from 1 to 5 μm. The TEM analysis further confirms the <001> growth direction of MoV 2O8 nanowires. The electrochemical properties of synthesized nanowires using cyclic voltammetry show the specific capacitance 56 Fg-1 at the scan rate of 5 mV s-1 that remains 24 Fg -1 at 100 mV s-1. The electrochemical measurements suggest that the MoV2O8 nanowires can be used as a material for the future electrochemical capacitors (energy storage devices). © 2012 Published by Elsevier Inc. All rights reserved.

Structural and electrochemical properties of single crystalline MoV 2O8 nanowires for energy storage devices

KAUST Repository

Shahid, Muhammad

2013-05-01

We report the synthesis of MoV2O8 nanowires of high quality using spin coating followed by the thermal annealing process. Transmission electron microscopy (TEM) reveals the average diameter of synthesized nanowire about 100 nm, and average length ranges from 1 to 5 μm. The TEM analysis further confirms the <001> growth direction of MoV 2O8 nanowires. The electrochemical properties of synthesized nanowires using cyclic voltammetry show the specific capacitance 56 Fg-1 at the scan rate of 5 mV s-1 that remains 24 Fg -1 at 100 mV s-1. The electrochemical measurements suggest that the MoV2O8 nanowires can be used as a material for the future electrochemical capacitors (energy storage devices). © 2012 Published by Elsevier Inc. All rights reserved.

Electrochemically Controlled Ion-exchange Property of Carbon Nanotubes/Polypyrrole Nanocomposite in Various Electrolyte Solutions

Energy Technology Data Exchange (ETDEWEB)

Choi, Daiwon [Pacific Northwest National Laboratory, 902 Battelle Boulevard P.O. Box 999 Richland WA 99352 USA; Zhu, Chengzhou [School of Mechanical and Materials Engineering, Washington State University, Pullman, Washington 99164-2920 United States; Fu, Shaofang [School of Mechanical and Materials Engineering, Washington State University, Pullman, Washington 99164-2920 United States; Du, Dan [School of Mechanical and Materials Engineering, Washington State University, Pullman, Washington 99164-2920 United States; Engelhard, Mark H. [Pacific Northwest National Laboratory, 902 Battelle Boulevard P.O. Box 999 Richland WA 99352 USA; Lin, Yuehe [Pacific Northwest National Laboratory, 902 Battelle Boulevard P.O. Box 999 Richland WA 99352 USA; School of Mechanical and Materials Engineering, Washington State University, Pullman, Washington 99164-2920 United States

2016-09-15

The electrochemically controlled ion-exchange properties of multi-wall carbon nanotube (MWNT)/electronically conductive polypyrrole (PPy) polymer composite in the various electrolyte solutions have been investigated. The ion-exchange behavior, rate and capacity of the electrochemically deposited polypyrrole with and without carbon nanotube (CNT) were compared and characterized using cyclic voltammetry (CV), chronoamperometry (CA), electrochemical quartz crystal microbalance (EQCM), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). It has been found that the presence of carbon nanotube backbone resulted in improvement in ion-exchange rate, stability of polypyrrole, and higher anion loading capacity per PPy due to higher surface area, electronic conductivity, porous structure of thin film, and thinner film thickness providing shorter diffusion path. Chronoamperometric studies show that electrically switched anion exchange could be completed more than 10 times faster than pure PPy thin film. The anion selectivity of CNT/PPy film is demonstrated using X-ray photoelectron spectroscopy (XPS).

Electrochemical deposition of magnesium from analogous ionic liquid based on dimethylformamide

International Nuclear Information System (INIS)

Wang, Huaiyou; Jia, Yongzhong; Wang, Xiaohua; Yao, Ying; Yue, Duyuan; Jing, Yan

2013-01-01

In this paper, a homogeneous, colorless analogous ionic liquid containing dimethylformamide (DMF) and magnesium chloride hexahydrate is synthesized. The conductivity of analogous ionic liquid is measured as a function of temperature and composition. Irreversible electrochemical behavior was generally observed by cyclic voltammetry (CV) in the analogous ionic liquid based electrolytes containing simple Mg salt. CV also shows that the reducing reaction of Mg 2+ is a diffusion control process. Electrochemical impedance spectroscopy (EIS) of analogous ionic liquid was measured at 20 °C, 40 °C and 60 °C. Electrodeposition of magnesium metal from analogous ionic liquid has been studied. The Mg deposits are also systematically characterized by the techniques of powder X-ray diffraction (XRD), scanning electron microscope (SEM) and energy dispersive spectroscopy (EDS). Results showed that magnesium was found in the deposited film

One step paired electrochemical synthesis of iron and iron oxide nanoparticles

Directory of Open Access Journals (Sweden)

Ordoukhanian Juliet

2016-09-01

Full Text Available In this study, a new one step paired electrochemical method is developed for simultaneous synthesis of iron and iron oxide nanoparticles. iron and iron oxide are prepared as cathodic and anodic products from iron (ii sulfate aqueous solution in a membrane divided electrolytic cell by the pulsed current electrosynthesis. Because of organic solvent-free and electrochemical nature of the synthesis, the process could be considered as green and environmentally friendly. The reduction of energy consumption and low cost are the other significant advantages of this new method that would have a great application potential in the chemical industry. The nanostructure of prepared samples was characterized by Fourier transform infrared spectroscopy (FT-IR, X-ray diffraction (XRD, scanning electron microscopy (SEM and transmission electron microscopy (TEM. The magnetic properties were studied by vibrating sample magnetometer (VsM.

Electrochemical catalytic activity of tungsten trioxide- modified graphite felt toward VO2+/VO2+ redox reaction

International Nuclear Information System (INIS)

Shen, Yang; Xu, Hongfeng; Xu, Pengcheng; Wu, Xiaoxin; Dong, Yiming; Lu, Lu

2014-01-01

A novel graphite felt electrode modified with tungsten trioxide (WO 3 ) was developed to improve the electrochemical performance of graphite felt toward the VO 2 + /VO 2+ redox pair. WO 3 was prepared using a hydrothermal method, and the morphology of WO 3 structures was investigated by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The electrochemical property of WO 3 -modified graphite felt toward VO 2 + /VO 2+ was carefully characterized using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) measurements. The hydrogen-vanadium redox flow battery (H-VRFB) test indicates that single cells using 1.1 mg cm −2 WO 3 -modified graphite felt exhibited excellent performance at 70 mA cm −2 , and the corresponding coulombic, voltage, and energy efficiencies were 99.1%, 88.66% and 87.86%, respectively

Electrochemically reduced graphene oxide-modified screen-printed carbon electrodes for a simple and highly sensitive electrochemical detection of synthetic colorants in beverages.

Science.gov (United States)

Jampasa, Sakda; Siangproh, Weena; Duangmal, Kiattisak; Chailapakul, Orawon

2016-11-01

A simple and highly sensitive electrochemical sensor based on an electrochemically reduced graphene oxide-modified screen-printed carbon electrode (ERGO-SPCE) for the simultaneous determination of sunset yellow (SY) and tartrazine (TZ) was proposed. An ERGO film was coated onto the electrode surface using a cyclic voltammetric method and then characterized by scanning electron microscopy (SEM). In 0.1M phosphate buffer at a pH of 6, the two oxidation peaks of SY and TZ appeared separately at 0.41 and 0.70V, respectively. Surprisingly, the electrochemical response remarkably increased approximately 90- and 20-fold for SY and TZ, respectively, using the modified electrode in comparison to the unmodified electrode. The calibration curves exhibited linear ranges from 0.01 to 20.0µM for SY and from 0.02 to 20.0µM for TZ. The limits of detection were found to be 0.50 and 4.50nM (at S/N=3) for SY and TZ, respectively. Furthermore, this detection platform provided very high selectivity for the measurement of both colorants. This electrochemical sensor was successfully applied to determine the amount of SY and TZ in commercial beverages. Comparison of the results obtained from this proposed method to those obtained by an in-house standard technique proved that this developed method has good agreement in terms of accuracy for practical applications. This sensor offers an inexpensive, rapid and sensitive determination. The proposed system is therefore suitable for routine analysis and should be an alternative method for the analysis of food colorants. Copyright © 2016 Elsevier B.V. All rights reserved.

The effect of recrystallization on corrosion and electrochemical behavior of 7150 Al alloy

Energy Technology Data Exchange (ETDEWEB)

Peng, G.S.; Chen, K.H.; Fang, H.C.; Chen, S.Y.; Chao, H. [State Key Laboratory for Powder Metallurgy, Central South University, Changsha, Hunan 410083 (China)

2011-01-15

By weight loss, potentiodynamic polarization, cyclic voltammetry, and electrochemical impedance spectroscopy (EIS) techniques complemented by optical and scanning electron microscopy observations, the effect of recrystallization on the corrosion, and electrochemical behavior of 7150 Al alloy was studied. The results indicated that the high recrystallization fraction 7150-1 was worse than the low recrystallization fraction 7150-2 on corrosion resistance. The analysis of EIS indicated that 7150-1 exhibited obvious pitting corrosion at 5 h immersion time, whereas 7150-2 showed no obvious pitting corrosion even at 33 h. The corrosion route developed along the grain boundary of recrystallization grains, not along the grain boundary of unrecrystallization grains. (Copyright copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Structure and electrochemical impedance of LiNi_xMn_2_-_xO_4

International Nuclear Information System (INIS)

Ta Anh Tan; Nguyen Si Hieu; Le Ha Chi; Pham Duy Long; Dang Tran Chien; Le Dinh Trong

2016-01-01

Ni-substitution spinel LiNi_xMn_2_-_xO_4 (x = 0, 0.1, 0.2) materials were synthesized by the sol--gel method. The structure and morphology of the samples were characterized by the X-ray diffraction (XRD) and the scanning electron microscopy. The ac conduction of the materials was investigated by electrochemical impedance spectroscopy (EIS) measurements. The refinement results showed that the substitution of Ni decreased the lattice constant and Mn--O distance, while increased Li--O bond length and 16c octahedral volume. The EIS results confirmed the decrease of conductivity with increasing Ni substitution content. Based on XRD and EIS results, the relationship between the crystal structure and electrochemical behavior of the materials was discussed and explained. (author)

On the possibility of electrochemical unzipping of multiwalled carbon nanotubes to produce graphene nanoribbons

Energy Technology Data Exchange (ETDEWEB)

Zehtab Yazdi, Alireza; Roberts, Edward P.L.; Sundararaj, Uttandaraman, E-mail: u.sundararaj@ucalgary.ca

2016-08-15

Highlights: • MWCNTs synthesized and electrochemically oxidized to study the formation of GNR • HRTEM, Raman and XPS confirmed no successful unzipping occurred after oxidation • Electrochemical oxidation very unlikely facilitate formation of intercalated MWCNTs - Abstract: Multiwalled carbon nanotubes (MWCNTs) with different geometrical characteristics and chemical doping have been synthesized and electrochemically oxidized to study the possibility of unzipping, and creating graphene nanoribbon (GNR) nanostructures. Modified glassy carbon electrodes of the MWCNTs have been tested in an aqueous electrolyte via anodic scans in a wide range of potentials, followed by keeping at the maximum potential for different times. The microstructural features, structural defects, and functional groups and their elements have been then studied using high resolution transmission electron microscopy (HRTEM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS), respectively. All results have confirmed that no successful unzipping occurs in the MWCNTs after electrochemical oxidation, even for the nitrogen-doped MWCNTs (CN{sub x}-MWCNTs) with reactive nitrogen groups and defective bamboo structures. In contrast to the report by Shinde et al. (J. Am. Chem. Soc. 2011, 133, 4168–4171), it has been concluded that the electrochemical oxidation in aqueous electrolytes is very unlikely to facilitate sufficient incorporation of the intercalated molecules among the walls of the MWCNTs. These molecules are, however, responsible for unzipping of MWCNTs.

Electrochemical characteristics of bioresorbable binary MgCa alloys in Ringer's solution: Revealing the impact of local pH distributions during in-vitro dissolution.

Science.gov (United States)

Mareci, D; Bolat, G; Izquierdo, J; Crimu, C; Munteanu, C; Antoniac, I; Souto, R M

2016-03-01

Biodegradable magnesium-calcium (MgCa) alloy is a very attractive biomaterial. Two MgCa alloys below the solid solubility of Ca were considered, as to solely investigate the effect of Ca content on the behavior of magnesium and the pH changes associated to metal dissolution. X-ray diffraction analysis and optical microscopy showed that both Mg-0.63Ca and Mg-0.89Ca alloys were solely composed of α(Mg) phase. Degradation characteristics and electrochemical characterization of MgCa alloys were investigated during exposure to Ringer's solution at 37 °C by electrochemical impedance spectroscopy and scanning electrochemical microscopy. The impedance behavior showed both capacitive and inductive features that are related to the alloy charge transfer reaction and the relaxation of the absorbed corrosion compounds, and can be described in terms of an equivalent circuit. Scanning electron microscopy (SEM) was employed to view the surface morphology of the MgCa samples after 1 week immersion in Ringer's solution showing extensive precipitation of corrosion products, whereas the substrate shows evidence of a non-uniform corrosion process. Energy dispersive analysis showed that the precipitates contained oxygen, calcium, magnesium and chlorine, and the Mg:Ca ratios were smaller than in the alloys. Scanning electrochemical microscopy (SECM) was used to visualize local pH changes associated to these physicochemical processes with high spatial resolution. The occurrence of pH variations in excess of 3 units between anodic and cathodic half-cell reactions was monitored in situ. Copyright © 2015 Elsevier B.V. All rights reserved.

Electrochemical capacitance characteristics of patterned ruthenium dioxide-carbon nanotube nanocomposites grown onto graphene

International Nuclear Information System (INIS)

Shih, Yi-Ting; Lee, Kuei-Yi; Huang, Ying-Sheng

2014-01-01

Highlights: • Graphene was grown on Cu foil by mobile thermal chemical vapor deposition system. • CNT was synthesized on graphene for RuO 2 nanostructure growth by thermal chemical vapor deposition system. • The CNT growth location was fixed through the use of photolithography technique, thereby increasing the specific area. • RuO 2 nanostructures were coated onto CNT bundle arrays through metal organic chemical vapor deposition, in order to utilize its pseudo capacitive property. - Abstract: In this study, graphene was used as a conductive substrate for vertically aligned carbon nanotube (CNT) bundle arrays growth, to be used as an electrode for electrochemical double layer capacitor (EDLC), as graphene and CNT exhibit good conductivity and excellent chemical stability. Both of them are composed of carbon, therefore making a superior adhesion between them. The configuration of bundle arrays provided a relatively higher specific surface area in contact with electrolyte, thereby resulting in demonstratively higher capacitance. Moreover, as the RuO 2 nanostructures have good pseudocapacitance characteristics, they were coated onto vertically aligned CNT bundle arrays in order to effectively enhance the EDLC performances. The characteristics of CNT/graphene, CNT bundle/graphene, and RuO 2 /CNT bundle/graphene electrodes were examined with the use of scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman spectroscopy. Furthermore, their electrochemical properties were investigated by an electrochemical analyzer. The specific capacitances of CNT/graphene, CNT bundle/graphene, and RuO 2 /CNT bundle/graphene were 4.64, 6.65, and 128.40 F/g at the scan rate of 0.01 V/s, respectively

Tuning the physico-electrochemical properties of novel cobalt (II) octa[(3,5-biscarboxylate)-phenoxy] phthalocyanine complex using phenylamine-functionalised SWCNTs

CSIR Research Space (South Africa)

Agboola, BO

2010-03-01

Full Text Available OBPPc-SWCNT-phenylamine hybrid were evaluated using spectroscopy (IR and UV–vis), field emission scanning electron microscopy and electrochemistry (cyclic voltammetry and electrochemical impedance spectroscopy). Integration of SWCNT-phenylamine resulted in the physical...

Electrochemical behaviour of gamma hydroxybutyric acid at a platinum electrode in acidic medium

International Nuclear Information System (INIS)

Jiménez-Pérez, R.; Sevilla, J.M.; Pineda, T.; Blázquez, M.; González-Rodríguez, J.

2013-01-01

Highlights: • This is the first reported electrochemical study of the behaviour of GHB. • The first study of the interaction of GHB on solid electrodes. • The GHB oxidation process in platinum electrodes is a complex process. • Re-dissolution and reduction of Pt oxides and oxidation of the GHB OH group. • The oxidation process is also influenced by pH and GHB concentration. -- Abstract: The electrooxidation of gamma hydroxybutyric acid (GHB) on a polycrystalline platinum electrode is studied by cyclic voltammetry in acidic medium. Two oxidation peaks, A and B, are obtained in the positive scan within the potential range of the double layer region and of the platinum oxide region, respectively. In the negative going potential sweep an inverted oxidation peak with an onset partially overlapping with the tail of the cathodic peak for the reduction of the platinum oxide formed during the anodic scan is obtained (peak C). This inverted peak can be observed at a potential close to +0.2 V (vs Ag/AgCl at pH 2) and separated 0.4 and 0.8 V from the two other oxidation peaks obtained during the anodic scan and in such conditions that the surface is particularly activated to favour this electrochemical process. The response obtained in the electronic current for the different peaks when GHB concentration and scan rate were changed to allows inferring that these are the result of a potential dependent mechanism. The behaviour observed is according with the oxidation of the alcohol group to the corresponding aldehyde and carboxylic acid (succinic acid) as main products

Spectro-electrochemical and DFT study of tenoxicam metabolites formed by electrochemical oxidation

International Nuclear Information System (INIS)

Ramírez-Silva, M.T.; Guzmán-Hernández, D.S.; Galano, A.; Rojas-Hernández, A.; Corona-Avendaño, S.; Romero-Romo, M.; Palomar-Pardavé, M.

2013-01-01

Highlights: • Tenoxicam deprotonation and electrochemical oxidation were studied. • Both spectro-electrochemical and theoretical DFT studies were considered. • It was found that the ampholitic species of tenoxicam is a zwitterion. • Electrochemical oxidation of tenoxicam yields two non-electroactive products. • The nature of these fragments was further confirmed by a chromatography study. -- Abstract: From experimental (spectro-electrochemical) and theoretical (DFT) studies, the mechanisms of tenoxicam deprotonation and electrochemical oxidation were assessed. From these studies, new insights on the nature of the ampholitic species involved during tenoxicam's deprotonation in aqueous solution are presented; see scheme A. Moreover, it is shown that, after the analysis of two different reaction schemes that involve up to 10 different molecules and 12 reaction paths, the electrochemical oxidation of tenoxicam, yields two non-electroactive products that are predominately formed by its fragmentation, after the loss of two electrons. The nature of these fragments was further confirmed by a chromatography study

Electrochemical performance of Li4Mn5O12 nano-crystallites prepared by spray-drying-assisted solid state reactions

International Nuclear Information System (INIS)

Jiang, Y.P.; Xie, J.; Cao, G.S.; Zhao, X.B.

2010-01-01

Nanosized Li 4 Mn 5 O 12 has been synthesized by a spray-drying-assisted solid state method. The effect of spray drying and drying temperature on the microstructure and electrochemical performance of the final products has been investigated. The microstructure of the products has been characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The electrochemical performance of the products has been studied by galvanostatic cycling, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). It has been found that the products prepared with a spray-drying pretreatment of the precursor exhibit a smaller grain size and a narrower size distribution than that prepared without the pretreatment. Among the three samples with a precursor pretreatment, that pretreated at 250 o C shows the best electrochemical performance due to the smallest grain size of below 50 nm and the narrowest size distribution.

Simultaneous measurement and quantitation of 4-hydroxyphenylacetic acid and dopamine with fast-scan cyclic voltammetry.

Science.gov (United States)

Shin, Mimi; Kaplan, Sam V; Raider, Kayla D; Johnson, Michael A

2015-05-07

Caged compounds have been used extensively to investigate neuronal function in a variety of preparations, including cell culture, ex vivo tissue samples, and in vivo. As a first step toward electrochemically measuring the extent of caged compound photoactivation while also measuring the release of the catecholamine neurotransmitter, dopamine, fast-scan cyclic voltammetry at carbon-fiber microelectrodes (FSCV) was used to electrochemically characterize 4-hydroxyphenylacetic acid (4HPAA) in the absence and presence of dopamine. 4HPAA is a by-product formed during the process of photoactivation of p-hydroxyphenacyl-based caged compounds, such as p-hydroxyphenylglutamate (pHP-Glu). Our data suggest that the oxidation of 4HPAA occurs through the formation of a conjugated species. Moreover, we found that a triangular waveform of -0.4 V to +1.3 V to -0.4 V at 600 V s(-1), repeated every 100 ms, provided an oxidation current of 4HPAA that was enhanced with a limit of detection of 100 nM, while also allowing the detection and quantitation of dopamine within the same scan. Along with quantifying 4HPAA in biological preparations, the results from this work will allow the electrochemical measurement of photoactivation reactions that generate 4HPAA as a by-product as well as provide a framework for measuring the photorelease of electroactive by-products from caged compounds that incorporate other chromophores.

Synthesis and electrochemical study of Pt-based nanoporous materials

International Nuclear Information System (INIS)

Wang Jingpeng; Holt-Hindle, Peter; MacDonald, Duncan; Thomas, Dan F.; Chen Aicheng

2008-01-01

In the present work, a variety of Pt-based bimetallic nanostructured materials including nanoporous Pt, Pt-Ru, Pt-Ir, Pt-Pd and Pt-Pb networks have been directly grown on titanium substrates via a facile hydrothermal method. The as-fabricated electrodes were characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, X-ray diffraction and electrochemical methods. The active surface areas of these nanoporous Pt-based alloy catalysts are increased by over 68 (Pt-Pd), 69 (Pt-Ru) and 113 (Pt-Ir) fold compared to a polycrystalline Pt electrode. All these synthesized nanoporous electrodes exhibit superb electrocatalytic performance towards electrochemical oxidation of methanol and formic acid. Among the five nanoporous Pt-based electrodes, the Pt-Ir shows the highest peak current density at +0.50 V, with 68 times of enhancement compared to the polycrystalline Pt for methanol oxidation, and with 86 times of enhancement in formic acid oxidation; whereas the catalytic activity of the nanoporous Pt-Pb electrode outperforms the other materials in formic acid oxidation at the low potential regions, delivering an enhanced current density by 280-fold compared to the polycrystalline Pt at +0.15 V. The new approach described in this study is suitable for synthesizing a wide range of bi-metallic and tri-metallic nanoporous materials, desirable for electrochemical sensor design and potential application in fuel cells

Synthesis and electrochemical study of Pt-based nanoporous materials

Energy Technology Data Exchange (ETDEWEB)

Wang Jingpeng [Department of Chemistry, Lakehead University, Thunder Bay, Ontario P7B 5E1 (Canada); Department of Chemistry, University of Guelph, Guelph, Ontario N1G 2W1 (Canada); Holt-Hindle, Peter; MacDonald, Duncan [Department of Chemistry, Lakehead University, Thunder Bay, Ontario P7B 5E1 (Canada); Thomas, Dan F. [Department of Chemistry, University of Guelph, Guelph, Ontario N1G 2W1 (Canada); Chen Aicheng [Department of Chemistry, Lakehead University, Thunder Bay, Ontario P7B 5E1 (Canada)], E-mail: aicheng.chen@lakeheadu.ca

2008-10-01

In the present work, a variety of Pt-based bimetallic nanostructured materials including nanoporous Pt, Pt-Ru, Pt-Ir, Pt-Pd and Pt-Pb networks have been directly grown on titanium substrates via a facile hydrothermal method. The as-fabricated electrodes were characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, X-ray diffraction and electrochemical methods. The active surface areas of these nanoporous Pt-based alloy catalysts are increased by over 68 (Pt-Pd), 69 (Pt-Ru) and 113 (Pt-Ir) fold compared to a polycrystalline Pt electrode. All these synthesized nanoporous electrodes exhibit superb electrocatalytic performance towards electrochemical oxidation of methanol and formic acid. Among the five nanoporous Pt-based electrodes, the Pt-Ir shows the highest peak current density at +0.50 V, with 68 times of enhancement compared to the polycrystalline Pt for methanol oxidation, and with 86 times of enhancement in formic acid oxidation; whereas the catalytic activity of the nanoporous Pt-Pb electrode outperforms the other materials in formic acid oxidation at the low potential regions, delivering an enhanced current density by 280-fold compared to the polycrystalline Pt at +0.15 V. The new approach described in this study is suitable for synthesizing a wide range of bi-metallic and tri-metallic nanoporous materials, desirable for electrochemical sensor design and potential application in fuel cells.0.

Synthesis and electrochemical study of Pt-based nanoporous materials

Energy Technology Data Exchange (ETDEWEB)

Wang, Jingpeng [Department of Chemistry, Lakehead University, Thunder Bay, Ontario P7B 5E1 (Canada); Department of Chemistry, University of Guelph, Guelph, Ontario N1G 2W1 (Canada); Holt-Hindle, Peter; MacDonald, Duncan; Chen, Aicheng [Department of Chemistry, Lakehead University, Thunder Bay, Ontario P7B 5E1 (Canada); Thomas, Dan F. [Department of Chemistry, University of Guelph, Guelph, Ontario N1G 2W1 (Canada)

2008-10-01

In the present work, a variety of Pt-based bimetallic nanostructured materials including nanoporous Pt, Pt-Ru, Pt-Ir, Pt-Pd and Pt-Pb networks have been directly grown on titanium substrates via a facile hydrothermal method. The as-fabricated electrodes were characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, X-ray diffraction and electrochemical methods. The active surface areas of these nanoporous Pt-based alloy catalysts are increased by over 68 (Pt-Pd), 69 (Pt-Ru) and 113 (Pt-Ir) fold compared to a polycrystalline Pt electrode. All these synthesized nanoporous electrodes exhibit superb electrocatalytic performance towards electrochemical oxidation of methanol and formic acid. Among the five nanoporous Pt-based electrodes, the Pt-Ir shows the highest peak current density at +0.50 V, with 68 times of enhancement compared to the polycrystalline Pt for methanol oxidation, and with 86 times of enhancement in formic acid oxidation; whereas the catalytic activity of the nanoporous Pt-Pb electrode outperforms the other materials in formic acid oxidation at the low potential regions, delivering an enhanced current density by 280-fold compared to the polycrystalline Pt at +0.15 V. The new approach described in this study is suitable for synthesizing a wide range of bi-metallic and tri-metallic nanoporous materials, desirable for electrochemical sensor design and potential application in fuel cells. (author)

Preparation of MnO2 electrodes coated by Sb-doped SnO2 and their effect on electrochemical performance for supercapacitor

International Nuclear Information System (INIS)

Zhang, Yuqing; Mo, Yan

2014-01-01

Highlights: • Sb-doped SnO 2 coated MnO 2 electrodes (SS-MnO 2 electrodes) are prepared. • The capacitive property and stability of SS-MnO 2 electrode is superior to uncoated MnO 2 electrode and SnO 2 coated MnO 2 electrode. • Sb-doped SnO 2 coating enhances electrochemical performance of MnO 2 effectively. • SS-MnO 2 electrodes are desirable to become a novel electrode material for supercapacitor. - Abstract: To enhance the specific capacity and cycling stability of manganese binoxide (MnO 2 ) for supercapacitor, antimony (Sb) doped tin dioxide (SnO 2 ) is coated on MnO 2 through a sol-gel method to prepare MnO 2 electrodes, enhancing the electrochemical performance of MnO 2 electrode in sodium sulfate electrolytes. The structure and composition of SS-MnO 2 electrode are characterized by using scanning electron microscope (SEM), transmission electron microscope (TEM), Fourier transform infrared spectroscopy (FT-IR) and X-Ray diffraction spectroscopy (XRD). The electrochemical performances are evaluated and researched by galvanostatic charge-discharge test, cyclic voltammogram (CV) and electrochemical impedance spectroscopy (EIS). The results show that SS-MnO 2 electrodes hold porous structure, displaying superior cycling stability at large current work condition in charge-discharge tests and good capacity performance at high scanning rate in CV tests. The results of EIS show that SS-MnO 2 electrodes have small internal resistance. Therefore, the electrochemical performances of MnO 2 electrodes are enhanced effectively by Sb-doped SnO 2 coating

"Slow-scanning" in Ground-based Mid-infrared Observations

Science.gov (United States)

Ohsawa, Ryou; Sako, Shigeyuki; Miyata, Takashi; Kamizuka, Takafumi; Okada, Kazushi; Mori, Kiyoshi; Uchiyama, Masahito S.; Yamaguchi, Junpei; Fujiyoshi, Takuya; Morii, Mikio; Ikeda, Shiro

2018-04-01

Chopping observations with a tip-tilt secondary mirror have conventionally been used in ground-based mid-infrared observations. However, it is not practical for next generation large telescopes to have a large tip-tilt mirror that moves at a frequency larger than a few hertz. We propose an alternative observing method, a "slow-scanning" observation. Images are continuously captured as movie data, while the field of view is slowly moved. The signal from an astronomical object is extracted from the movie data by a low-rank and sparse matrix decomposition. The performance of the "slow-scanning" observation was tested in an experimental observation with Subaru/COMICS. The quality of a resultant image in the "slow-scanning" observation was as good as in a conventional chopping observation with COMICS, at least for a bright point-source object. The observational efficiency in the "slow-scanning" observation was better than that in the chopping observation. The results suggest that the "slow-scanning" observation can be a competitive method for the Subaru telescope and be of potential interest to other ground-based facilities to avoid chopping.

Carbon paste electrode with covalently immobilized thionine for electrochemical sensing of hydrogen peroxide

Science.gov (United States)

Thenmozhi, K.; Sriman Narayanan, S.

2017-11-01

A water-soluble redox mediator, thionin was covalently immobilized to the functionalized graphite powder and a carbon paste electrode was fabricated from this modified graphite powder. The immobilization procedure proved to be effective in anchoring the thionin mediator in the graphite electrode setup without any leakage problem during the electrochemical studies. The covalent immobilization of the thionin mediator was studied with FT-IR and the electrochemical response of the thionin carbon paste electrode was optimized on varying the supporting electrolyte, pH and scan rate. The modified electrode exhibited well-defined electrocatalytic activity towards the reduction of H2O2 at a lower potential of -0.266 V with good sensitivity. The developed amperometric sensor was efficient towards H2O2 in the linear range from 2.46 × 10-5 M to 4.76 × 10-3 M, with a detection limit of 1.47 × 10-5 M respectively. Important advantages of this sensor are its excellent electrochemical performance, simple fabrication, easy renewability, reproducible analytical results, acceptable accuracy and good operational and long-term stability.

Application of Elimination Voltammetry to the Study of Electrochemical Reduction and Determination of the Herbicide Metribuzin

Czech Academy of Sciences Publication Activity Database

Skopalová, J.; Navrátil, Tomáš

2007-01-01

Roč. 52, č. 6 (2007), s. 961-977 ISSN 0009-2223 R&D Projects: GA ČR GA203/07/1195 Institutional research plan: CEZ:AV0Z40400503 Keywords : Elimination voltammetry with linear scan (EVLS) * metribuzin * electrochemical reduction * mercury electrodes Subject RIV: CG - Electrochemistry Impact factor: 0.529, year: 2007

Electrochemical Oxidation of Propene with a LSF15/CGO10 Electrochemical Reactor

DEFF Research Database (Denmark)

Ippolito, Davide; Kammer Hansen, Kent

2014-01-01

A porous electrochemical reactor, made of La0.85Sr0.15FeO3 (LSF) as electrode and Ce0.9Gd0.1O1.95 (CGO) as electrolyte, was studied for the electrochemical oxidation of propene over a wide range of temperatures. Polarization was found to enhance propene oxidation rate. Ce0.9Gd0.1O1.95 was used...... as infiltration material to enhance the effect of polarization on propene oxidation rate, especially at low temperatures. The influence of infiltrated material, as a function of heat treatment, on the reactor electrochemical behavior has been evaluated by using electrochemical impedance spectroscopy...... in suppressing the competing oxygen evolution reaction and promoting the oxidation of propene under polarization, with faradaic efficiencies above 70% at 250◦C. © 2014 The Electrochemical Society....

Electrochemical characteristics of bioresorbable binary MgCa alloys in Ringer's solution: Revealing the impact of local pH distributions during in-vitro dissolution

Energy Technology Data Exchange (ETDEWEB)

Mareci, D., E-mail: danmareci@yahoo.com [Faculty of Chemical Engineering and Environmental Protection, The “Gheorghe Asachi” Technical University of Iasi, 700050, Iasi (Romania); Bolat, G. [Faculty of Chemical Engineering and Environmental Protection, The “Gheorghe Asachi” Technical University of Iasi, 700050, Iasi (Romania); Izquierdo, J. [Department of Chemistry, University of La Laguna, P.O. Box 456, E-38200 La Laguna (Tenerife) (Spain); Crimu, C.; Munteanu, C. [Faculty of Mechanical Engineering, The “Gheorghe Asachi” Technical University of Iasi, 700050, Iasi (Romania); Antoniac, I. [Faculty of Materials Science and Engineering, Politehnica of Bucharest, 060042 Bucharest (Romania); Souto, R.M., E-mail: rsouto@ull.es [Department of Chemistry, University of La Laguna, P.O. Box 456, E-38200 La Laguna (Tenerife) (Spain); Faculty of Materials Science and Engineering, Politehnica of Bucharest, 060042 Bucharest (Romania)

2016-03-01

Biodegradable magnesium–calcium (MgCa) alloy is a very attractive biomaterial. Two MgCa alloys below the solid solubility of Ca were considered, as to solely investigate the effect of Ca content on the behavior of magnesium and the pH changes associated to metal dissolution. X-ray diffraction analysis and optical microscopy showed that both Mg–0.63Ca and Mg–0.89Ca alloys were solely composed of α(Mg) phase. Degradation characteristics and electrochemical characterization of MgCa alloys were investigated during exposure to Ringer's solution at 37 °C by electrochemical impedance spectroscopy and scanning electrochemical microscopy. The impedance behavior showed both capacitive and inductive features that are related to the alloy charge transfer reaction and the relaxation of the absorbed corrosion compounds, and can be described in terms of an equivalent circuit. Scanning electron microscopy (SEM) was employed to view the surface morphology of the MgCa samples after 1 week immersion in Ringer's solution showing extensive precipitation of corrosion products, whereas the substrate shows evidence of a non-uniform corrosion process. Energy dispersive analysis showed that the precipitates contained oxygen, calcium, magnesium and chlorine, and the Mg:Ca ratios were smaller than in the alloys. Scanning electrochemical microscopy (SECM) was used to visualize local pH changes associated to these physicochemical processes with high spatial resolution. The occurrence of pH variations in excess of 3 units between anodic and cathodic half-cell reactions was monitored in situ. - Highlights: • Spontaneous degradation of MgCa alloys in Ringer's solution characterized at 37 °C • Reactivity differences between Mg0.63Ca and Mg0.89Ca are evidenced using multiscale electrochemical characterization. • Electrochemical activation occurs heterogeneously on the alloy surface. • Metal dissolution is accompanied by local pH changes. • Mg0.63Ca degrades faster

Electrochemical determination of morin in Kiwi and Strawberry fruit samples using vanadium pentoxide nano-flakes.

Science.gov (United States)

Sasikumar, Ragu; Govindasamy, Mani; Chen, Shen-Ming; Chieh-Liu, Yu; Ranganathan, Palraj; Rwei, Syang-Peng

2017-10-15

Herein, we report the synthesis of Vanadium Pentoxide Nanoflakes (V 2 O 5 NF) using ionic liquid and employed the V 2 O 5 NF in electrochemical determination of Morin (MR) in fruit samples. The V 2 O 5 NF were characterized by Powder X-ray diffraction (PXRD), scanning electron microscope (SEM), energy-dispersive X-ray analyzer (EDX), differential pulse voltammetry (DPV), and cyclic voltammetry (CV). Remarkably, the as-synthesized V 2 O 5 NF exhibited excellent electrochemical behavior and electrochemical ability towards MR. The CV and DPV studies were recognized that the electrochemical performance of V 2 O 5 NF film modified glassy carbon electrode (V 2 O 5 NF/GCE) towards detection of MR is outstanding in comparison with unmodified GCE. The proposed MR sensor shows a wide linear range, high sensitivity, and low limit of detection are 0.05-10.93μm, 1.130μAμM -1 cm -2 , and 9nM respectively. The fabulous analytical parameters of the developed sensor surpassed the previously reported modified electrodes, rendering the potential application of V 2 O 5 NF in environmental, biomedical, and pharmaceutical samples. Copyright © 2017. Published by Elsevier Inc.

Coating manganese oxide onto graphite electrodes by immersion for electrochemical capacitors

International Nuclear Information System (INIS)

Lin, C.-C.; Chen, H.-W.

2009-01-01

In this study, manganese oxide was coated on a graphite electrode by immersion. Durations for immersion were varied to control the amount of manganese oxide coated onto the electrode surface. Maximum capacitance of 556 mF cm -2 was obtained in 0.5 M LiCl and with better/superior conditions (immersion time = 80 min and potential scan rate = 10 mV s -1 ). In addition, cyclic voltammograms of the prepared electrode at different potential scan rates exhibited the approximately rectangular and symmetric current-potential characteristics of a capacitor. Furthermore, the chronopotentiometry (CP) charge-discharge curves of the electrode prepared at 80 min of immersion time with a constant current of 1 mA were symmetric and similar isosceles triangles, which demonstrate its high electrochemical reversibility and good stability. Finally, under scanning electron microscope (SEM), the surface of the electrode prepared at 80 min of immersion time and after 1500 cycles of potential cycling revealed that numerously three-dimensional network of macropores appeared on large spherical grains

An investigation of the electrochemical action of the epoxy zinc-rich coatings containing surface modified aluminum nanoparticle

Science.gov (United States)

Jalili, M.; Rostami, M.; Ramezanzadeh, B.

2015-02-01

Aluminum nanoparticle was modified with amino trimethylene phosphonic acid (ATMP). The surface characterization of the nanoparticles was done by X-ray photo electron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and thermal gravimetric analysis. The influence of the replacement of 2 wt% of zinc dust in the standard zinc-rich epoxy coating by nanoparticles on the electrochemical action of the coating was studied by electrochemical impedance spectroscopy (EIS) and salt spray tests. The morphology and phase composition of the zinc rich paints were evaluated by X-ray diffraction (XRD) and filed-emission scanning electron microscopy (FE-SEM). Results showed that the ATMP molecules successfully adsorbed on the surface of Al nanoparticles. Results obtained from salt spray and electrochemical measurements revealed that the addition of surface modified nanoparticles to the zinc rich coating enhanced its galvanic action and corrosion protection properties.

Carbon steel corrosion induced by sulphate-reducing bacteria in artificial seawater: electrochemical and morphological characterizations

International Nuclear Information System (INIS)

Paula, Mariana Silva de; Goncalves, Marcia Monteiro Machado; Rola, Monick Alves da Cruz; Maciel, Diana Jose; Senna, Lilian Ferreira de; Lago, Dalva Cristina Baptista do

2016-01-01

In this work, the corrosion behavior of carbon steel AISI 1020 was evaluated in artificial seawater in the presence of mixed sulfate-reducing bacteria (SRB) culture isolated from the rust of a pipeline. The corrosion evaluation was performed by electrochemical techniques (open circuit potential (E_o_c_p), polarization curves and electrochemical impedance spectroscopy (EIS)), while the formation of a biofilm and corrosion products were observed by scanning electron microscopy (SEM) and X-ray energy dispersive spectroscopy (EDS). The presence of SRB in the medium shifted the open circuit potential to more positive values and increased the corrosion rate of the steel. Electrochemical and morphological techniques confirmed the presence of a biofilm on the steel surface. EDS spectra data showed the presence of sulfur in the corrosion products. After removing the biofilm, localized corrosion was observed on the surface, confirming that localized corrosion had occurred. The biogenic sulfide may lead to the formation of galvanic cells and contributes to cathodic depolarization. (author)

Carbon steel corrosion induced by sulphate-reducing bacteria in artificial seawater: electrochemical and morphological characterizations

Energy Technology Data Exchange (ETDEWEB)

Paula, Mariana Silva de; Goncalves, Marcia Monteiro Machado; Rola, Monick Alves da Cruz; Maciel, Diana Jose; Senna, Lilian Ferreira de; Lago, Dalva Cristina Baptista do, E-mail: sdp.mari@gmail.com, E-mail: marciamg@uerj.br, E-mail: monickcruz@yahoo.com.br, E-mail: dijmaciel@gmail.com, E-mail: lsenna@uerj.br, E-mail: dalva@uerj.br [Universidade do Estado do Rio de Janeiro (UERJ), Rio de Janeiro, RJ (Brazil). Instituto de Quimica

2016-10-15

In this work, the corrosion behavior of carbon steel AISI 1020 was evaluated in artificial seawater in the presence of mixed sulfate-reducing bacteria (SRB) culture isolated from the rust of a pipeline. The corrosion evaluation was performed by electrochemical techniques (open circuit potential (E{sub ocp}), polarization curves and electrochemical impedance spectroscopy (EIS)), while the formation of a biofilm and corrosion products were observed by scanning electron microscopy (SEM) and X-ray energy dispersive spectroscopy (EDS). The presence of SRB in the medium shifted the open circuit potential to more positive values and increased the corrosion rate of the steel. Electrochemical and morphological techniques confirmed the presence of a biofilm on the steel surface. EDS spectra data showed the presence of sulfur in the corrosion products. After removing the biofilm, localized corrosion was observed on the surface, confirming that localized corrosion had occurred. The biogenic sulfide may lead to the formation of galvanic cells and contributes to cathodic depolarization. (author)

Preparation and property study of MnO2/CNPs as electrode materials of electrochemical supercapacitors

Directory of Open Access Journals (Sweden)

JIANG Chao

2016-12-01

Full Text Available MnO2 nanorods deposited on carbon nanospheres (MnO2/CNPs as electrode materials of electrochemical supercapacitors have been synthesized via a hydrothermal synthesis.The micro morphologies and phases of the as-prepared MnO2/CNPs were characterized by field emission scanning electro microscopy(FESEM and X-ray diffraction(XRD.The electrochemical properties of nanomaterials were tested by cyclic voltammetry and galvanostatic charge-discharge.At a current density of 0.1 A/g using 1 mol/L Na2SO4 as electrolyte,the as-prepared MnO2/CNPs exhibit excellent specific capacitance of 305.6 F/g,far larger than carbon nanospheres (49.3 F/g.At a current density of 5 A/g,the specific capacitance of MnO2/CNPs is 235 F/g,which is 76.9% of the specific capacitance under 1 A/g current density.These results demonstrated that MnO2/CNPs may show potential application for electrode materials in electrochemical supercapacitors.

Electrochemical and AFM Characterization of G-Quadruplex Electrochemical Biosensors and Applications

Science.gov (United States)

2018-01-01

Guanine-rich DNA sequences are able to form G-quadruplexes, being involved in important biological processes and representing smart self-assembling nanomaterials that are increasingly used in DNA nanotechnology and biosensor technology. G-quadruplex electrochemical biosensors have received particular attention, since the electrochemical response is particularly sensitive to the DNA structural changes from single-stranded, double-stranded, or hairpin into a G-quadruplex configuration. Furthermore, the development of an increased number of G-quadruplex aptamers that combine the G-quadruplex stiffness and self-assembling versatility with the aptamer high specificity of binding to a variety of molecular targets allowed the construction of biosensors with increased selectivity and sensitivity. This review discusses the recent advances on the electrochemical characterization, design, and applications of G-quadruplex electrochemical biosensors in the evaluation of metal ions, G-quadruplex ligands, and other small organic molecules, proteins, and cells. The electrochemical and atomic force microscopy characterization of G-quadruplexes is presented. The incubation time and cations concentration dependence in controlling the G-quadruplex folding, stability, and nanostructures formation at carbon electrodes are discussed. Different G-quadruplex electrochemical biosensors design strategies, based on the DNA folding into a G-quadruplex, the use of G-quadruplex aptamers, or the use of hemin/G-quadruplex DNAzymes, are revisited. PMID:29666699

Electrochemical migration, whisker formation, and corrosion behavior of printed circuit board under wet H2S environment

International Nuclear Information System (INIS)

Zou, Shiwen; Li, Xiaogang; Dong, Chaofang; Ding, Kangkang; Xiao, Kui

2013-01-01

Highlights: •The electrochemical migration, whisker formation, and corrosion behavior of PCB under wet H 2 S environment were observed and studied systematically. •The process of electrochemical migration of solder joints is explained. •The corrosion mechanism of PCB interconnectors induced by micro pores under wet H 2 S environment is discussed, and the corrosion reaction model is proposed. -- Abstract: Electrochemical migration, whisker formation, and corrosion behavior of printed circuit board (PCB) under wet H 2 S environment were analyzed by environment scanning electron microscope (ESEM), Energy dispersive X-ray spectroscopy (EDS) with mapping and element phase cluster (EPC) techniques, Raman Spectrum analysis and electrochemical impedance spectroscopy (EIS) technology. The results showed that nonuniform corrosion behavior occurred on PCB surfaces under 1 ppm wet H 2 S at 40 °C; whiskers formed on the inner sidewall of via-holes with a growth rate of 1.2 Å/s; numerous corrosion products migrated through the pore of plated gold layer, which broke off the protective layer. The corrosion rate was accelerated according to the big-cathode-small-anode model

Hydroxyapatite/gelatin functionalized graphene oxide composite coatings deposited on TiO2 nanotube by electrochemical deposition for biomedical applications

International Nuclear Information System (INIS)

Yan, Yajing; Zhang, Xuejiao; Mao, Huanhuan; Huang, Yong; Ding, Qiongqiong; Pang, Xiaofeng

2015-01-01

Highlights: • Graphene oxide cross-linked gelatin was firstly employed as reinforcement fillers in hydroxyapatite coatings by electrochemical deposition process on TiO 2 nanotube arrays. • Gelatin functionalized graphene oxide induced the formation of hydroxyapatite coatings. • The success of gelatin and graphene oxide incorporation was evidenced with FTIR and XPS. • The synthesized composite coatings showed good biocompatibility and no adverse effect in cell culture tests. - Abstract: Graphene oxide cross-linked gelatin was employed as reinforcement fillers in hydroxyapatite coatings by electrochemical deposition process on TiO 2 nanotube arrays (TNs). The TNs were grown on titanium by electrochemical anodization in hydrofluoric electrolyte using constant voltage. Fourier transform infrared spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, Field emission scanning electron microscopy equipped with energy dispersive X-ray analysis and biological studies were used to characterize the coatings. The corrosion resistance of the coatings was also investigated by electrochemical method in simulated body fluid solution

V2O5 xerogel-poly(ethylene oxide) hybrid material: Synthesis, characterization, and electrochemical properties

International Nuclear Information System (INIS)

Guerra, Elidia M.; Ciuffi, Katia J.; Oliveira, Herenilton P.

2006-01-01

In this work, we report the synthesis, characterization, and electrochemical properties of vanadium pentoxide xerogel-poly(ethylene oxide) (PEO) hybrid materials obtained by varying the average molecular weight of the organic component as well as the components' ratios. The materials were characterized by X-ray diffraction, ultraviolet/visible and infrared spectroscopies, thermogravimetric analysis, scanning electron microscopy, electron paramagnetic resonance, and cyclic voltammetry. Despite the presence of broad and low intensity peaks, the X-ray diffractograms indicate that the lamellar structure of the vanadium pentoxide xerogel is preserved, with increase in the interplanar spacing, giving evidence of a low-crystalline structure. We found that the electrochemical behaviour of the hybrid materials is quite similar to that found for the V 2 O 5 xerogel alone, and we verified that PEO leads to stabilization and reproducibility of the Li + electrochemical insertion/de-insertion into the V 2 O 5 xerogel structure, which makes these materials potential components of lithium ion batteries. - Graphical abstract: The synthesis, structural and electrochemical properties of vanadium pentoxide xerogel-poly(ethylene oxide) hybrid materials have been described. Despite the presence of broad and low intensity peaks, the X-ray diffractograms indicate that the lamellar structure of the vanadium pentoxide xerogel is preserved. The cyclic voltammetry technique demonstrated that PEO intercalation provides an improvement in the electrochemical properties, mainly with respect to the lithium electroinsertion process into the oxide matrix

Synthesis of binary bismuth-cadmium oxide nanorods with sensitive electrochemical sensing performance

International Nuclear Information System (INIS)

Wen, Yong; Pei, Lizhai; Wei, Tian

2017-01-01

Binary bismuth-cadmium oxide nanorods have been synthesized by a simple hydrothermal process without templates and additives. X-ray diffraction and high-resolution transmission electron microscopy reveal that the nanorods possess single crystalline tetragonal Bi 2 CdO 4 phase. Scanning electron microscopy and transmission electron microscopy images show that the length and diameter of the nanorods are 20-300 nm and 5-10 μm, respectively. The formation of the binary bismuth-cadmium oxide nanorods is closely related to the hydrothermal parameters. The electrochemical sensing performance of the binary bismuth-cadmium oxide nanorods has been investigated using the nanorods as glassy carbon electrode modifiers. The detection limit is 0.19 μM with a linear range of 0.0005-2 mM. The nanorod-modified glassy carbon electrode exhibits good electrocatalytic activity toward L-cysteine and great application potential for electrochemical sensors.

Electrochemical characterization of aminated acrylic conducting polymer

International Nuclear Information System (INIS)

Rashid, Norma Mohammad; Heng, Lee Yook; Ling, Tan Ling

2015-01-01

New attempt has been made to synthesize aminated acrylic conducting polymer (AACP) using precursor of phenylvinylsulfoxide (PVS). The process was conducted via the integration of microemulsion and photopolymerization techniques. It has been utilized for covalent immobilization of amino groups by the adding of N-achryiloxisuccinimide (NAS). Thermal eliminating of benzene sulfenic acids from PVS has been done at 250 °C to form electroactive polyacetylene (PA) segment. Characterization of AACP has been conducted using fourier transform infrared (FTIR), scanning electron microscopy (SEM) and linear sweep cyclic voltammetry (CV). A range of 0.3-1.25μm particle size obtained from SEM characterization. A quasi-reversible system performed as shown in electrochemical study

Electrochemical characterization of aminated acrylic conducting polymer

Energy Technology Data Exchange (ETDEWEB)

Rashid, Norma Mohammad [School of Chemical Sciences and Food Technology, Faculty of Science and Technology, Lestari Universiti Kebangsaan Malaysia (UKM), 43600 Bangi, Selangor Darul Ehsan (Malaysia); Heng, Lee Yook [School of Chemical Sciences and Food Technology, Faculty of Science and Technology, Lestari Universiti Kebangsaan Malaysia (UKM), 43600 Bangi, Selangor Darul Ehsan (Malaysia); Southeast Asia Disaster Prevention Research Initiative, Lestari Universiti Kebangsaan Malaysia (UKM), 43600 Bangi, Selangor Darul Ehsan (Malaysia); Ling, Tan Ling [Southeast Asia Disaster Prevention Research Initiative, Lestari Universiti Kebangsaan Malaysia (UKM), 43600 Bangi, Selangor Darul Ehsan (Malaysia)

2015-09-25

New attempt has been made to synthesize aminated acrylic conducting polymer (AACP) using precursor of phenylvinylsulfoxide (PVS). The process was conducted via the integration of microemulsion and photopolymerization techniques. It has been utilized for covalent immobilization of amino groups by the adding of N-achryiloxisuccinimide (NAS). Thermal eliminating of benzene sulfenic acids from PVS has been done at 250 °C to form electroactive polyacetylene (PA) segment. Characterization of AACP has been conducted using fourier transform infrared (FTIR), scanning electron microscopy (SEM) and linear sweep cyclic voltammetry (CV). A range of 0.3-1.25μm particle size obtained from SEM characterization. A quasi-reversible system performed as shown in electrochemical study.

Production and characterization of TI/PbO2 electrodes by a thermal-electrochemical method

Directory of Open Access Journals (Sweden)

Laurindo Edison A.

2000-01-01

Full Text Available Looking for electrodes with a high overpotential for the oxygen evolution reaction (OER, useful for the oxidation of organic pollutants, Ti/PbO2 electrodes were prepared by a thermal-electrochemical method and their performance was compared with that of electrodeposited electrodes. The open-circuit potential for these electrodes in 0.5 mol L-1 H2SO4 presented quite stable similar values. X-ray diffraction analyses showed the thermal-electrochemical oxide to be a mixture of ort-PbO, tetr-PbO and ort-PbO2. On the other hand, the electrodes obtained by electrodeposition were in the tetr-PbO2 form. Analyses by scanning electron microscopy showed that the basic morphology of the thermal-electrochemical PbO2 is determined in the thermal step, being quite distinct from that of the electrodeposited electrodes. Polarization curves in 0.5 mol L-1 H2SO4 showed that in the case of the thermal-electrochemical PbO2 electrodes the OER was shifted to more positive potentials. However, the values of the Tafel slopes, quite high, indicate that passivating films were possibly formed on the Ti substrates, which could eventually explain the somewhat low current values for OER.

Facile synthesis and photo electrochemical performance of SnSe thin films

Science.gov (United States)

Pusawale, S. N.; Jadhav, P. S.; Lokhande, C. D.

2018-05-01

Orthorhombic structured SnSe thin films are synthesized via SILAR (successive ionic layer adsorption and reaction) method on glass substrates. The structural properties of thin films are characterized by x-ray diffraction, scanning electron microscopy studies from which nanoparticles with an elongated shape and hydrophilic behavior are observed. UV -VIS absorption spectroscopy study showed the maximum absorption in the visible region with a direct band gap of 1.55 eV. The photo electrochemical study showed p-type electrical conductivity.

Electrochemical capacitance characteristics of patterned ruthenium dioxide-carbon nanotube nanocomposites grown onto graphene

Energy Technology Data Exchange (ETDEWEB)

Shih, Yi-Ting [Graduate Institute of Electro-Optical Engineering, National Taiwan University of Science and Technology, No. 43, Section 4, Keelung Road, Taipei 10607, Taiwan (China); Lee, Kuei-Yi, E-mail: kylee@mail.ntust.edu.tw [Graduate Institute of Electro-Optical Engineering, National Taiwan University of Science and Technology, No. 43, Section 4, Keelung Road, Taipei 10607, Taiwan (China); Department of Electronic Engineering, National Taiwan University of Science and Technology, No. 43, Section 4, Keelung Road, Taipei 10607, Taiwan (China); Huang, Ying-Sheng [Graduate Institute of Electro-Optical Engineering, National Taiwan University of Science and Technology, No. 43, Section 4, Keelung Road, Taipei 10607, Taiwan (China); Department of Electronic Engineering, National Taiwan University of Science and Technology, No. 43, Section 4, Keelung Road, Taipei 10607, Taiwan (China)

2014-03-01

Highlights: • Graphene was grown on Cu foil by mobile thermal chemical vapor deposition system. • CNT was synthesized on graphene for RuO{sub 2} nanostructure growth by thermal chemical vapor deposition system. • The CNT growth location was fixed through the use of photolithography technique, thereby increasing the specific area. • RuO{sub 2} nanostructures were coated onto CNT bundle arrays through metal organic chemical vapor deposition, in order to utilize its pseudo capacitive property. - Abstract: In this study, graphene was used as a conductive substrate for vertically aligned carbon nanotube (CNT) bundle arrays growth, to be used as an electrode for electrochemical double layer capacitor (EDLC), as graphene and CNT exhibit good conductivity and excellent chemical stability. Both of them are composed of carbon, therefore making a superior adhesion between them. The configuration of bundle arrays provided a relatively higher specific surface area in contact with electrolyte, thereby resulting in demonstratively higher capacitance. Moreover, as the RuO{sub 2} nanostructures have good pseudocapacitance characteristics, they were coated onto vertically aligned CNT bundle arrays in order to effectively enhance the EDLC performances. The characteristics of CNT/graphene, CNT bundle/graphene, and RuO{sub 2}/CNT bundle/graphene electrodes were examined with the use of scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman spectroscopy. Furthermore, their electrochemical properties were investigated by an electrochemical analyzer. The specific capacitances of CNT/graphene, CNT bundle/graphene, and RuO{sub 2}/CNT bundle/graphene were 4.64, 6.65, and 128.40 F/g at the scan rate of 0.01 V/s, respectively.

Design and Electrochemical Study of Platinum-Based Nanomaterials for Sensitive Detection of Nitric Oxide in Biomedical Applications

Directory of Open Access Journals (Sweden)

Maduraiveeran Govindhan

2016-11-01

Full Text Available The extensive physiological and regulatory roles of nitric oxide (NO have spurred the development of NO sensors, which are of critical importance in neuroscience and various medical applications. The development of electrochemical NO sensors is of significant importance, and has garnered a tremendous amount of attention due to their high sensitivity and selectivity, rapid response, low cost, miniaturization, and the possibility of real-time monitoring. Nanostructured platinum (Pt-based materials have attracted considerable interest regarding their use in the design of electrochemical sensors for the detection of NO, due to their unique properties and the potential for new and innovative applications. This review focuses primarily on advances and insights into the utilization of nanostructured Pt-based electrode materials, such as nanoporous Pt, Pt and PtAu nanoparticles, PtAu nanoparticle/reduced graphene oxide (rGO, and PtW nanoparticle/rGO-ionic liquid (IL nanocomposites, for the detection of NO. The design, fabrication, characterization, and integration of electrochemical NO sensing performance, selectivity, and durability are addressed. The attractive electrochemical properties of Pt-based nanomaterials have great potential for increasing the competitiveness of these new sensors and open up new opportunities in the creation of novel NO-sensing technologies for biological and medical applications.

Electrochemical thermodynamic measurement system

Science.gov (United States)

Reynier, Yvan [Meylan, FR; Yazami, Rachid [Los Angeles, CA; Fultz, Brent T [Pasadena, CA

2009-09-29

The present invention provides systems and methods for accurately characterizing thermodynamic and materials properties of electrodes and electrochemical energy storage and conversion systems. Systems and methods of the present invention are configured for simultaneously collecting a suite of measurements characterizing a plurality of interconnected electrochemical and thermodynamic parameters relating to the electrode reaction state of advancement, voltage and temperature. Enhanced sensitivity provided by the present methods and systems combined with measurement conditions that reflect thermodynamically stabilized electrode conditions allow very accurate measurement of thermodynamic parameters, including state functions such as the Gibbs free energy, enthalpy and entropy of electrode/electrochemical cell reactions, that enable prediction of important performance attributes of electrode materials and electrochemical systems, such as the energy, power density, current rate and the cycle life of an electrochemical cell.

Facile electrochemical synthesis of tellurium nanorods and their photoconductive properties

Energy Technology Data Exchange (ETDEWEB)

Li, H.H. [Center for Photon Manufacturing Science and Technology, School of Materials Science and Engineering, Jiangsu University, Zhenjiang - 212013 (China); Zhang, P. [Dongguan University of Technology, Dongguan-523808 (China); School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou - 510275 (China); Liang, C.L. [Instrumental Analysis and Research Center, SunYat-sen University, Guangzhou - 510275 (China); Yang, J. [School of Materials Science and Engineering, Jiangsu University, Zhenjiang - 212013 (China); Zhou, M. [Center for Photon Manufacturing Science and Technology, School of Materials Science and Engineering, Jiangsu University, Zhenjiang - 212013 (China); The State Key Laboratory of Tribology, Tsinghua University, Beijing - 10084 (China); Lu, X.H. [School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou - 510275 (China); Hope, G.A. [School of Biomolecular and Physical Sciences, Griffith University, Nathan - Qld 4111 (Australia)

2012-10-15

Tellurium nanorods have been successfully fabricated by template and surfactant-free electrochemical technique from an aqueous solution at room temperature. The as-prepared tellurium nanorods were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectrometry, UV-vis spectroscopy and photoluminescence spectroscopy. Films based on tellurium nanorods were constructed to study the photoresponse and I-V curves. These photoresponse measurements demonstrate that tellurium nanorods exhibited enhanced conductivity under illumination compared to in the dark measurement. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Electrochemical doping of mesoporous silicon with Er: the effect of the current intensity

Energy Technology Data Exchange (ETDEWEB)

Mula, Guido, E-mail: guido.mula@unica.it [Dipartimento di Fisica, Università degli Studi di Cagliari, Cittadella Universitaria di Monserrato, S.P. 8 km 0.700, 09042 Cagliari (Italy); Pinna, Elisa [Dipartimento di Fisica, Università degli Studi di Cagliari, Cittadella Universitaria di Monserrato, S.P. 8 km 0.700, 09042 Cagliari (Italy); Falqui, Andrea [Nanochemistry, Istituto Italiano di Tecnologia, Via Morego 30, 16163 Genova (Italy); Dipartimento di Scienze Chimiche e Geologiche, Università degli Studi di Cagliari, Cittadella Universitaria di Monserrato, S.P. 8 km 0.700, 09042 Cagliari (Italy); Ruffilli, Roberta [Dipartimento di Scienze Chimiche e Geologiche, Università degli Studi di Cagliari, Cittadella Universitaria di Monserrato, S.P. 8 km 0.700, 09042 Cagliari (Italy); Palmas, Simonetta; Mascia, Michele [Dipartimento di Ingegneria Meccanica Chimica e dei Materiali, Università degli Studi di Cagliari, Piazza d’Armi, 09126 Cagliari (Italy)

2014-08-30

Graphical abstract: - Highlights: • A multidisciplinary approach on porous Si electrochemical Er doping is proposed. • The phenomena taking place at the large developed surface of porous silicon are studied. • Electrochemical, optical and structural characterizations are used. • The early stages of doping are studied by electrochemical impedance spectroscopy. • The dependence of the final amount of Er deposited on the current intensity and not only on the transferred charge is shown. - Abstract: There is an ongoing intense research for cost-effective Er-doped Si-based light-emitting devices at the 1.5 μm wavelength. The efficient electrochemical Er-doping of porous silicon for this purpose requires a good understanding of the phenomena involved, since those taking place at the pores inner surface control the doping process. However, almost no attention has been given, to date, to the relevant effects of the current intensity onto the doping results. In this work, the effect of the current intensity on the doping process is explored by means of electrochemical impedance spectroscopy, optical reflectivity and energy dispersive spectrometry via scanning electron microscopy. The combined analysis of all results strongly suggests that the formation of a gel-like Er ethanolate, unaffected by changes in the sample thickness, occurs from the very first stages of the doping process. Moreover, while for constant current doping processes we show that, under any given doping condition, the doping level is proportional to the transferred charge, we demonstrate that performing the doping process using different current intensities may lead to dramatically different results.

Electrochemical studies of Copper, Tantalum and Tantalum Nitride surfaces in aqueous solutions for applications in chemical-mechanical and electrochemical-mechanical planarization

Science.gov (United States)

Sulyma, Christopher Michael

lines and Ta barriers in the fabrication of semiconductor devices. It is shown that in non-alkaline solutions of H2O2, the SA-promoted surface complexes of Cu and Ta can potentially support chemically enhanced material removal in low-pressure CMP of surface topographies overlying fragile low-k dielectrics. ADS can suppress Cu dissolution without significantly affecting the surface chemistry of Ta. Chapter 6 discusses anodic corrosion of Ta, which is examined as a possible route to voltage induced removal of Ta for potential applications in electrochemical mechanical planarization (ECMP) of diffusion barriers. This strategy involves electro-oxidation of Ta in the presence of NO3- anions to form mechanically weak surface oxide films, followed by removal of the oxide layers by moderate mechanical abrasion. This NO3 - system is compared with a reference solution of Br -. In both electrolytes, the voltammetric currents of anodic oxidation exhibit oscillatory behaviors in the initial cycles of slow (5 mV s-1) voltage scans. The frequencies of these current oscillations are show signature attributes of localized pitting or general surface corrosion caused by Br- or NO3 -, respectively. Scanning electron microscopy, cyclic voltammetry, polarization resistance measurements, and time resolved Fourier transform impedance spectroscopy provide additional details about these corrosion mechanism. Apart from their relevance in the context of ECMP, the results also address certain fundamental aspects of pitting and general corrosions. The general protocols necessary to combine and analyze the results of D.C. and A.C. electrochemical measurements involving such valve metal corrosion systems are discussed in detail. In chapter 7 potassium salts of certain oxyanions (nitrate, sulfate and phosphate in particular) are shown to serve as effective surface-modifying agents in chemically enhanced, low-pressure chemical mechanical planarization (CMP) of Ta and TaN barrier layers for interconnect

Chitosan-iron oxide nanocomposite based electrochemical aptasensor for determination of malathion

Energy Technology Data Exchange (ETDEWEB)

Prabhakar, Nirmal, E-mail: nirmalprabhakar@gmail.com; Thakur, Himkusha; Bharti, Anu; Kaur, Navpreet

2016-10-05

An electrochemical aptasensor based on chitosan-iron oxide nanocomposite (CHIT-IO) film deposited on fluorine tin Oxide (FTO) was developed for the detection of malathion. Iron oxide nanoparticles were prepared by co-precipitation method and characterized by Transmission electron microscopy and UV–Visible spectroscopy. The biotinylated DNA aptamer sequence specific to the malathion was immobilized onto the iron oxide doped-chitosan/FTO electrode by using streptavidin as linking molecule. Various characterization studies like Field Emission-Scanning Electron Microscopy (FE-SEM), Fourier Transform Infrared Spectroscopy (FT-IR), and Electrochemical studies were performed to attest the successful fabrication of bioelectrodes. Experimental parameters like aptamer concentration, response time, stability of electrode and reusability studies were optimized. Aptamer immobilized chitosan-iron oxide nanocomposite (APT/SA/CHIT-IO/FTO) bioelectrodes exhibited LOD of about 0.001 ng/mL within 15 min and spike-in studies revealed about 80–92% recovery of malathion from the lettuce leaves and soil sample. - Highlights: • An electrochemical aptasensor for the detection of Malathion has been developed. • Chitosan-iron oxide NP deposited FTO sheets provides platform for aptamer immobilization. • Aptasensor has efficiency to detect malathion upto 0.001 ng/mL within 15 min.

Enhanced optical performance of electrochemically etched porous silicon carbide

International Nuclear Information System (INIS)

Naderi, N; Hashim, M R; Saron, K M A; Rouhi, J

2013-01-01

Porous silicon carbide (PSC) was successfully synthesized via electrochemical etching of an n-type hexagonal silicon carbide (6H-SiC) substrate using various current densities. The cyclic voltammograms of SiC dissolution show that illumination is required for the accumulation of carriers at the surface, followed by surface oxidation and dissolution of the solid. The morphological and optical characterizations of PSC were reported. Scanning electron microscopy results demonstrated that the current density can be considered an important etching parameter that controls the porosity and uniformity of PSC; hence, it can be used to optimize the optical properties of the porous samples. (paper)

Palladium nanoparticles decorated on activated fullerene modified screen printed carbon electrode for enhanced electrochemical sensing of dopamine.

Science.gov (United States)

Palanisamy, Selvakumar; Thirumalraj, Balamurugan; Chen, Shen-Ming; Ali, M Ajmal; Al-Hemaid, Fahad M A

2015-06-15

In the present work, an enhanced electrochemical sensor for dopamine (DA) was developed based on palladium nanoparticles decorated activated fullerene-C60 (AC60/PdNPs) composite modified screen printed carbon electrode (SPCE). The scanning electron microscopy and elemental analysis confirmed the formation of PdNPs on AC60. The fabricated AC60/PdNPs composite modified electrode exhibited an enhanced electrochemical response to DA with a lower oxidation potential than that of SPCE modified with PdNPs and C60, indicating the excellent electrooxidation behavior of the AC60/PdNPs composite modified electrode. The electrochemical studies confirmed that the electrooxidation of DA at the composite electrode is a diffusion controlled electrochemical process. The differential pulse voltammetry was employed for the determination of DA; under optimum conditions, the electrochemical oxidation signal of DA increased linearly at the AC60/PdNPs composite from 0.35 to 133.35 μM. The limit of detection was found as 0.056 μM with a sensitivity of 4.23 μA μM(-1) cm(-2). The good recovery of DA in the DA injection samples further revealed the good practicality of AC60/PdNPs modified electrode. Copyright © 2015 Elsevier Inc. All rights reserved.

Highly sensitive electrochemical determination of Sunset Yellow based on gold nanoparticles/graphene electrode

International Nuclear Information System (INIS)

Wang, Jin; Yang, Beibei; Wang, Huiwen; Yang, Ping; Du, Yukou

2015-01-01

An electrochemical sensor was prepared using Au nanoparticles and reduced graphene successfully decorated on the glassy carbon electrode (Au/RGO/GCE) through an electrochemical method which was applied to detect Sunset Yellow (SY). The as-prepared electrode was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM) and electrochemical measurements. The results of cyclic voltammetry (CV) proved that Au/RGO/GCE had the highest catalytic activity for the oxidation of SY as compared with GCE, Au/GCE, and RGO/GCE. Differential pulse voltammetry (DPV) showed that the linear calibration curves for SY on Au/RGO/GCE in the range of 0.002 μM–109.14 μM, and the detection limit was estimated to be 2 nM (S/N = 3). These results suggested that the obtained Au/RGO/GCE was applied to detect SY with high sensitivity, low detection limit and good stability, which provided a promising future for the development of portable sensor in food additives. - Highlights: • An Au/RGO composite was fabricated by electrochemical deposition method. • The oxidation current of SY on the composition is up to 10 μA. • The detection range of SY is 0.002–109.14 μM with a detection limit of 2 nM.

Molecular assembly and electro polymerization of 3,4-ethylenedioxy thiophene on Au(100) single crystal electrode using in-situ electrochemical scanning tunneling microscopy

International Nuclear Information System (INIS)

Garcia, Jonyl L.; Tongol, Bernard John V.; ShuehLin Yau

2012-01-01

Electrochemical scanning tunneling microscopy (Ec-STM) is a powerful technique that can provide molecular-level information regarding electrode surface processes in-situ in electrolyte solvent under ambient conditions. In this study, the adsorption and electro polymerization of an industrially important conducting polymer precursor, 3,4-ethylenedioxy thiophene (EDOT), on Au (100) single crystal was probed using Ec-STM. The Au (100) single crystal electrode substrate used for this study was fabricated using the well-known Clavilier's flame melting procedure. Cyclic voltammetry (CV) was used along with Ec-STM to characterize the bare, EDOT-modified, and poly(EDOT)-modified Au (100) single crystal electrode. Time-dependent Ec-STM imaging at 0.550 V showed the formation of an EDOT self-assembled monolayer through 2-D surface dillusion. The resulting EDOT molecular assembly on Au (100) single crystal electrode was found to fit in a 4√2χ3√2 unit cell. Difference in apparent corrugation between molecular rows was attributed to different angular orientation with respect to the substrate. The electro polymerization of EDOT on Au (100) single crystal electrode was done by potentiostatic and potentiodynamic methods. Both methods suggested a solution-process mechanism for EDOT electro polymerization. (author)

Electrochemical impedance spectroscopic characterization of titanium during alkali treatment and apatite growth in simulated body fluid

International Nuclear Information System (INIS)

Raman, V.; Tamilselvi, S.; Rajendran, N.

2007-01-01

Alkali treatment of titanium with subsequent heat treatment has been adapted as an important pre-treatment procedure for hydroxyapatite formation in orthopaedic applications. The electrochemical study during the alkali treatment process has not been explored yet. In the present work, electrochemical impedance spectroscopic (EIS) studies have been employed to analyse the electrochemical behaviour of titanium during the alkali treatment. The open circuit potential and potentiodynamic polarisation measurements were carried out in simulated body fluid (SBF) solution. Scanning electron microscopy and energy dispersive X-ray analysis were used to characterize the surface morphology and to correlate the results obtained from the electrochemical studies. An optimum growth of the passive film was found to occur at the end of 17th hour of treatment by alkali treatment. The alkali treated titanium immersed in SBF solution for various durations exhibited the formation of a duplex layer structure due to an inner barrier layer and an outer gel layer during the initial periods of immersion. However, with increase in immersion time to 10 days, a stable apatite layer was formed over the barrier layer and this was confirmed from the equivalent circuit fitted for the impedance data

Electrochemical impedance spectroscopic characterization of titanium during alkali treatment and apatite growth in simulated body fluid

Energy Technology Data Exchange (ETDEWEB)

Raman, V.; Tamilselvi, S. [Department of Chemistry, MIT Campus, Anna University, Chennai 600 044 (India); Rajendran, N. [Department of Chemistry, MIT Campus, Anna University, Chennai 600 044 (India)], E-mail: nrajendran@annauniv.edu

2007-09-30

Alkali treatment of titanium with subsequent heat treatment has been adapted as an important pre-treatment procedure for hydroxyapatite formation in orthopaedic applications. The electrochemical study during the alkali treatment process has not been explored yet. In the present work, electrochemical impedance spectroscopic (EIS) studies have been employed to analyse the electrochemical behaviour of titanium during the alkali treatment. The open circuit potential and potentiodynamic polarisation measurements were carried out in simulated body fluid (SBF) solution. Scanning electron microscopy and energy dispersive X-ray analysis were used to characterize the surface morphology and to correlate the results obtained from the electrochemical studies. An optimum growth of the passive film was found to occur at the end of 17th hour of treatment by alkali treatment. The alkali treated titanium immersed in SBF solution for various durations exhibited the formation of a duplex layer structure due to an inner barrier layer and an outer gel layer during the initial periods of immersion. However, with increase in immersion time to 10 days, a stable apatite layer was formed over the barrier layer and this was confirmed from the equivalent circuit fitted for the impedance data.

Sensitive determination of citrinin based on molecular imprinted electrochemical sensor

Energy Technology Data Exchange (ETDEWEB)

Atar, Necip [Department of Chemical Engineering, Faculty of Engineering, Pamukkale University, Denizli (Turkey); Yola, Mehmet Lütfi, E-mail: mehmetyola@gmail.com [Department of Metallurgical and Materials Engineering, Faculty of Engineering, Sinop University, Sinop (Turkey); Eren, Tanju [Department of Chemical Engineering, Faculty of Engineering, Pamukkale University, Denizli (Turkey)

2016-01-30

Graphical abstract: - Highlights: • Citrinin-imprinted electrochemical sensor is developed for the sensitive detection of citrinin. • The nanomaterial and citrinin-imprinted surfaces were characterized by several methods. • Citrinin-imprinted electrochemical sensor is sensitive and selective in analysis of food. • Citrinin-imprinted electrochemical sensor is preferred to the other methods. - Abstract: In this report, a novel molecular imprinted voltammetric sensor based on glassy carbon electrode (GCE) modified with platinum nanoparticles (PtNPs) involved in a polyoxometalate (H{sub 3}PW{sub 12}O{sub 40}, POM) functionalized reduced graphene oxide (rGO) was prepared for the determination of citrinin (CIT). The developed surfaces were characterized by using scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) method. CIT imprinted GCE was prepared via electropolymerization process of 80.0 mM pyrrole as monomer in the presence of phosphate buffer solution (pH 6.0) containing 20.0 mM CIT. The linearity range and the detection limit of the developed method were calculated as 1.0 × 10{sup −12}–1.0 × 10{sup −10} M and 2.0 × 10{sup −13} M, respectively. In addition, the voltammetric sensor was applied to rye samples. The stability and selectivity of the voltammetric sensor were also reported.

Sensitive determination of citrinin based on molecular imprinted electrochemical sensor

International Nuclear Information System (INIS)

Atar, Necip; Yola, Mehmet Lütfi; Eren, Tanju

2016-01-01

Graphical abstract: - Highlights: • Citrinin-imprinted electrochemical sensor is developed for the sensitive detection of citrinin. • The nanomaterial and citrinin-imprinted surfaces were characterized by several methods. • Citrinin-imprinted electrochemical sensor is sensitive and selective in analysis of food. • Citrinin-imprinted electrochemical sensor is preferred to the other methods. - Abstract: In this report, a novel molecular imprinted voltammetric sensor based on glassy carbon electrode (GCE) modified with platinum nanoparticles (PtNPs) involved in a polyoxometalate (H_3PW_1_2O_4_0, POM) functionalized reduced graphene oxide (rGO) was prepared for the determination of citrinin (CIT). The developed surfaces were characterized by using scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) method. CIT imprinted GCE was prepared via electropolymerization process of 80.0 mM pyrrole as monomer in the presence of phosphate buffer solution (pH 6.0) containing 20.0 mM CIT. The linearity range and the detection limit of the developed method were calculated as 1.0 × 10"−"1"2–1.0 × 10"−"1"0 M and 2.0 × 10"−"1"3 M, respectively. In addition, the voltammetric sensor was applied to rye samples. The stability and selectivity of the voltammetric sensor were also reported.

Electrochemical deposition of gold-platinum alloy nanoparticles on an indium tin oxide electrode and their electrocatalytic applications

Energy Technology Data Exchange (ETDEWEB)

Song Yan; Ma Yuting; Wang Yuan [Department of Chemistry, Soochow University, Suzhou, Jiangsu 215123 (China); Di Junwei, E-mail: djw@suda.edu.c [Department of Chemistry, Soochow University, Suzhou, Jiangsu 215123 (China); Tu Yifeng [Department of Chemistry, Soochow University, Suzhou, Jiangsu 215123 (China)

2010-07-01

Gold-platinum (Au-Pt) hybrid nanoparticles (Au-PtNPs) were successfully deposited on an indium tin oxide (ITO) surface using a direct electrochemical method. The resulting nanoparticles were characterized by scanning electron microscopy (SEM), UV-vis spectroscopy, X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDX), and electrochemical methods. It was found that the size of the Au-PtNPs depends on the number of electrodeposition cycles. Au-PtNPs obtained by 20 electrodeposition cycles had a cauliflower-shaped structure with an average diameter of about 60 nm. These Au-PtNPs exhibited alloy properties. Electrochemical measurements showed that the charge transfer resistivity was significantly decreased for the Au-PtNPs/ITO electrode. Additionally, the Au-PtNPs displayed an electrocatalytic activity for nitrite oxidation and oxygen reduction. The Au-PtNPs/ITO electrodes reported herein could possibly be used as electrocatalysts and sensors.

Enhanced electrochemical performance of LiVPO4F/f-graphene composite electrode prepared via ionothermal process

KAUST Repository

Rangaswamy, Puttaswamy

2016-10-13

Abstract: In this article, we report the synthesis of 1,2-dimethyl-3-(3-hydroxypropyl) imidazolium dicyanamide ionic liquid and its used as a reaction medium for low-temperature synthesis of triclinic LiVPOF electrode material. Structural and morphological features of LiVPOF were characterized using X-ray diffraction and scanning electron microscopy techniques. The electrochemical studies have been investigated using cyclic voltammetry, galvanostatic charge/discharge studies, and electrochemical impedance spectroscopic techniques. The ionothermally obtained LiVPOF is modified to LiVPOF/f-graphene composite electrode to obtain high specific capacity, better rate performance, and longer cycle life. Even after 250 cycles, the LiVPOF/f-graphene composite electrode exhibited a specific capacity more than 84 % with good reversible de-intercalation/intercalation of Li-ions. This article also provides the comparative electrochemical performances of LiVPOF/f-graphene composite, LiVPOF/carbon, and LiVPOF/graphene composite electrodes in a nonaqueous rechargeable Li-ion battery system. Graphical Abstract: [Figure not available: see fulltext.

Enhanced electrochemical performance of LiVPO4F/f-graphene composite electrode prepared via ionothermal process

KAUST Repository

Rangaswamy, Puttaswamy; Shetty, Vijeth Rajshekar; Suresh, Gurukar Shivappa; Mahadevan, Kittappa Malavalli; Nagaraju, Doddahalli H.

2016-01-01

Abstract: In this article, we report the synthesis of 1,2-dimethyl-3-(3-hydroxypropyl) imidazolium dicyanamide ionic liquid and its used as a reaction medium for low-temperature synthesis of triclinic LiVPOF electrode material. Structural and morphological features of LiVPOF were characterized using X-ray diffraction and scanning electron microscopy techniques. The electrochemical studies have been investigated using cyclic voltammetry, galvanostatic charge/discharge studies, and electrochemical impedance spectroscopic techniques. The ionothermally obtained LiVPOF is modified to LiVPOF/f-graphene composite electrode to obtain high specific capacity, better rate performance, and longer cycle life. Even after 250 cycles, the LiVPOF/f-graphene composite electrode exhibited a specific capacity more than 84 % with good reversible de-intercalation/intercalation of Li-ions. This article also provides the comparative electrochemical performances of LiVPOF/f-graphene composite, LiVPOF/carbon, and LiVPOF/graphene composite electrodes in a nonaqueous rechargeable Li-ion battery system. Graphical Abstract: [Figure not available: see fulltext.

Preparation and electrochemical performances of nanoporous/cracked cobalt oxide layer for supercapacitors

Science.gov (United States)

Gobal, Fereydoon; Faraji, Masoud

2014-12-01

Nanoporous/cracked structures of cobalt oxide (Co3O4) electrodes were successfully fabricated by electroplating of zinc-cobalt onto previously formed TiO2 nanotubes by anodizing of titanium, leaching of zinc in a concentrated alkaline solution and followed by drying and annealing at 400 °C. The structure and morphology of the obtained Co3O4 electrodes were characterized by X-ray diffraction, EDX analysis and scanning electron microscopy. The results showed that the obtained Co3O4 electrodes were composed of the nanoporous/cracked structures with an average pore size of about 100 nm. The electrochemical capacitive behaviors of the nanoporous Co3O4 electrodes were investigated by cyclic voltammetry, galvanostatic charge-discharge studies and electrochemical impedance spectroscopy in 1 M NaOH solution. The electrochemical data demonstrated that the electrodes display good capacitive behavior with a specific capacitance of 430 F g-1 at a current density of 1.0 A g-1 and specific capacitance retention of ca. 80 % after 10 days of being used in electrochemical experiments, indicating to be promising electroactive materials for supercapacitors. Furthermore, in comparison with electrodes prepared by simple cathodic deposition of cobalt onto TiO2 nanotubes(without dealloying procedure), the impedance studies showed improved performances likely due to nanoporous/cracked structures of electrodes fabricated by dealloying of zinc, which provide fast ion and electron transfer routes and large reaction surface area with the ensued fast reaction kinetics.

In-situ SEM microchip setup for electrochemical experiments with water based solutions

International Nuclear Information System (INIS)

Jensen, E.; Købler, C.; Jensen, P.S.; Mølhave, K.

2013-01-01

Studying electrochemical (EC) processes with electron microscopes offers the possibility of achieving much higher resolution imaging of nanoscale processes in real time than with optical microscopes. We have developed a vacuum sealed liquid sample electrochemical cell with electron transparent windows, microelectrodes and an electrochemical reference electrode. The system, called the EC-SEM Cell, is used to study electrochemical reactions in liquid with a standard scanning electron microscope (SEM). The central component is a microfabricated chip with a thin (50 nm) Si-rich silicon nitride (SiNx) window with lithographically defined platinum microelectrodes. We show here the design principles of the EC-SEM system, its detailed construction and how it has been used to perform a range of EC experiments, two of which are presented here. It is shown that the EC-SEM Cell can survive extended in-situ EC experiments. Before the EC experiments we characterized the beam current being deposited in the liquid as this will affect the experiments. The first EC experiment shows the influence of the electron-beam (e-beam) on a nickel solution by inducing electroless nickel deposition on the window when increasing the current density from the e-beam. The second experiment shows electrolysis in EC-SEM Cell, induced by the built-in electrodes. - Highlights: • New in-situ SEM system for electrochemistry. • In-situ Beam current measurements through liquid. • In-situ SEM E-beam-induced electroless deposition of Ni. • In-situ electrolysis

In-situ SEM microchip setup for electrochemical experiments with water based solutions

Energy Technology Data Exchange (ETDEWEB)

Jensen, E., E-mail: eric.jensen@nanotech.dtu.dk [DTU Nanotech, Technical University of Denmark, Ørsteds Plads, Building 345E, 2800 Kongens Lyngby (Denmark); DTU CEN, Technical University of Denmark, Fysikvej, Building 307, 2800 Kongens Lyngby (Denmark); Købler, C., E-mail: carsten.kobler@nanotech.dtu.dk [DTU Nanotech, Technical University of Denmark, Ørsteds Plads, Building 345E, 2800 Kongens Lyngby (Denmark); DTU CEN, Technical University of Denmark, Fysikvej, Building 307, 2800 Kongens Lyngby (Denmark); Jensen, P.S., E-mail: psj@kemi.dtu.dk [DTU Kemi, Technical University of Denmark, Kemitorvet, Building 207, 2800 Kongens Lyngby (Denmark); Mølhave, K., E-mail: kristian.molhave@nanotech.dtu.dk [DTU Nanotech, Technical University of Denmark, Ørsteds Plads, Building 345E, 2800 Kongens Lyngby (Denmark)

2013-06-15

Studying electrochemical (EC) processes with electron microscopes offers the possibility of achieving much higher resolution imaging of nanoscale processes in real time than with optical microscopes. We have developed a vacuum sealed liquid sample electrochemical cell with electron transparent windows, microelectrodes and an electrochemical reference electrode. The system, called the EC-SEM Cell, is used to study electrochemical reactions in liquid with a standard scanning electron microscope (SEM). The central component is a microfabricated chip with a thin (50 nm) Si-rich silicon nitride (SiNx) window with lithographically defined platinum microelectrodes. We show here the design principles of the EC-SEM system, its detailed construction and how it has been used to perform a range of EC experiments, two of which are presented here. It is shown that the EC-SEM Cell can survive extended in-situ EC experiments. Before the EC experiments we characterized the beam current being deposited in the liquid as this will affect the experiments. The first EC experiment shows the influence of the electron-beam (e-beam) on a nickel solution by inducing electroless nickel deposition on the window when increasing the current density from the e-beam. The second experiment shows electrolysis in EC-SEM Cell, induced by the built-in electrodes. - Highlights: • New in-situ SEM system for electrochemistry. • In-situ Beam current measurements through liquid. • In-situ SEM E-beam-induced electroless deposition of Ni. • In-situ electrolysis.

Investigation of Electrochemically Deposited and Chemically Reduced Platinum Nanostructured Thin Films as Counter Electrodes in Dye-Sensitized Solar Cells

Directory of Open Access Journals (Sweden)

Chih-Hung Tsai

2018-02-01

Full Text Available In this paper, we demonstrated that platinum (Pt counter electrodes (CEs fabricated using electrochemical deposition and chemical reduction can replace conventional high-temperature thermally decomposed Pt electrodes. In this study, Pt electrodes were fabricated using thermal decomposition, electrochemical deposition, and chemical reduction, and the influence of the different Pt counter electrodes on the efficiency of the dye-sensitized solar cells (DSSCs was analyzed. The properties of the various Pt CEs were analyzed using scanning electron microscopy (SEM, surface area analysis, X-ray diffraction (XRD, electrochemical impedance spectroscopy (EIS, and cyclic voltammetry (CV. DSSCs with various Pt CEs were characterized using current density-voltage (J-V, incident photo-current conversion efficiency (IPCE, and EIS measurements. The results show that the power conversion efficiencies of these three types of DSSC devices were between 7.43% and 7.72%. The DSSCs based on the Pt electrode fabricated through electrochemical deposition exhibited the optimal power conversion efficiency. Because the processes of electrochemical deposition and chemical reduction do not require high-temperature sintering, these two methods are suitable for the fabrication of Pt on flexible plastic substrates.

Electrochemical and SEM studies of tetra-ammine platinum (II) (Pt(NH3)4)(OH)2 solution

International Nuclear Information System (INIS)

Wan Jeffrey Basirun

2002-01-01

Electrochemical studies include cyclic voltammetry with microelectrodes were done on a solution of tetra-ammine platinum (II) (Pt(NH 3 ) 4 )(OH) 2 at pH 13 and showed that the electrochemical reduction of this compound was no different from the tetra-ammine platinum (II) (Pt(NH 3 ) 4 )(HPO 4 ) at pH 10.4. The solution was instable to high temperatures and results have shown that electroplating can be done at a limited temperature range for longer periods of time or at higher temperatures for short periods of time. Scanning electron microscopy was done on some of the constant current electrodeposited samples at high temperatures and result obtained was satisfactory. (Authors)

The EKAR Process: application of electrochemical technologies to the treatment of industrial waste waters; Proceso EKAR: aplicacion de tecnologias electroquimicas al tratamiento de aguas residuales industriales

Energy Technology Data Exchange (ETDEWEB)

Alberti, J.; Sanchez, G.

2000-07-01

The EKAR process is a technology for treating waste and sewage by electrochemical oxidation. It is based on the oxidation of chemical compounds by means of anodic processes in which oxygen is transferred from the water to the products to be oxidised. This technology employs an electrochemical reactor and an intermediary oxidising agent to form intermediary oxidised species and/or to oxidize the contaminating species. This technology can be applied to effluents with high salinity, COD and/or toxicity, achieving reductions in these parameters of up to 95% at extremely competitive cost. (Author) 9 refs.

The Use Of Scanning Probe Microscopy To Investigate Crystal-Fluid Interfaces

International Nuclear Information System (INIS)

Orme, C A; Giocondi, J L

2007-01-01

Over the past decade there has been a natural drive to extend the investigation of dynamic surfaces in fluid environments to higher resolution characterization tools. Various aspects of solution crystal growth have been directly visualized for the first time. These include island nucleation and growth using transmission electron microscopy and scanning tunneling microscopy; elemental step motion using scanning probe microscopy; and the time evolution of interfacial atomic structure using various diffraction techniques. In this lecture we will discuss the use of one such in situ method, scanning probe microscopy, as a means of measuring surface dynamics during crystal growth and dissolution. We will cover both practical aspects of imaging such as environmental control, fluid flow, and electrochemical manipulation, as well as the types of physical measurements that can be made. Measurements such as step motion, critical lengths, nucleation density, and step fluctuations, will be put in context of the information they provide about mechanistic processes at surfaces using examples from metal and mineral crystal growth

Electrochemical corrosion behavior of AZ91D alloy in ethylene glycol

International Nuclear Information System (INIS)

Fekry, A.M.; Fatayerji, M.Z.

2009-01-01

The effect of concentration on the corrosion behavior of Mg-based alloy AZ91D was investigated in ethylene glycol-water solutions using electrochemical techniques i.e. potentiodynamic polarization, electrochemical impedance measurements (EIS) and surface examination via scanning electron microscope (SEM) technique. This can provide a basis for developing new coolants for magnesium alloy engine blocks. Corrosion behavior of AZ91D alloy by coolant is important in the automotive industry. It was found that the corrosion rate of AZ91D alloy decreased with increasing concentration of ethylene glycol. For AZ91D alloy in chloride >0.05 M or fluoride 0.05 M for fluoride containing ethylene glycol solution, some inhibition effect has been observed. The corrosion of AZ91D alloy in the blank can be effectively inhibited by addition of 0.05 mM paracetamol that reacts with AZ91D alloy and forms a protective film on the surface at this concentration as confirmed by surface examination.

Nickel oxide/hydroxide nanoplatelets synthesized by chemical precipitation for electrochemical capacitors

International Nuclear Information System (INIS)

Wu, M.-S.; Hsieh, H.-H.

2008-01-01

Nickel hydroxide powder prepared by directly chemical precipitation method at room temperature has a nanoplatelet-like morphology and could be converted into nickel oxide at annealing temperature higher than 300 deg. C, confirmed by the thermal gravimetric analysis and X-ray diffraction. Annealing temperature influences significantly both the electrical conductivity and the specific surface area of nickel oxide/hydroxide powder, and consequently determines the capacitor behavior. Electrochemical capacitive behavior of the synthesized nickel hydroxide/oxide film is investigated by cyclic voltammetry and electrochemical impedance spectroscope methods. After 300 deg. C annealing, the highest specific capacitance of 108 F g -1 is obtained at scan rate of 10 mV s -1 . When annealing temperature is lower than 300 deg. C, the electrical conductivity of nickel hydroxide dominates primarily the capacitive behavior. When annealing temperature is higher than 300 deg. C, both electrical conductivity and specific surface area of the nickel oxide dominate the capacitive behavior

Unusual electrochemical response of ZnO nanowires-decorated multiwalled carbon nanotubes

International Nuclear Information System (INIS)

Mo Guangquan; Ye Jianshan; Zhang Weide

2009-01-01

A novel type of ZnO nanowires-modified multiwalled carbon nanotubes (MWCNTs) nanocomposite (ZnO-NWs/MWCNTs) has been prepared by a hydrothermal process. The ZnO-NWs/MWCNTs nanocomposite has a uniform surface distribution and large coverage of ZnO nanowires onto MWCNTs with 3D configuration, which was characterized by scanning electron microscopy. Cyclic voltammetry and electrochemical impedance spectroscopy methods were applied to investigate the electrochemical properties of ZnO-NWs/MWCNTs nanocomposite. Surprisingly, unlike the conventional n-type semiconducting ZnO nanowires grown on Ta substrate, the ZnO-NWs/MWCNTs nanocomposite exhibits excellent electron transfer capability and gives a pair of well-defined symmetric redox peaks towards ferricyanide probe. What's more, the ZnO-NWs/MWCNTs nanocomposite shows remarkable electrocatalytic activity (current response increased 4 folds at 0.3 V) towards H 2 O 2 by comparing with bare MWCNTs. The ZnO-NWs/MWCNTs nanocomposite could find applications in novel biosensors and other electronic devices.

An electrochemical immunosensor based on pristine graphene for rapid determination of ractopamine

Science.gov (United States)

Qi, Shaopeng; Zhao, Bo; Zhou, Bo; Jiang, Xiaoqing

2017-10-01

A new electrochemical immunosensor for fast determination of ractopamine (RAC) is fabricated based on pristine graphene (PG). The PG provides a microenvironment beneficial the immobilization of RAC, promotes the electron transfer, and raises the sensitivity of the immunosensor. The free RAC in solution can be effectively measured based on the competitive immunoreaction between RAC-antibody and RAC. The calibration graph shows linearity over the concentration ranges of 0.1-10 and 10-4000 ng mL-1. The proposed immunosensor displays a satisfactory stability, selectivity, and reproducibility and has been applied to the quantificational detection of RAC in real pork samples.

Electrochemical impedance spectroscopy investigation on indium tin oxide films under cathodic polarization in NaOH solution

International Nuclear Information System (INIS)

Gao, Wenjiao; Cao, Si; Yang, Yanze; Wang, Hao; Li, Jin; Jiang, Yiming

2012-01-01

The electrochemical corrosion behaviors of indium tin oxide (ITO) films under the cathodic polarization in 0.1 M NaOH solution were investigated by electrochemical impedance spectroscopy. The as-received and the cathodically polarized ITO films were characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy and X-ray diffraction for morphological, compositional and structural studies. The results showed that ITO films underwent a corrosion process during the cathodic polarization and the main component of the corrosion products was body-centered cubic indium. The electrochemical impedance parameters were related to the effect of the cathodic polarization on the ITO specimens. The capacitance of ITO specimens increased, while the charge transfer resistance and the inductance decreased with the increase of the polarization time. The proposed mechanism indicated that the corrosion products (metallic indium) were firstly formed during the cathodic polarization and then absorbed on the surface of the ITO film. As the surface was gradually covered by indium particles, the corrosion process was suppressed. - Highlights: ► Cathodic polarization of indium tin oxide (ITO) in 0.1 M NaOH. ► Cathodic polarization studied with electrochemical impedance spectroscopy. ► ITO underwent a corrosion attack during cathodic polarization, indium was observed. ► Electrochemical parameters of ITO were obtained using equivalent electrical circuit. ► A corrosion mechanism is proposed.

Electrochemical analysis

International Nuclear Information System (INIS)

Hwang, Hun

2007-02-01

This book explains potentiometry, voltametry, amperometry and basic conception of conductometry with eleven chapters. It gives the specific descriptions on electrochemical cell and its mode, basic conception of electrochemical analysis on oxidation-reduction reaction, standard electrode potential, formal potential, faradaic current and faradaic process, mass transfer and overvoltage, potentiometry and indirect potentiometry, polarography with TAST, normal pulse and deferential pulse, voltammetry, conductometry and conductometric titration.

Effects of transition-metal ions on the morphology and electrochemical properties of δ-MnO2 for supercapacitors

Science.gov (United States)

Wang, Jia-Wei; Chen, Ya; Chen, Bai-Zhen

2014-11-01

δ-MnO2 materials doped with transition-metal cations (Zn, Co, and Ag) were successfully synthesized using a hydrothermal technique. The structures and morphologies of the obtained oxides were analyzed using X-ray diffraction, scanning electron microscopy and Brunauer-Emmett-Teller measurements. Additionally, the electrochemical properties were evaluated through cyclic voltammetry, electrochemical impedance spectroscopy and galvanostatic cycling measurements. The results indicate that the pure and doped samples crystallize in the δ form with a layered structure and that the Mn/Zn, Mn/Co and Mn/Ag molar ratios are all approximately 1:0.09. Both the Zn-doped and pure MnO2 materials exhibit a petal-like morphology; however, the former has a higher specific surface area of up to 98.97m2 g-1. Furthermore, the Zn-doped MnO2 exhibits a near-rectangular cyclic voltammetry (CV) curve with broad quasi-reversible redox peaks and a specific capacitance of 182.9 F g-1 at a CV scan rate of 2 mV s-1. The Co-doped material exhibits a distinct spiny-fiber morphology, and the electrochemical performance of this material is significantly worse than that of pure MnO2. The average attenuation rate of the Ag-doped material is only 0.028% after 1000 cycles, which is lower than that of pure MnO2.

Reactivity at the film/solution interface of ex situ prepared bismuth film electrodes: A scanning electrochemical microscopy (SECM) and atomic force microscopy (AFM) investigation

International Nuclear Information System (INIS)

Hocevar, Samo B.; Daniele, Salvatore; Bragato, Carlo; Ogorevc, Bozidar

2007-01-01

Bismuth film electrodes (BiFEs) prepared ex situ with and without complexing bromide ions in the modification solution were investigated using scanning electrochemical microscopy (SECM) and atomic force microscopy (AFM). A feedback mode of the SECM was employed to examine the conductivity and reactivity of a series of thin bismuth films deposited onto disk glassy carbon substrate electrodes (GCEs) of 3 mm in diameter. A platinum micro-electrode (φ = 25 μm) was used as the SECM tip, and current against tip/substrate distance was recorded in solutions containing either Ru(NH 3 ) 6 3+ or Fe(CN) 6 4- species as redox mediators. With both redox mediators positive feedback approach curves were recorded, which indicated that the bismuth film deposition protocol associated with the addition of bromide ions in the modification solution did not compromise the conductivity of the bismuth film in comparison with that prepared without bromide. However, at the former Bi film a slight kinetic hindering was observed in recycling Ru(NH 3 ) 6 3+ , suggesting a different surface potential. On the other hand, the approach curves recorded by using Fe(CN) 6 4- showed that both types of the aforementioned bismuth films exhibited local reactivity with the oxidised form of the redox mediator, and that bismuth film obtained with bromide ions exhibited slightly lower reactivity. The use of SECM in the scanning operation mode allowed us to ascertain that the bismuth deposits were uniformly distributed across the whole surface of the glassy carbon substrate electrode. Comparative AFM measurements corroborated the above findings and additionally revealed a denser growth of smaller bismuth crystals over the surface of the substrate electrode in the presence of bromide ions, while the crystals were bigger but sparser in the absence of bromide ions in the modification solution

Synthesis of binary bismuth-cadmium oxide nanorods with sensitive electrochemical sensing performance

Energy Technology Data Exchange (ETDEWEB)

Wen, Yong [Xinjiang Univ., Xinjiang (China). School of Civil Engineering and Architecture; Pei, Lizhai; Wei, Tian [Anhui Univ. of Technology, Anhui (China). School of Materials Science and Engineering

2017-07-15

Binary bismuth-cadmium oxide nanorods have been synthesized by a simple hydrothermal process without templates and additives. X-ray diffraction and high-resolution transmission electron microscopy reveal that the nanorods possess single crystalline tetragonal Bi{sub 2}CdO{sub 4} phase. Scanning electron microscopy and transmission electron microscopy images show that the length and diameter of the nanorods are 20-300 nm and 5-10 μm, respectively. The formation of the binary bismuth-cadmium oxide nanorods is closely related to the hydrothermal parameters. The electrochemical sensing performance of the binary bismuth-cadmium oxide nanorods has been investigated using the nanorods as glassy carbon electrode modifiers. The detection limit is 0.19 μM with a linear range of 0.0005-2 mM. The nanorod-modified glassy carbon electrode exhibits good electrocatalytic activity toward L-cysteine and great application potential for electrochemical sensors.

Electrochemical deposition of buried contacts in high-efficiency crystalline silicon photovoltaic cells

DEFF Research Database (Denmark)

Jensen, Jens Arne Dahl; Møller, Per; Bruton, Tim

2003-01-01

This article reports on a newly developed method for electrochemical deposition of buried Cu contacts in Si-based photovoltaic ~PV! cells. Contact grooves, 20 mm wide by 40 mm deep, were laser-cut into Si PV cells, hereafter applied with a thin electroless NiP base and subsequently filled with Cu...... by electrochemical deposition at a rate of up to 10 mm per min. With the newly developed process, void-free, superconformal Cu-filling of the laser-cut grooves was observed by scanning electron microscopy and focused ion beam techniques. The Cu microstructure in grooves showed both bottom and sidewall texture......, with a grain-size decreasing from the center to the edges of the buried Cu contacts and a pronounced lateral growth outside the laser-cut grooves. The measured specific contact resistances of the buried contacts was better than the production standard. Overall performance of the new PV cells was equal...

Electrochemical immunoassay using magnetic beads for the determination of zearalenone in baby food: An anticipated analytical tool for food safety

International Nuclear Information System (INIS)

Hervas, Miriam; Lopez, Miguel Angel; Escarpa, Alberto

2009-01-01

In this work, electrochemical immunoassay involving magnetic beads to determine zearalenone in selected food samples has been developed. The immunoassay scheme has been based on a direct competitive immunoassay method in which antibody-coated magnetic beads were employed as the immobilisation support and horseradish peroxidase (HRP) was used as enzymatic label. Amperometric detection has been achieved through the addition of hydrogen peroxide substrate and hydroquinone as mediator. Analytical performance of the electrochemical immunoassay has been evaluated by analysis of maize certified reference material (CRM) and selected baby food samples. A detection limit (LOD) of 0.011 μg L -1 and EC 50 0.079 μg L -1 were obtained allowing the assessment of the detection of zearalenone mycotoxin. In addition, an excellent accuracy with a high recovery yield ranging between 95 and 108% has been obtained. The analytical features have shown the proposed electrochemical immunoassay to be a very powerful and timely screening tool for the food safety scene.

Electrochemical immunoassay using magnetic beads for the determination of zearalenone in baby food: an anticipated analytical tool for food safety.

Science.gov (United States)

Hervás, Miriam; López, Miguel Angel; Escarpa, Alberto

2009-10-27

In this work, electrochemical immunoassay involving magnetic beads to determine zearalenone in selected food samples has been developed. The immunoassay scheme has been based on a direct competitive immunoassay method in which antibody-coated magnetic beads were employed as the immobilisation support and horseradish peroxidase (HRP) was used as enzymatic label. Amperometric detection has been achieved through the addition of hydrogen peroxide substrate and hydroquinone as mediator. Analytical performance of the electrochemical immunoassay has been evaluated by analysis of maize certified reference material (CRM) and selected baby food samples. A detection limit (LOD) of 0.011 microg L(-1) and EC(50) 0.079 microg L(-1) were obtained allowing the assessment of the detection of zearalenone mycotoxin. In addition, an excellent accuracy with a high recovery yield ranging between 95 and 108% has been obtained. The analytical features have shown the proposed electrochemical immunoassay to be a very powerful and timely screening tool for the food safety scene.

Electrochemical immunoassay using magnetic beads for the determination of zearalenone in baby food: An anticipated analytical tool for food safety

Energy Technology Data Exchange (ETDEWEB)

Hervas, Miriam; Lopez, Miguel Angel [Departamento Quimica Analitica, Universidad de Alcala, Ctra. Madrid-Barcelona, Km. 33600, E-28871 Alcala de Henares, Madrid (Spain); Escarpa, Alberto, E-mail: alberto.escarpa@uah.es [Departamento Quimica Analitica, Universidad de Alcala, Ctra. Madrid-Barcelona, Km. 33600, E-28871 Alcala de Henares, Madrid (Spain)

2009-10-27

In this work, electrochemical immunoassay involving magnetic beads to determine zearalenone in selected food samples has been developed. The immunoassay scheme has been based on a direct competitive immunoassay method in which antibody-coated magnetic beads were employed as the immobilisation support and horseradish peroxidase (HRP) was used as enzymatic label. Amperometric detection has been achieved through the addition of hydrogen peroxide substrate and hydroquinone as mediator. Analytical performance of the electrochemical immunoassay has been evaluated by analysis of maize certified reference material (CRM) and selected baby food samples. A detection limit (LOD) of 0.011 {mu}g L{sup -1} and EC{sub 50} 0.079 {mu}g L{sup -1} were obtained allowing the assessment of the detection of zearalenone mycotoxin. In addition, an excellent accuracy with a high recovery yield ranging between 95 and 108% has been obtained. The analytical features have shown the proposed electrochemical immunoassay to be a very powerful and timely screening tool for the food safety scene.

Facile electrochemical synthesis of few layered graphene from discharged battery electrode and its

Directory of Open Access Journals (Sweden)

Santosh K. Tiwari

2017-05-01

Full Text Available A cost-effective, simple and non-hazardous route for synthesis of few-layered graphene from waste zinc carbon battery (ZCB electrodes via electrochemical expansion (ECE has been reported. In this synthesis, we have electrochemically exfoliated the graphene layers, by intercalating sodium dodecyl benzenesulfonate (SDBS surfactant into graphitic layers at different D.C. voltages with a constant SDBS concentration. The graphene sheets were isolated, purified and characterized by Transmission electron microscopy (TEM, Scanning electron microscopy (SEM, Fourier transform infrared spectrometry (FTIR, X-ray diffraction (XRD, Raman spectrometry, Ultraviolet absorption (UV, Selected area electron diffraction (SAED and Cyclic voltammetry. Best result was obtained at 4.5 V of D.C. A possible mechanism for the intercalation process has been proposed. A promising application of the produced material for supercapacitor application has also been explored in combination with polyaniline.

Corrosion resistance of plasma-anodized AZ91D magnesium alloy by electrochemical methods

International Nuclear Information System (INIS)

Barchiche, C.-E.; Rocca, E.; Juers, C.; Hazan, J.; Steinmetz, J.

2007-01-01

Anodic coatings formed on magnesium alloys by plasma anodization process are mainly used as protective coatings against corrosion. The effects of KOH concentration, anodization time and current density on properties of anodic layers formed on AZ91D magnesium alloy were investigated to obtain coatings with improved corrosion behaviour. The coatings were characterized by scanning electron microscopy (SEM), electron dispersion X-ray spectroscopy (EDX), X-ray diffraction (XRD) and micro-Raman spectroscopy. The film is porous and cracked, mainly composed of magnesium oxide (MgO), but contains all the elements present in the electrolyte and alloy. The corrosion behaviour of anodized Mg alloy was examined by using stationary and dynamic electrochemical techniques in corrosive water. The best corrosion resistance measured by electrochemical methods is obtained in the more concentrated electrolyte 3 M KOH + 0.5 M KF + 0.25 M Na 3 PO 4 .12 H 2 O, with a long anodization time and a low current density. A double electrochemical effects of the anodized layer on the magnesium corrosion is observed: a large inhibition of the cathodic process and a stabilization of a large passivation plateau

Solvothermal and electrochemical synthetic method of HKUST-1 and its methane storage capacity

Science.gov (United States)

Wahyu Lestari, Witri; Adreane, Marisa; Purnawan, Candra; Fansuri, Hamzah; Widiastuti, Nurul; Budi Rahardjo, Sentot

2016-02-01

A comparison synthetic strategy of Metal-Organic Frameworks, namely, Hongkong University of Techhnology-1 {HKUST-1[Cu3(BTC)]2} (BTC = 1,3,5-benzene-tri-carboxylate) through solvothermal and electrochemical method in ethanol:water (1:1) has been conducted. The obtained material was analyzed using powder X-ray diffraction, Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FTIR), Thermo-Gravimetric Analysis (TGA) and Surface Area Analysis (SAA). While the voltage in the electrochemical method are varied, ranging from 12 to 15 Volt. The results show that at 15 V the texture of the material has the best degree of crystallinity and comparable with solvothermal product. This indicated from XRD data and supported by the SEM image to view the morphology. The thermal stability of the synthesized compounds is up to 320 °C. The shape of the nitrogen sorption isotherm of the compound corresponds to type I of the IUPAC adsorption isotherm classification for microporous materials with BET surface area of 629.2 and 324.3 m2/g (for solvothermal and electrochemical product respectively) and promising for gas storage application. Herein, the methane storage capacities of these compounds are also tested.

Demolishing the competition: the longitudinal link between competitive video games, competitive gambling, and aggression.

Science.gov (United States)

Adachi, Paul J C; Willoughby, Teena

2013-07-01

The majority of research on the link between video games and aggression has focused on the violent content in games. In contrast, recent experimental research suggests that it is video game competition, not violence, that has the greatest effect on aggression in the short-term. However, no researchers have examined the long-term relationship between video game competition and aggression. In addition, if competition in video games is a significant reason for the link between video game play and aggression, then other competitive activities, such as competitive gambling, also may predict aggression over time. In the current study, we directly assessed the socialization (competitive video game play and competitive gambling predicts aggression over time) versus selection hypotheses (aggression predicts competitive video game play and competitive gambling over time). Adolescents (N = 1,492, 50.8 % female) were surveyed annually from Grade 9 to Grade 12 about their video game play, gambling, and aggressive behaviors. Greater competitive video game play and competitive gambling predicted higher levels of aggression over time, after controlling for previous levels of aggression, supporting the socialization hypothesis. The selection hypothesis also was supported, as aggression predicted greater competitive video game play and competitive gambling over time, after controlling for previous competitive video game play and competitive gambling. Our findings, taken together with the fact that millions of adolescents play competitive video games every day and that competitive gambling may increase as adolescents transition into adulthood, highlight the need for a greater understanding of the relationship between competition and aggression.

Modeling of Electrochemical Process for the Treatment of Wastewater Containing Organic Pollutants

Science.gov (United States)

Rodrigo, Manuel A.; Cañizares, Pablo; Lobato, Justo; Sáez, Cristina

Electrocoagulation and electrooxidation are promising electrochemical technologies that can be used to remove organic pollutants contained in wastewaters. To make these technologies competitive with the conventional technologies that are in use today, a better understanding of the processes involved must be achieved. In this context, the development of mathematical models that are consistent with the processes occurring in a physical system is a relevant advance, because such models can help to understand what is happening in the treatment process. In turn, a more detailed knowledge of the physical system can be obtained, and tools for a proper design of the processes, or for the analysis of operating problems, are attained. The modeling of these technologies can be carried out using single-variable or multivariable models. Likewise, the position dependence of the model species can be described with different approaches. In this work, a review of the basics of the modeling of these processes and a description of several representative models for electrochemical oxidation and coagulation are carried out. Regarding electrooxidation, two models are described: one which summarizes the pollution of a wastewater in only one model species and that considers a macroscopic approach to formulate the mass balances and other that considers more detailed profile of concentration to describe the time course of pollutants and intermediates through a mixed maximum gradient/macroscopic approach. On the topic of electrochemical coagulation, two different approaches are also described in this work: one that considers the hydrodynamic conditions as the main factor responsible for the electrochemical coagulation processes and the other that considers the chemical interaction of the reagents and the pollutants as the more significant processes in the description of the electrochemical coagulation of organic compounds. In addition, in this work it is also described a multivariable model

Novel Electrochemical Synthesis of Polypyrrole/Ag Nanocomposite and Its Electrocatalytic Performance towards Hydrogen Peroxide Reduction

OpenAIRE

Ruma Gupta; Kavitha Jayachandran; J. S. Gamare; B. Rajeshwari; Santosh K. Gupta; J. V. Kamat

2015-01-01

A simple electrochemical method of synthesis of polypyrrole/silver (PPy/Ag) nanocomposite is presented. The method is based on potentiodynamic polymerization of pyrrole followed by electrodeposition of silver employing a single potentiostatic pulse. The synthesized PPy film has embedded Ag nanocubes. The morphology and structure of the resulting nanocomposite were characterized by field emission scanning electron microscopy and X-ray diffraction. Electron paramagnetic resonance studies showed...

Photoassisted Electrochemical Treatment of Azo and Phtalocyanine Reactive Dyes in the Presence of Surfactants

Science.gov (United States)

Sala, Mireia; López-Grimau, Víctor; Gutiérrez-Bouzán, Carmen

2016-01-01

An electrochemical treatment (EC) was applied at different intensities to degrade the chromophoric groups of dyes C.I. Reactive Black 5 (RB5) and C.I. Reactive Blue 7 (Rb7) until uncolored species were obtained. Decolorization rate constants of the azo dye RB5 were higher than the phtalocyanine Rb7 ones. In addition, the EC treatment was more efficient at higher intensities, but these conditions significantly increased the generation of undesirable by-products such as chloroform. The combination of EC with UV irradiation (UVEC) drastically minimized the generation of chloroform. The photo-assisted electrochemical treatment was also able to achieve decolorization values of 99%. Finally, mixtures of dyes and surfactants were treated by EC and UVEC. In the presence of surfactants, the decolorization kinetic of dyes was slowed due to the competitive reactions of surfactants degradation. Both methods achieved total decolorization and in both cases, the generation of haloforms was negligible. PMID:28773335

Electrochemical behaviour of titanium coated stainless steel by r.f. sputtering in synthetic sweat solutions for electrode applications

International Nuclear Information System (INIS)

Fonseca, C.; Vaz, F.; Barbosa, M.A.

2004-01-01

The r.f. sputtering technique was used to deposit titanium thin films on stainless steel substrates, aiming at the application of the coated samples as skin contact materials for 'dry' active electrodes. In this work the electrochemical behaviour of the coated samples was investigated in synthetic sweat solutions and their performance was compared with that of uncoated stainless steel and bulk titanium. The characterisation of the samples was carried out by electrochemical techniques and scanning electron microscopy. The coated samples displayed corrosion resistance values in synthetic sweat solutions much higher than stainless steel samples and of the same order of the values measured for bulk titanium in the same conditions

Preparation and characterization of zinc oxide nanoparticles and their sensor applications for electrochemical monitoring of nucleic acid hybridization.

Science.gov (United States)

Yumak, Tugrul; Kuralay, Filiz; Muti, Mihrican; Sinag, Ali; Erdem, Arzum; Abaci, Serdar

2011-09-01

In this study, ZnO nanoparticles (ZNP) of approximately 30 nm in size were synthesized by the hydrothermal method and characterized by X-ray diffraction (XRD), Braun-Emmet-Teller (BET) N2 adsorption analysis and transmission electron microscopy (TEM). ZnO nanoparticles enriched with poly(vinylferrocenium) (PVF+) modified single-use graphite electrodes were then developed for the electrochemical monitoring of nucleic acid hybridization related to the Hepatitis B Virus (HBV). Firstly, the surfaces of polymer modified and polymer-ZnO nanoparticle modified single-use pencil graphite electrodes (PGEs) were characterized using scanning electron microscopy (SEM). The electrochemical behavior of these electrodes was also investigated using differential pulse voltammetry (DPV) and electrochemical impedance spectroscopy (EIS). Subsequently, the polymer-ZnO nanoparticle modified PGEs were evaluated for the electrochemical detection of DNA based on the changes at the guanine oxidation signals. Various modifications in DNA oligonucleotides and probe concentrations were examined in order to optimize the electrochemical signals that were generated by means of nucleic acid hybridization. After the optimization studies, the sequence-selective DNA hybridization was investigated in the case of a complementary amino linked probe (target), or noncomplementary (NC) sequences, or target and mismatch (MM) mixture in the ratio of (1:1). Copyright © 2011 Elsevier B.V. All rights reserved.

Hydrogen storage material, electrochemically active material, electrochemical cell and electronic equipment

NARCIS (Netherlands)

2008-01-01

The invention relates to a hydrogen storage material comprising an alloy of magnesium. The invention further relates to an electrochemically active material and an electrochemical cell provided with at least one electrode comprising such a hydrogen storage material. Also, the invention relates to

Influence of Monomer Concentration on the Morphologies and Electrochemical Properties of PEDOT, PANI, and PPy Prepared from Aqueous Solution

Directory of Open Access Journals (Sweden)

Shalini Kulandaivalu

2016-01-01

Full Text Available Poly(3,4-ethylenedioxyhiophene (PEDOT, polyaniline (PANI, and polypyrrole (PPy were prepared on indium tin oxide (ITO substrate via potentiostatic from aqueous solutions containing monomer and lithium perchlorate. The concentration of monomers was varied between 1 and 10 mM. The effects of monomer concentration on the polymers formation were investigated and compared by using Fourier transform infrared spectroscopy (FTIR, Raman spectroscopy, scanning electron microscopy (SEM, cyclic voltammetry (CV, and electrochemical impedance spectroscopy (EIS measurements. FTIR and Raman spectra showed no changes in the peaks upon the increment of the concentration. Based on the SEM images, the increment in monomer concentration gives significant effect on morphologies and eventually affects the electrochemical properties. PEDOT electrodeposited from 10 mM solution showed excellent electrochemical properties with the highest specific capacitance value of 12.8 mF/cm2.

Graphene-Paper Based Electrochemical Sensors

DEFF Research Database (Denmark)

Zhang, Minwei; Halder, Arnab; Cao, Xianyi

2017-01-01

in electrochemical sensors and energy technologies amongothers. In this chapter, we present some examples to overview recent advances in theresearch and development of two-dimensional (2D) graphene papers as new materialsfor electrochemical sensors. The chapter covers the design, fabrication, functionalizationand...... functionalization ofgraphene papers with polymer and nanoscale functional building blocks for electrochemical-sensing purposes. In terms of electrochemical-sensing applications, the emphasis ison enzyme-graphene and nanoparticle-graphene paper-based systems for the detectionof glucose. We finally conclude...

Electrochemical characterization of screen-printed and conventional carbon paste electrodes

Energy Technology Data Exchange (ETDEWEB)

Fanjul-Bolado, Pablo; Hernandez-Santos, David; Lamas-Ardisana, Pedro Jose [Departamento de Quimica Fisica y Analitica, Universidad de Oviedo, 33006 Oviedo, Asturias (Spain); Martin-Pernia, Alberto [Departamento de Ingenieria Electrica, Electronica de Computadores y Sistemas, Universidad de Oviedo, 33204 Gijon, Asturias (Spain); Costa-Garcia, Agustin [Departamento de Quimica Fisica y Analitica, Universidad de Oviedo, 33006 Oviedo, Asturias (Spain)], E-mail: costa@fq.uniovi.es

2008-04-01

This work compares the electroactivity of a conventional carbon paste electrode and non-pretreated commercially available screen-printed carbon electrodes (from Alderon Biosciences, University of Florence and DropSens) towards some benchmark redox couples like hexaammineruthenium (III), ferricyanide, p-aminophenol and hydroquinone. While cyclic voltammograms of Ru{sup 3+} did not show significative electron transfer reactivity differences between the electrodes tested, the other redox systems exhibited higher reversible behaviours on DropSens electrodes. Scanning electron microscopy and roughness analysis with a profilometer were applied to detect the surface morphology of the working electrodes. The roughness evaluated of the screen-printed carbon working electrodes increased in this order Alderon < University of Florence < DropSens. Finally, the most electrochemically active and rough unpretreated electrode (DropSens commercial screen-printed electrode) was used to study the electrochemical-chemical reaction mechanism of indigo carmine oxidation in 0.1 M sulphuric acid. This study showed that the adsorption of the oxidation product of indigo carmine is stabilized when it is adsorbed on the surface of the electrode.

Electrochemical characterization of screen-printed and conventional carbon paste electrodes

International Nuclear Information System (INIS)

Fanjul-Bolado, Pablo; Hernandez-Santos, David; Lamas-Ardisana, Pedro Jose; Martin-Pernia, Alberto; Costa-Garcia, Agustin

2008-01-01

This work compares the electroactivity of a conventional carbon paste electrode and non-pretreated commercially available screen-printed carbon electrodes (from Alderon Biosciences, University of Florence and DropSens) towards some benchmark redox couples like hexaammineruthenium (III), ferricyanide, p-aminophenol and hydroquinone. While cyclic voltammograms of Ru 3+ did not show significative electron transfer reactivity differences between the electrodes tested, the other redox systems exhibited higher reversible behaviours on DropSens electrodes. Scanning electron microscopy and roughness analysis with a profilometer were applied to detect the surface morphology of the working electrodes. The roughness evaluated of the screen-printed carbon working electrodes increased in this order Alderon < University of Florence < DropSens. Finally, the most electrochemically active and rough unpretreated electrode (DropSens commercial screen-printed electrode) was used to study the electrochemical-chemical reaction mechanism of indigo carmine oxidation in 0.1 M sulphuric acid. This study showed that the adsorption of the oxidation product of indigo carmine is stabilized when it is adsorbed on the surface of the electrode

Hydrothermal-reduction synthesis of manganese oxide nanomaterials for electrochemical supercapacitors.

Science.gov (United States)

Zhang, Xiong; Chen, Yao; Yu, Peng; Ma, Yanwei

2010-11-01

In the present work, amorphous manganese oxide nanomaterials have been synthesized by a common hydrothermal method based on the redox reaction between MnO4(-) and Fe(2+) under an acidic condition. The synthesized MnO2 samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and electrochemical studies. XRD results showed that amorphous manganese oxide phase was obtained. XPS quantitative analysis revealed that the atomic ratio of Mn to Fe was 3.5 in the MnO2 samples. TEM images showed the porous structure of the samples. Electrochemical properties of the MnO2 electrodes were studied using cyclic voltammetry and galvanostatic charge-discharge cycling in 1 M Na2SO4 aqueous electrolyte, which showed excellent pseudocapacitance properties. A specific capacitance of 192 Fg(-1) at a current density of 0.5 Ag(-1) was obtained at the potential window from -0.1 to 0.9 V (vs. SCE).

Structural and Electrochemical Properties of Lithium Nickel Oxide Thin Films

Directory of Open Access Journals (Sweden)

Gyu-bong Cho

2014-01-01

Full Text Available LiNiO2 thin films were fabricated by RF magnetron sputtering. The microstructure of the films was determined by X-ray diffraction and field-emission scanning electron microscopy. The electrochemical properties were investigated with a battery cycler using coin-type half-cells. The LiNiO2 thin films annealed below 500°C had the surface carbonate. The results suggest that surface carbonate interrupted the Li intercalation and deintercalation during charge/discharge. Although the annealing process enhanced the crystallization of LiNiO2, the capacity did not increase. When the annealing temperature was increased to 600°C, the FeCrNiO4 oxide phase was generated and the discharge capacity decreased due to an oxygen deficiency in the LiNiO2 thin film. The ZrO2-coated LiNiO2 thin film provided an improved discharge capacity compared to bare LiNiO2 thin film suggesting that the improved electrochemical characteristic may be attributed to the inhibition of surface carbonate by ZrO2 coating layer.

Comparison of electrochemical method with ozonation, chlorination and monochloramination in drinking water disinfection

Energy Technology Data Exchange (ETDEWEB)

Li Hongna, E-mail: lihongna@gmail.com [Department of Environmental Engineering, Peking University, Key Laboratory of Water and Sediment Sciences, Ministry of Education, Beijing 100871 (China); Zhu Xiuping [Department of Environmental Engineering, Peking University, Key Laboratory of Water and Sediment Sciences, Ministry of Education, Beijing 100871 (China); Ni Jinren, E-mail: nijinren@iee.pku.edu.cn [Department of Environmental Engineering, Peking University, Key Laboratory of Water and Sediment Sciences, Ministry of Education, Beijing 100871 (China)

2011-11-30

inactivation of the two Bacillus was much slower than E. coli and S. aureus. As a result, the non-selectivity of electrochemical disinfection with BDD anode to different kinds of microorganisms was further proved, which was primarily controlled by the hydroxyl radicals existed in the free state. For each bacterium, the order of disinfection availability of the four processes was consistent. Finally, scanning electron microscopy (SEM) was implemented to observe the cell morphology. It was shown that cell surface damage was more obvious in electrochemical system with strong oxidants compared with that after ozone treatment, while the integrity of cells were not affected in weak oxidizing chlorine and monochloramine.

Comparison of electrochemical method with ozonation, chlorination and monochloramination in drinking water disinfection

International Nuclear Information System (INIS)

Li Hongna; Zhu Xiuping; Ni Jinren

2011-01-01

Bacillus was much slower than E. coli and S. aureus. As a result, the non-selectivity of electrochemical disinfection with BDD anode to different kinds of microorganisms was further proved, which was primarily controlled by the hydroxyl radicals existed in the free state. For each bacterium, the order of disinfection availability of the four processes was consistent. Finally, scanning electron microscopy (SEM) was implemented to observe the cell morphology. It was shown that cell surface damage was more obvious in electrochemical system with strong oxidants compared with that after ozone treatment, while the integrity of cells were not affected in weak oxidizing chlorine and monochloramine.

The Comparative Study of Electrochemical Capacitance Performance between Sulphur-Doped Co3O4 and CoS Anodes

Directory of Open Access Journals (Sweden)

Wei Xu

2016-01-01

Full Text Available Anode materials with high capacitance performance are highly desirable for supercapacitors (SCs. In this work, nanomaterials cobalt sulfide (CoS, sulphur-doped Co3O4 (S-Co3O4, and Co3O4 were fabricated on a carbon cloth substrate by hydrothermal method. The composition and morphology of the material were characterized by X-ray diffraction (XRD patterns and Scanning Electron Microscope (SEM. The electrochemical measurements were performed in a three-electrode system. The result shows that CoS nanomaterial as anode is of the best electrochemical performance, achieving areal capacitance of 1.98 F/cm2 at 2 mA/cm2 in a 5 M LiCl solution. Moreover, the CoS anode has long-term cycling stability with more than 85.7% capacitance retention after 10000 cycles, confirming its larger capacitance, good redox activity, and electrochemical stability.

Electrochemical extraction of neodymium by co-reduction with aluminum in LiCl–KCl molten salt

International Nuclear Information System (INIS)

Yan, Yong-De; Xu, Yan-Lu; Zhang, Mi-Lin; Xue, Yun; Han, Wei; Huang, Ying; Chen, Qiong; Zhang, Zhi-Jian

2013-01-01

The electrochemical behavior of Nd(III) ions in LiCl–KCl and LiCl–KCl–AlCl 3 melts on a Mo electrode at 723 K was studied by various electrochemical techniques. The results showed that Nd(III) ions are reduced to Nd(0) through two consecutive steps, and the underpotential deposition of neodymium on pre-deposited Al electrode formed two kinds of Al–Nd intermetallic compounds in LiCl–KCl–AlCl 3 solutions. The electrochemical extraction of neodymium was carried out in LiCl–KCl–AlCl 3 melts on a Mo electrode at 873 K by potentiostatic and galvanostatic electrolysis. The extraction efficiency was 99.25% after potentiostatic electrolysis for 30 h. Al–Li–Nd bulk alloy was obtained by galvanostatic electrolysis. X-ray diffraction (XRD) suggested that Al 2 Nd and Al 3 Nd phases were formed in Al–Li–Nd alloy. The microstructure and micro-zone chemical analysis of Al–Li–Nd alloy were characterized by scanning electron microscopy (SEM) with energy dispersive spectrometry (EDS), respectively

Surface Properties of PAN-based Carbon Fibers Modified by Electrochemical Oxidization in Organic Electrolyte Systems

Directory of Open Access Journals (Sweden)

WU Bo

2016-09-01

Full Text Available PAN-based carbon fibers were modified by electrochemical oxidization using fatty alcohol polyoxyethylene ether phosphate (O3P, triethanolamine (TEOA and fatty alcohol polyoxyethylene ether ammonium phosphate (O3PNH4 as organic electrolyte respectively. Titration analysis, single fiber fracture strength measurement and field emission scanning electron microscopy (FE-SEM were used to evaluate the content of acidic functional group on the surface, mechanical properties and surface morphology of carbon fiber. The optimum process of electrochemical treatment obtained is at 50℃ for 2min and O3PNH4 (5%, mass fraction as the electrolyte with current density of 2A/g. In addition, the surface properties of modified carbon fibers were characterized by X-ray photoelectron spectroscopy (XPS and single fiber contact angle test. The results show that the hydrophilic acidic functional groups on the surface of carbon fiber which can enhance the surface energy are increased by the electrochemical oxidation using O3PNH4 as electrolyte, almost without any weakening to the mechanical properties of carbon fiber.

An Electrochemical pH Sensor Based on the Amino-Functionalized Graphene and Polyaniline Composite Film.

Science.gov (United States)

Su, W; Xu, J; Ding, Xianting

2016-12-01

Conventional glass-based pH sensors are usually fragile and space consuming. Herein, a miniature electrochemical pH sensor based on amino-functionalized graphene fragments and polyaniline (NH 2 -G/PANI) composite film is developed via simply one-pot electrochemical polymerization on the ITO-coated glass substrates. Cyclic Voltammetry (CV), Scanning Electron Microscopy (SEM), Transmission electron microscopy (TEM), X-ray Photoelectron Spectroscopy (XPS), and Raman Spectra are involved to confirm the successful synthesis and to characterize the properties of the NH 2 -G/PANI composite film. The developed electrochemical pH sensor presents fast response, high sensitivity (51.1 mV/pH) and wide detection range when applied to PBS solutions of pH values from 1 to 11. The robust reproducibility and good stability of the developed pH sensors are investigated as well. Compared to the conventional glass-based pH meters, the NH 2 -G/PANI composite film-based pH sensor could be a promising contender for the flexible and miniaturized pH-sensing devices.

Parallel- and serial-contact electrochemical metallization of monolayer nanopatterns: A versatile synthetic tool en route to bottom-up assembly of electric nanocircuits

Directory of Open Access Journals (Sweden)

Jonathan Berson

2012-02-01

Full Text Available Contact electrochemical transfer of silver from a metal-film stamp (parallel process or a metal-coated scanning probe (serial process is demonstrated to allow site-selective metallization of monolayer template patterns of any desired shape and size created by constructive nanolithography. The precise nanoscale control of metal delivery to predefined surface sites, achieved as a result of the selective affinity of the monolayer template for electrochemically generated metal ions, provides a versatile synthetic tool en route to the bottom-up assembly of electric nanocircuits. These findings offer direct experimental support to the view that, in electrochemical metal deposition, charge is carried across the electrode–solution interface by ion migration to the electrode rather than by electron transfer to hydrated ions in solution.

Electrochemical Behavior Assessment of As-Cast Mg-Y-RE-Zr Alloy in Phosphate Buffer Solutions (X Na3PO4 + Y Na2HPO4) Using Electrochemical Impedance Spectroscopy and Mott-Schottky Techniques

Science.gov (United States)

Fattah-alhosseini, Arash; Asgari, Hamed

2018-05-01

In the present study, electrochemical behavior of as-cast Mg-Y-RE-Zr alloy (RE: rare-earth alloying elements) was investigated using electrochemical tests in phosphate buffer solutions (X Na3PO4 + Y Na2HPO4). X-ray diffraction techniques and Scanning electron microscopy equipped with energy dispersive x-ray spectroscopy were used to investigate the microstructure and phases of the experimental alloy. Different electrochemical tests such as potentiodynamic polarization (PDP), electrochemical impedance spectroscopy (EIS) and Mott-Schottky (M-S) analysis were carried out in order to study the electrochemical behavior of the experimental alloy in phosphate buffer solutions. The PDP curves and EIS measurements indicated that the passive behavior of the as-cast Mg-Y-RE-Zr alloy in phosphate buffer solutions was weakened by an increase in the pH, which is related to formation of an imperfect and less protective passive layer on the alloy surface. The presence of the insoluble zirconium particles along with high number of intermetallic phases of RE elements mainly Mg24Y5 in the magnesium matrix can deteriorate the corrosion performance of the alloy by disrupting the protective passive layer that is formed at pH values over 11. These insoluble zirconium particles embedded in the matrix can detrimentally influence the passivation. The M-S analysis revealed that the formed passive layers on Mg-Y-RE-Zr alloy behaved as an n-type semiconductor. An increase in donor concentration accompanying solutions of higher alkalinity is thought to result in the formation of a less resistive passive layer.

Competitive Self-Assembly Manifests Supramolecular Darwinism in Soft-Oxometalates

Science.gov (United States)

Das, Santu; Kumar, Saurabh; Mallick, Apabrita; Roy, Soumyajit

2015-09-01

Topological transformation manifested in inorganic materials shows manifold possibilities. In our present work, we show a clear topological transformation in a soft-oxometalate (SOM) system which was formed from its polyoxometalate (POM) precursor [PMo12@Mo72Fe30]. This topological transformation was observed due to time dependent competitive self-assembly of two different length scale soft-oxometalate moieties formed from this two-component host-guest reaction. We characterized different morphologies by scanning electron microscopy, electron dispersive scattering spectroscopy, dynamic light scattering, horizontal attenuated total reflection-infrared spectroscopy and Raman spectroscopy. The predominant structure is selected by its size in a sort of supramolecular Darwinian competition in this process and is described here.

Chemical and Electrochemical Synthesis of Polypyrrole Using Carrageenan as a Dopant: Polypyrrole/Multi-Walled Carbon Nanotube Nanocomposites

Directory of Open Access Journals (Sweden)

Mostafizur Rahaman

2018-06-01

Full Text Available In this article, iota-carrageenan (IC and kappa-carrageenan (KC are used as dopants for the chemical and electrochemical synthesis of polypyrrole (PPy. The composites of chemically synthesized PPy with multi-walled carbon nanotubes (MWNTs were prepared using an in situ technique. Both the dialyzed and non-dialyzed IC and KC were used as dopants for electrochemical polymerization of pyrrole. Chemically synthesized PPy and PPy/MWNTs composites were studied by ultraviolet visible (UV-vis absorption spectra to investigate the effect of the concentration and the incorporation of MWNTs. In addition, the electrical, thermal, mechanical, and microscopic characterizations of these films were performed to examine the effect of the dopants and MWNTs on these properties, along with their surface morphology. The films of electrochemically polymerized PPy were characterized using UV-vis absorption spectra, scanning electron microscopy, and cyclic voltammetry (CV. The results were then compared with the chemical polymerized PPy.

Electrodeposition synthesis and electrochemical properties of nanostructured γ-MnO 2 films

Science.gov (United States)

Chou, Shulei; Cheng, Fangyi; Chen, Jun

The thin films of carambola-like γ-MnO 2 nanoflakes with about 20 nm in thickness and at least 200 nm in width were prepared on nickel sheets by combination of potentiostatic and cyclic voltammetric electrodeposition techniques. The as-prepared MnO 2 nanomaterials, which were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS), were used as the active material of the positive electrode for primary alkaline Zn/MnO 2 batteries and electrochemical supercapacitors. Electrochemical measurements showed that the MnO 2 nanoflake films displayed high potential plateau (around 1.0 V versus Zn) in primary Zn/MnO 2 batteries at the discharge current density of 500 mA g -1 and high specific capacitance of 240 F g -1 at the current density of 1 mA cm -2. This indicated the potential application of carambola-like γ-MnO 2 nanoflakes in high-power batteries and electrochemical supercapacitors. The growth process for the one- and three-dimensional nanostructured MnO 2 was discussed on the basis of potentiostatic and cyclic voltammetric techniques. The present synthesis method can be extended to the preparation of other nanostructured metal-oxide films.

Nonenzymatic electrochemical sensor based on imidazole-functionalized graphene oxide for progesterone detection.

Science.gov (United States)

Gevaerd, Ava; Blaskievicz, Sirlon F; Zarbin, Aldo J G; Orth, Elisa S; Bergamini, Márcio F; Marcolino-Junior, Luiz H

2018-07-30

The modification of electrode surfaces has been the target of study for many researchers in order to improve the analytical performance of electrochemical sensors. Herein, the use of an imidazole-functionalized graphene oxide (GO-IMZ) as an artificial enzymatic active site for voltammetric determination of progesterone (P4) is described for the first time. The morphology and electrochemical performance of electrode modified with GO-IMZ were characterized by scanning electron microscopy and cyclic voltammetry, respectively. Under optimized conditions, the proposed sensor showed a synergistic effect of the GO sheets and the imidazole groups anchored on its backbone, which promoted a significant enhancement on electrochemical reduction of P4. Figures of merits such as linear dynamic response for P4 concentration ranging from 0.22 to 14.0 μmol L -1 , limit of detection of 68 nmol L -1 and limit of quantification and 210 nmol L -1 were found. In addition, presented a higher sensitivity, 426 nA L µmol -1 , when compared to the unmodified electrode. Overall, the proposed device showed to be a promising platform for a simple, rapid, and direct analysis of progesterone. Copyright © 2018 Elsevier B.V. All rights reserved.

Microwave synthesis of molybdenum doped LiFePO4/C and its electrochemical studies.

Science.gov (United States)

Naik, Amol; P, Sajan C

2016-05-10

A Mo-doped LiFePO4 composite was prepared successfully from an iron carbonyl complex by adopting a facile and rapid microwave assisted solid state method. The evolution of gases from the iron precursor produces a highly porous product. The formation and substitution of Mo in LiFePO4 were confirmed by X-ray diffraction; surface analysis was carried out by scanning electron microscopy, field emission scanning electron microscopy, and transmission electron microscopy. The electrochemical properties of the substituted LiFePO4 were examined by cyclic voltammetry, electrochemical impedance spectroscopy and by recording charge-discharge cycles. It was observed that the as prepared composites consisted of a single phase orthorhombic olivine-type structure, where Mo(6+) was successfully introduced into the M2(Fe) sites. Incorporation of supervalent Mo(6+) introduced Li(+) ion vacancies in LiFePO4. The synthesized material facilitated lithium ion diffusion during charging/discharging due to the charge compensation effect and porosity. The battery performance studies showed that LiMo0.05Fe0.095PO4 exhibited a maximum capacity of 169.7 mA h g(-1) at 0.1 C current density, with admirable stability retention. Even at higher current densities, the retention of the specific capacity was exceptional.

Micro-electrochemical characterization of galvanic corrosion of TA2/316L composite plate

Energy Technology Data Exchange (ETDEWEB)

Cheng, X.; Li, X.; Dong, C.; Xiao, K. [Corrosion and Protection Center, University of Science and Technology Beijing (China)

2011-12-15

Galvanic corrosion behavior of TA2/316L composite plate was investigated in the solution of 3.5 wt% NaCl by galvanic potential monitoring, scanning localized electrochemical impedance spectroscopy (LEIS) and scanning vibrating micro-electrode (SVME) techniques. The results demonstrated that the pitting corrosion resistance of 316L for the galvanic combination sample is lower, and the coupled current density is higher than for the single 316L sample. It indicates that the galvanic action works on the corrosion behavior of the TA2 titanium alloy/316L stainless steel galvanic combination in sodium chloride solution. The galvanic effect width was determined as 1500 {mu}m. (Copyright copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Amperometric sensing of NADH and ethanol using a hybrid film electrode modified with electrochemically fabricated zirconia nanotubes and poly (acid fuchsin)

International Nuclear Information System (INIS)

Liu, X.; Li, B.; Zhan, G.; Liu, C.; Li, C.; Ma, M.

2012-01-01

We report on a glassy carbon electrode (GCE) modified with a film of chitosin containing acid fuchsin (AF) adsorbed onto zirconia nanotubes. The mixture was polymerized by cyclic voltammetric scannings in the potential range from - 0. 8 V to +1. 3 V in buffer solution to produce a hybrid film electrode (nano-ZrO 2 /PAF/GCE). The morphology of the hybrid film electrode surface was characterized by scanning electron microscopy. Its electrochemical properties were studied via electrochemical impedance spectroscopy. The electrochemical response of nicotinamide adenine dinucleotide (NADH) was investigated by differential pulse voltammetry and amperometry. The results indicated that the nano-ZrO 2 /PAF/GCE possesses well synergistic catalytic activity towards NADH. Compared to an unmodified GCE, the oxidation overpotential is negatively shifted by 224 mV, and the oxidation current is significantly increased. Under optimal conditions, the amperometric response is linearly proportional to the concentration of NADH in the 1. 0 - 100. 0 μM concentration range. Ethanol also can be determined by amperometry if alcohol dehydrogenase and NADH are added to the sample. Two linear relationships between current and alcohol concentration were obtained. They cover the range from 0. 03 to 1. 0 mM, and from 1. 0 to 12. 0 mM. (author)

Electrochemical force microscopy

Energy Technology Data Exchange (ETDEWEB)

Kalinin, Sergei V.; Jesse, Stephen; Collins, Liam F.; Rodriguez, Brian J.

2017-01-10

A system and method for electrochemical force microscopy are provided. The system and method are based on a multidimensional detection scheme that is sensitive to forces experienced by a biased electrode in a solution. The multidimensional approach allows separation of fast processes, such as double layer charging, and charge relaxation, and slow processes, such as diffusion and faradaic reactions, as well as capturing the bias dependence of the response. The time-resolved and bias measurements can also allow probing both linear (small bias range) and non-linear (large bias range) electrochemical regimes and potentially the de-convolution of charge dynamics and diffusion processes from steric effects and electrochemical reactivity.

On the mechanism of electrochemical ammonia synthesis on the Ru catalyst.

Science.gov (United States)

Back, Seoin; Jung, Yousung

2016-04-07

We theoretically investigate the electrochemical N2 reduction reaction (NRR) mechanism to produce NH3 on the Ru catalyst. All possible N-N dissociation steps during the reduction processes were evaluated along with the conventional associative and dissociative pathways. Based on the calculated free energy diagrams, it is revealed that the kinetically facile intermediate dissociative pathways during the NRR require a thermodynamic limiting potential (-0.71 V) similar to the associative pathway (-0.68 V), although the initial dissociative pathway as in the Haber-Bosch process has a substantial kinetic barrier for the N-N bond dissociation. The competitive hydrogen evolution is found to be a major hurdle for achieving a high efficiency for the electrochemical nitrogen reduction. In the low overpotential region, the hydrogen adsorption is thermodynamically more favorable than the protonation of N2, thereby reducing the number of active sites for the N2 activation. A comparison of free energies in the presence of different H-coverages on the Ru further demonstrates that the H-coverage can significantly increase the energy barrier for the first protonation of N2, resulting in a change of the potential determining step and an increase in the overpotentials.

Electrochemical characteristics of Shewanella loihica on carbon nanotubes-modified graphite surfaces

International Nuclear Information System (INIS)

Zhang, Xiaoming; Epifanio, Monica; Marsili, Enrico

2013-01-01

Highlights: • We deposited CNT coatings on graphite electrode by electrophoretic deposition. • CNT coating increased extracellular electron transfer in Shewanella loihica biofilms. • Thick electroactive biofilms hinder the electroactivity of CNT coatings. -- Abstract: High specific surface and electrocatalytic activity of the electrode surface favour extracellular electron transfer from electrochemically active biofilms to polarized electrodes. We coated layer-by-layer carbon nanotubes (CNTs) on graphite electrodes through electrophoretic deposition, thus increasing the electrocatalytic activity. After determining the optimal number of CNT layers through electrochemical methods, we grew Shewanella loihica PV-4 biofilms on the CNT-coated electrodes to quantify the increase in extracellular electron transfer rate compared with unmodified electrodes. Current density on CNT-modified electrodes was 1.7 times higher than that observed on unmodified electrodes after 48 h from inoculation. Rapid microbial cells attachment on CNT-coated electrodes, as determined from scanning electronic microscopy, explained the rapid increase of the current. Also, the CNT reduced the charge transfer resistance of the graphite electrodes, as measured by Electrochemical Impedance Spectroscopy. However, the electrocatalytic activity of the CNT-coated electrode decreased as the biofilm grew thicker and covered the CNT-coating. These result confirmed that surface-modified electrodes improve the electron transfer rate in thin biofilms (<5 μm), but are not feasible for power production in microbial fuel cells, where the biofilm thickness is much higher

A highly selective copper-indium bimetallic electrocatalyst for the electrochemical reduction of aqueous CO2to CO

KAUST Repository

Rasul, Shahid

2014-12-23

The challenge in the electrochemical reduction of aqueous carbon dioxide is in designing a highly selective, energy-efficient, and non-precious-metal electrocatalyst that minimizes the competitive reduction of proton to form hydrogen during aqueous CO2 conversion. A non-noble metal electrocatalyst based on a copper-indium (Cu-In) alloy that selectively converts CO2 to CO with a low overpotential is reported. The electrochemical deposition of In on rough Cu surfaces led to Cu-In alloy surfaces. DFT calculations showed that the In preferentially located on the edge sites rather than on the corner or flat sites and that the d-electron nature of Cu remained almost intact, but adsorption properties of neighboring Cu was perturbed by the presence of In. This preparation of non-noble metal alloy electrodes for the reduction of CO2 provides guidelines for further improving electrocatalysis.

Hydrothermal synthesis of flower-like MoS2 nanospheres for electrochemical supercapacitors.

Science.gov (United States)

Zhou, Xiaoping; Xu, Bin; Lin, Zhengfeng; Shu, Dong; Ma, Lin

2014-09-01

Flower-like MoS2 nanospheres were synthesized by a hydrothermal route. The structure and surface morphology of the as-prepared MoS2 was characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The supercapacitive behavior of MoS2 in 1 M KCl electrolyte was studied by means of cyclic voltammetry (CV), constant current charge-discharge cycling (CD) and electrochemical impedance spectroscopy (EIS). The XRD results indicate that the as-prepared MoS2 has good crystallinity. SEM images show that the MoS2 nanospheres have uniform sizes with mean diameter about 300 nm. Many nanosheets growing on the surface make the MoS2 nanospheres to be a flower-like structure. The specific capacitance of MoS2 is 122 F x g(-1) at 1 A x g(-1) or 114 F x g(-1) at 2 mv s(-1). All the experimental results indicate that MoS2 is a promising electrode material for electrochemical supercapacitors.

Combination Carbon Nanotubes with Graphene Modified Natural Graphite and Its Electrochemical Performance

Directory of Open Access Journals (Sweden)

DENG Ling-feng

2017-04-01

Full Text Available The CNTs/rGO/NG composite lithiumion battery anode material was synthesized by thermal reducing, using graphene oxide (GO and carbon nanotubes (CNTs as precursors for a 5 ∶ 3 proportion. The morphology, structure, and electrochemical performance of the composite were characterized by scanning electron microscopy(SEM, X-ray diffractometry(XRD, Fourier transform infrared spectra (FTIR and electrochemical measurements. The results show that reduced graphene oxide and carbon nanotubes form a perfect three-dimensional network structure on the surface of natural graphite. CNTs/rGO/NG composite has good rate performance and cycle life,compared with pure natural graphite.The initial discharge capacity of designed anode is 479mAh/g at 0.1C, the reversible capacity up to 473mAh/g after 100 cycles,the capacity is still 439.5mAh/g, the capacity retention rate is 92%,and the capacity is 457, 433, 394mAh/g at 0.5, 1, 5C, respectively.

Electrochemical Water Oxidation by a Catalyst-Modified Metal-Organic Framework Thin Film

Energy Technology Data Exchange (ETDEWEB)

Lin, Shaoyang; Pineda-Galvan, Yuliana; Maza, William A.; Epley, Charity C.; Zhu, Jie; Kessinger, Matthew C.; Pushkar, Yulia; Morris, Amanda J. (VP); (Purdue)

2016-12-15

Water oxidation, a key component in artificial photosynthesis, requires high overpotentials and exhibits slow reaction kinetics that necessitates the use of stable and efficient heterogeneous water-oxidation catalysts (WOCs). Here, we report the synthesis of UiO-67 metal–organic framework (MOF) thin films doped with [Ru(tpy)(dcbpy)OH2]2+ (tpy=2,2':6',2''-terpyridine, dcbpy=5,5'-dicarboxy-2,2'-bipyridine) on conducting surfaces and their propensity for electrochemical water oxidation. The electrocatalyst oxidized water with a turnover frequency (TOF) of (0.2±0.1) s-1 at 1.71 V versus the normal hydrogen electrode (NHE) in buffered solution (pH~7) and exhibited structural and electrochemical stability. The electroactive sites were distributed throughout the MOF thin film on the basis of scan-ratedependent voltammetry studies. This work demonstrates a promising way to immobilize large concentrations of electroactive WOCs into a highly robust MOF scaffold and paves the way for future photoelectrochemical water-splitting systems.

Graphene/SnO2 nanocomposite-modified electrode for electrochemical detection of dopamine

Directory of Open Access Journals (Sweden)

R. Nurzulaikha

2015-09-01

Full Text Available A graphene-tin oxide (G-SnO2 nanocomposite was prepared via a facile hydrothermal route using graphene oxide and Sn precursor solution without addition of any surfactant. The hydrothermally synthesized G-SnO2 nanocomposite was characterized using a field emission scanning electron microscope (FESEM, high resolution transmission electron microscope (HRTEM, X-ray diffraction (XRD, and energy dispersive spectroscopy (EDS. A homogeneous deposition of SnO2 nanoparticles with an average particle size of 10 nm on the graphene was observed in the FESEM and HRTEM images. The G-SnO2 nanocomposite was used to fabricate a modified electrode for the electrochemical detection of dopamine (DA in the presence of ascorbic acid (AA. Differential pulse voltammetry (DPV showed a limit of detection (LoD of 1 μM (S/N = 3 in the presence of ascorbic acid (AA. Keywords: Graphene, Tin oxide, Nanocomposite, Electrochemical sensor, Biosensor, Dopamine

Sustainable remediation: electrochemically assisted microbial dechlorination of tetrachloroethene-contaminated groundwater.

Science.gov (United States)

Patil, Sayali S; Adetutu, Eric M; Rochow, Jacqueline; Mitchell, James G; Ball, Andrew S

2014-01-01

Microbial electric systems (MESs) hold significant promise for the sustainable remediation of chlorinated solvents such as tetrachlorethene (perchloroethylene, PCE). Although the bio-electrochemical potential of some specific bacterial species such as Dehalcoccoides and Geobacteraceae have been exploited, this ability in other undefined microorganisms has not been extensively assessed. Hence, the focus of this study was to investigate indigenous and potentially bio-electrochemically active microorganisms in PCE-contaminated groundwater. Lab-scale MESs were fed with acetate and carbon electrode/PCE as electron donors and acceptors, respectively, under biostimulation (BS) and BS-bioaugmentation (BS-BA) regimes. Molecular analysis of the indigenous groundwater community identified mainly Spirochaetes, Firmicutes, Bacteroidetes, and γ and δ-Proteobacteria. Environmental scanning electron photomicrographs of the anode surfaces showed extensive indigenous microbial colonization under both regimes. This colonization and BS resulted in 100% dechlorination in both treatments with complete dechlorination occurring 4 weeks earlier in BS-BA samples and up to 11.5 μA of current being generated. The indigenous non-Dehalococcoides community was found to contribute significantly to electron transfer with ∼61% of the current generated due to their activities. This study therefore shows the potential of the indigenous non-Dehalococcoides bacterial community in bio-electrochemically reducing PCE that could prove to be a cost-effective and sustainable bioremediation practice. © 2013 The Authors. Microbial Biotechnology published by John Wiley & Sons Ltd and Society for Applied Microbiology.

Acoustic, electrochemical and microscopic characterization of interaction of Arthrospira platensis biofilm and heavy metal ions

OpenAIRE

Tekaya , Nadèje; Gammoudi , Ibtissèm; Braiek , Mohamed; Tarbague , Hakim; Morote , Fabien; Raimbault , Vincent; Sakly , Nawfel; Rebière , Dominique; Ben Ouada , Hatem; Lagarde , Florence; Ben Ouada , Hafedh; Cohen-Bouhacina , Touria; Déjous , Corinne; Jaffrezic-Renault , Nicole

2013-01-01

International audience; This study examines a biofilm of Arthrospira platensis and its interactions with cadmium and mercury, using electrochemical admittance spectroscopy technique combined with highly sensitive Love wave platform for the real-time detection in liquid medium. Spirulina cells were immobilized via multilayers of polyelectrolyte (PEM) on Si/SiO2 surface of both transducers and characterized using atomic force microscopy (AFM). Scanning electron microscopy (SEM) cell images reve...

Materials for electrochemical capacitors

Science.gov (United States)

Simon, Patrice; Gogotsi, Yury

2008-11-01

Electrochemical capacitors, also called supercapacitors, store energy using either ion adsorption (electrochemical double layer capacitors) or fast surface redox reactions (pseudo-capacitors). They can complement or replace batteries in electrical energy storage and harvesting applications, when high power delivery or uptake is needed. A notable improvement in performance has been achieved through recent advances in understanding charge storage mechanisms and the development of advanced nanostructured materials. The discovery that ion desolvation occurs in pores smaller than the solvated ions has led to higher capacitance for electrochemical double layer capacitors using carbon electrodes with subnanometre pores, and opened the door to designing high-energy density devices using a variety of electrolytes. Combination of pseudo-capacitive nanomaterials, including oxides, nitrides and polymers, with the latest generation of nanostructured lithium electrodes has brought the energy density of electrochemical capacitors closer to that of batteries. The use of carbon nanotubes has further advanced micro-electrochemical capacitors, enabling flexible and adaptable devices to be made. Mathematical modelling and simulation will be the key to success in designing tomorrow's high-energy and high-power devices.

Electrochemical reduction of NOx

DEFF Research Database (Denmark)

Traulsen, Marie Lund

NO and NO2 (collectively referred to as NOx) are air pollutants, and the largest single contributor to NOx pollution is automotive exhaust. This study investigates electrochemical deNOx, a technology which aims to remove NOx from automotive diesel exhaust by electrochemical reduction of NOx to N2...... and O2. The focus in this study is on improving the activity and selectivity of solid oxide electrodes for electrochemical deNOx by addition of NOx storage compounds to the electrodes. Two different composite electrodes, La0.85Sr0.15MnO3-δ-Ce0.9Gd0.1O1.95 (LSM15-CGO10) and La0.85Sr0.15FeO3-δ-Ce0.9Gd0.1O......1.95 (LSF15-CGO10), have been investigated in combination with three different NOx storage compounds: BaO, K2O and MnOx. The main focus in the investigation has been on conversion measurements and electrochemical characterization, the latter by means of electrochemical impedance spectroscopy...

Adherence and electrochemical behavior of calcium titanate coatings onto 304 stainless steel substrate

Energy Technology Data Exchange (ETDEWEB)

Esguerra A, J.; Aguilar, Y. [Universidad del Valle, Escuela de Ingenieria de Materiales, TPMR, Calle 13 No. 100-00, A. A. 25360 Cali (Colombia); Aperador, W. [Escuela Colombiana de Ingenieria Julio Garavito, Escuela de Ingenieria Mecanica, AK 45 No. 205-59 (Autopista Norte), A. A. 14520 Bogota (Colombia); Alba de Sanchez, N. [Universidad Autonoma de Occidente, Grupo de Investigacion en Ciencia e Ingenieria de Materiales, Calle 25 No. 115-85, A. A. 2790 Cali (Colombia); Bolanos P, G.; Rincon, C., E-mail: johanna.esguerra@univalle.edu.co [Universidad del Cauca, Departamento de Fisica, Laboratorio de Fisica de Bajas Temperaturas, Calle 5 No. 4-70, A. A. 996 Popayan (Colombia)

2014-07-01

Calcium titanate has been proposed as a coating for biomedical applications but it has not been reported characterization of adhesion failure mechanisms or electrochemical properties in time. In this work have been studied these properties of a calcium titanate coating growth onto AISI 304 steel deposited by r.f. magnetron sputtering. It was found that the coating has a critical adhesive load of 6.53 ± 0.14 N. With respect to its electrochemical properties potentiodynamic polarization curves show that the calcium titanate coating provides protection to AISI 304 steel. However. EIS indicates that even though metal dissolution occur through the pores in the coating, this leads to the precipitation of salts that block pores; this precipitates layer acts like and additional barrier to the metal dissolution in the system. The coatings deposition was carried out via magnetron sputtering during 4 hours at 500 grades C. The crystal structure of the films was determined by using glancing incident X-ray diffraction. The chemical composition of deposited films was performed by impedance dispersive X-ray spectroscopy (EDX) in the scanning electron microscopy (Jeol JSM-649 OLV Sem), and the grain size and the roughness was obtained using an atomic force microscopy from Asylum Research MFP-3D using a cantilever silicon tip in non-contact mode and calculated by scanning probe image processor. (Author)

Adherence and electrochemical behavior of calcium titanate coatings onto 304 stainless steel substrate

International Nuclear Information System (INIS)

Esguerra A, J.; Aguilar, Y.; Aperador, W.; Alba de Sanchez, N.; Bolanos P, G.; Rincon, C.

2014-01-01

Calcium titanate has been proposed as a coating for biomedical applications but it has not been reported characterization of adhesion failure mechanisms or electrochemical properties in time. In this work have been studied these properties of a calcium titanate coating growth onto AISI 304 steel deposited by r.f. magnetron sputtering. It was found that the coating has a critical adhesive load of 6.53 ± 0.14 N. With respect to its electrochemical properties potentiodynamic polarization curves show that the calcium titanate coating provides protection to AISI 304 steel. However. EIS indicates that even though metal dissolution occur through the pores in the coating, this leads to the precipitation of salts that block pores; this precipitates layer acts like and additional barrier to the metal dissolution in the system. The coatings deposition was carried out via magnetron sputtering during 4 hours at 500 grades C. The crystal structure of the films was determined by using glancing incident X-ray diffraction. The chemical composition of deposited films was performed by impedance dispersive X-ray spectroscopy (EDX) in the scanning electron microscopy (Jeol JSM-649 OLV Sem), and the grain size and the roughness was obtained using an atomic force microscopy from Asylum Research MFP-3D using a cantilever silicon tip in non-contact mode and calculated by scanning probe image processor. (Author)

Preparation, electrochemical characterization and charge-discharge of reticulated vitreous carbon/polyaniline composite electrodes

International Nuclear Information System (INIS)

Dalmolin, Carla; Biaggio, Sonia R.; Rocha-Filho, Romeu C.; Bocchi, Nerilso

2009-01-01

Polyaniline was electrodeposited onto reticulated vitreous carbon - RVC - in order to obtain a tridimensional composite electrode. Three variations of these electrodes were analysed: a small-anion-doped polyaniline (RVC/Pani), a polyanion-doped polyaniline (RVC/PaniPSS) and a bi-layer type formed by an inner layer of the first electrode and an outer layer of the second one (RVC/Pani/PaniPSS). These composites were characterized by cyclic voltammetry, scanning electronic microscopy and electrochemical impedance spectroscopy. Photomicrographies, voltammetric profiles and impedance data pointed to different morphological and electrochemical characteristics for polyaniline doped with small or large anions, and a mixed behavior for the bi-layer electrodes. Charge-discharge tests for these tridimensional (3D) electrodes, employed as the cathode in lithium batteries, indicated better performance for the RVC/Pani electrode. These RVC composites presented higher specific capacities when compared with those obtained for Pani deposited onto bidimensional substrates.

Facile synthesis of polypyrrole nanofiber and its enhanced electrochemical performances in different electrolytes

Directory of Open Access Journals (Sweden)

C. K. Das

2012-12-01

Full Text Available A porous nanocomposite based on polypyrrole (PPy and sodium alginate (SA has been synthesized by easy, inexpensive, eco-friendly method. As prepared nanocomposite showed fibrillar morphology in transmission electron microscopic (TEM analysis. The average diameter of ~100 nm for the nanofibers was observed from scanning electron microscopic (SEM analysis. As prepared nanofiber, was investigated as an electrode material for supercapacitor application in different aqueous electrolyte solutions. PPy nanofiber showed enhanced electrochemical performances in 1M KCl solution as compared to 1M Na2SO4 solution. Maximum specific capacitance of 284 F/g was found for this composite in 1 M KCl electrolyte. It showed 76% specific capacitance retention after 600 cycles in 1 M KCl solution. Electrochemical Impedance Spectra showed moderate capacitive behavior of the composite in both the electrolytes. Further PPy nanofiber demonstrated higher thermal stability as compared to pure PPy.

Monitoring dynamic electrochemical processes with in situ ptychography

Science.gov (United States)

Kourousias, George; Bozzini, Benedetto; Jones, Michael W. M.; Van Riessen, Grant A.; Dal Zilio, Simone; Billè, Fulvio; Kiskinova, Maya; Gianoncelli, Alessandra

2018-03-01

The present work reports novel soft X-ray Fresnel CDI ptychography results, demonstrating the potential of this method for dynamic in situ studies. Specifically, in situ ptychography experiments explored the electrochemical fabrication of Co-doped Mn-oxide/polypyrrole nanocomposites for sustainable and cost-effective fuel-cell air-electrodes. Oxygen-reduction catalysts based on Mn-oxides exhibit relatively high activity, but poor durability: doping with Co has been shown to improve both reduction rate and stability. In this study, we examine the chemical state distribution of the catalytically crucial Co dopant to elucidate details of the Co dopant incorporation into the Mn/polymer matrix. The measurements were performed using a custom-made three-electrode thin-layer microcell, developed at the TwinMic beamline of Elettra Synchrotron during a series of experiments that were continued at the SXRI beamline of the Australian Synchrotron. Our time-resolved ptychography-based investigation was carried out in situ after two representative growth steps, controlled by electrochemical bias. In addition to the observation of morphological changes, we retrieved the spectroscopic information, provided by multiple ptychographic energy scans across Co L3-edge, shedding light on the doping mechanism and demonstrating a general approach for the molecular-level investigation complex multimaterial electrodeposition processes.

Palladium nanoparticles in electrochemical sensing of trace terazosin in human serum and pharmaceutical preparations

Energy Technology Data Exchange (ETDEWEB)

Sefid-sefidehkhan, Yasaman [Department of Chemistry, University of Mohaghegh Ardabili, Ardabil (Iran, Islamic Republic of); Nekoueian, Khadijeh [Laboratory of Green Chemistry, Faculty of Technology, Lappeenranta University of Technology, Sammonkatu 12, FI-50130 Mikkeli (Finland); Amiri, Mandana, E-mail: mandanaamiri@uma.ac.ir [Department of Chemistry, University of Mohaghegh Ardabili, Ardabil (Iran, Islamic Republic of); Sillanpaa, Mika [Laboratory of Green Chemistry, Faculty of Technology, Lappeenranta University of Technology, Sammonkatu 12, FI-50130 Mikkeli (Finland); Eskandari, Habibollah [Department of Chemistry, University of Mohaghegh Ardabili, Ardabil (Iran, Islamic Republic of)

2017-06-01

In this approach, palladium nanoparticle film was simply fabricated on the surface of carbon paste electrode by electrochemical deposition method. The film was characterized using scanning electron microscopy, electrochemical impedance spectroscopy and cyclic voltammetry. The prepared electrode exhibited an excellent electrocatalytic activity toward detection of trace amounts of terazosin, which is an antihypertensive drug. Under the optimum experimental conditions, a linear range of 1.0 × 10{sup −8}–1.0 × 10{sup −3} mol L{sup −1} with a detection limit of 1.9 × 10{sup −9} mol L{sup −1} was obtained for determination of terazosin using differential pulse voltammetry as a sensitive method. The efficiency of palladium nanoparticle film on the surface of carbon paste electrode successfully proved for determination of terazosin in pharmaceutical sample and human serum sample with promising recovery results. The effect of some foreign species has been studied. - Highlights: • PdNPs were simply fabricated by electrochemical deposition. • PdNPs exhibited an excellent electrocatalytic activity toward oxidation of terazosin. • Terazosin has been determined in pharmaceutical sample and human serum sample.

Microwave assisted synthesis of MnO2 on nickel foam-graphene for electrochemical capacitor

International Nuclear Information System (INIS)

Bello, A.; Fashedemi, O.O.; Fabiane, M.; Lekitima, J.N.; Ozoemena, K.I.; Manyala, N.

2013-01-01

Highlights: •Three-dimensional synthesis of graphene using CVD. •Hydrothermal deposition (microwave irradiation) of MnO 2 on graphene. •Morphologies of the composite reveals flower-like nanostructures of MnO 2 on graphene. •Composite exhibit excellent electrochemical performance. -- Abstract: A green chemistry approach (hydrothermal microwave irradiation) has been used to deposit manganese oxide on nickel foam-graphene. The 3D graphene was synthesized using nickel foam template by chemical vapor deposition (CVD) technique. Raman spectroscopy, X-ray diffraction (XRD), scanning electron and transmission electron microscopies (SEM and TEM) have been used to characterize structure and surface morphology of the composite, respectively. The Raman spectroscopy measurements on the samples reveal that 3D graphene consists of mostly few layers with low defect density. The composite was tested in a three electrode configuration for electrochemical capacitor, and exhibited a specific capacitance of 305 F g −1 at a current density of 1 A g −1 and showed excellent cycling stability. The obtained results demonstrate that microwave irradiation technique could be a promising approach to synthesis graphene based functional materials for electrochemical applications

Electrochemical performances of diamond-like carbon coatings on carbon steel, stainless steel, and brass

International Nuclear Information System (INIS)

Hadinata, Samuel-Sudibyo; Lee, Ming-Tsung; Pan, Szu-Jung; Tsai, Wen-Ta; Tai, Chen-Yi; Shih, Chuan-Feng

2013-01-01

Diamond-like carbon (DLC) coatings have been deposited onto stainless steel, carbon steel and brass by plasma-enhanced chemical vapor deposition, respectively. Atomic arrangement, chemical structure, surface morphology and cross-section microstructure of the DLC coatings were examined by X-ray diffraction, Raman scattering spectroscopy and scanning electron microscopy. The electrochemical behaviors of the DLC coatings in 3.5 wt.% NaCl solution were investigated by performing an open circuit potential (OCP) measurement and a potentiodynamic polarization test. The experimental results showed that properly deposited DLC coatings could cause an increase of OCP by hundreds of millivolts and a reduction of anodic current density by several orders of magnitude as compared to that of the substrate. The results also demonstrated that electrochemical techniques could be used as tools to detect the soundness of the DLC coating by examining OCP and polarization curve, which varied with the form of defect and depended on the type of substrate. - Highlights: ► The substrate could affect the quality of diamond-like carbon (DLC) coating. ► Defect-free DLC coating exhibited extremely low anodic current density. ► The quality of DLC coating on metal could be evaluated by electrochemical test

Electrochemical performances of diamond-like carbon coatings on carbon steel, stainless steel, and brass

Energy Technology Data Exchange (ETDEWEB)

Hadinata, Samuel-Sudibyo; Lee, Ming-Tsung [Department of Materials Science and Engineering, National Cheng Kung University, 1, Ta-Hsueh Road, Tainan 701, Taiwan (China); Pan, Szu-Jung [Ocean Energy Research Center, Tainan Hydraulics Laboratory, National Cheng Kung University, 1, Ta-Hsueh Road, Tainan 701, Taiwan (China); Tsai, Wen-Ta, E-mail: wttsai@mail.ncku.edu.tw [Department of Materials Science and Engineering, National Cheng Kung University, 1, Ta-Hsueh Road, Tainan 701, Taiwan (China); Ocean Energy Research Center, Tainan Hydraulics Laboratory, National Cheng Kung University, 1, Ta-Hsueh Road, Tainan 701, Taiwan (China); Tai, Chen-Yi [Ocean Energy Research Center, Tainan Hydraulics Laboratory, National Cheng Kung University, 1, Ta-Hsueh Road, Tainan 701, Taiwan (China); Shih, Chuan-Feng [Ocean Energy Research Center, Tainan Hydraulics Laboratory, National Cheng Kung University, 1, Ta-Hsueh Road, Tainan 701, Taiwan (China); Department of Electrical Engineering, National Cheng Kung University, 1, Ta-Hsueh Road, Tainan 701, Taiwan (China)

2013-02-01

Diamond-like carbon (DLC) coatings have been deposited onto stainless steel, carbon steel and brass by plasma-enhanced chemical vapor deposition, respectively. Atomic arrangement, chemical structure, surface morphology and cross-section microstructure of the DLC coatings were examined by X-ray diffraction, Raman scattering spectroscopy and scanning electron microscopy. The electrochemical behaviors of the DLC coatings in 3.5 wt.% NaCl solution were investigated by performing an open circuit potential (OCP) measurement and a potentiodynamic polarization test. The experimental results showed that properly deposited DLC coatings could cause an increase of OCP by hundreds of millivolts and a reduction of anodic current density by several orders of magnitude as compared to that of the substrate. The results also demonstrated that electrochemical techniques could be used as tools to detect the soundness of the DLC coating by examining OCP and polarization curve, which varied with the form of defect and depended on the type of substrate. - Highlights: ► The substrate could affect the quality of diamond-like carbon (DLC) coating. ► Defect-free DLC coating exhibited extremely low anodic current density. ► The quality of DLC coating on metal could be evaluated by electrochemical test.

Synthesis, characterization and electrochemical performance of core/shell structured carbon coated silicon powders for lithium ion battery negative electrodes

Directory of Open Access Journals (Sweden)

Tuğrul Çetinkaya

2017-06-01

Full Text Available Surface of nano silicon powders were coated with amorphous carbon by pyrolysis of polyacronitrile (PAN polymer. Microstructural characterization of amorphous carbon coated silicon powders (Si-C were carried out using scanning electron microscopy (SEM and thickness of carbon coating is defined by transmission electron microscopy (TEM. Elemental analyses of Si-C powders were performed using energy dispersive X-ray spectroscopy (EDS. Structural and phase characterization of Si-C composite powders were investigated using X-ray diffractometer (XRD and Raman spectroscopy. Produced Si-C powders were prepared as an electrode on the copper current collector and electrochemical tests were carried out using CR2016 button cells at 200 mA/g constant current density. According to electrochemical test results, carbon coating process enhanced the electrochemical performance by reducing the problems stem from volume change and showed 770 mAh/g discharge capacity after 30 cycles.

Enhanced electrochemical performance of porous activated carbon by forming composite with graphene as high-performance supercapacitor electrode material

Energy Technology Data Exchange (ETDEWEB)

Wang, Zhi-Hang; Yang, Jia-Ying [Central South University, College of Chemistry and Chemical Engineering, Hunan Provincial Key Laboratory of Efficient and Clean Utilization of Manganese Resources (China); Wu, Xiong-Wei [Hunan Agricultural University, College of Science (China); Chen, Xiao-Qing; Yu, Jin-Gang, E-mail: yujg@csu.edu.cn [Central South University, College of Chemistry and Chemical Engineering, Hunan Provincial Key Laboratory of Efficient and Clean Utilization of Manganese Resources (China); Wu, Yu-Ping, E-mail: wuyp@fudan.edu.cn [Fudan University, New Energy and Materials Laboratory (NEML), Department of Chemistry and Shanghai Key Laboratory of Molecular Catalysis and Innovative Materials (China)

2017-02-15

In this work, a novel activated carbon containing graphene composite was developed using a fast, simple, and green ultrasonic-assisted method. Graphene is more likely a framework which provides support for activated carbon (AC) particles to form hierarchical microstructure of carbon composite. Scanning electron microscope (SEM), transmission electron microscope (TEM), Brunauer–Emmett–Teller (BET) surface area measurement, thermogravimetric analysis (TGA), Raman spectra analysis, XRD, and XPS were used to analyze the morphology and surface structure of the composite. The electrochemical properties of the supercapacitor electrode based on the as-prepared carbon composite were investigated by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), charge/discharge, and cycling performance measurements. It exhibited better electrochemical performance including higher specific capacitance (284 F g{sup −1} at a current density of 0.5 A g{sup −1}), better rate behavior (70.7% retention), and more stable cycling performance (no capacitance fading even after 2000 cycles). It is easier for us to find that the composite produced by our method was superior to pristine AC in terms of electrochemical performance due to the unique conductive network between graphene and AC.

Facile synthesis of Co3O4 nanowires grown on hollow NiO microspheres with superior electrochemical performance

International Nuclear Information System (INIS)

Fan, Meiqing; Ren, Bo; Yu, Lei; Song, Dalei; Liu, Qi; Liu, Jingyuan; Wang, Jun; Jing, Xiaoyan; Liu, Lianhe

2015-01-01

Graphical abstract: Display Omitted - Highlights: • The NiO hollow spheres were decorated by Co 3 O 4 nanowires. • The NiO hollow spheres were comprised of many NiO particles. • The Co 3 O 4 nanowires were composed of nanoparticles. • The NiO/Co 3 O 4 core/shell nanocomposites have good electrochemical properties. - Abstract: The NiO/Co 3 O 4 core/shell composites as a promising supercapacitor material have been fabricated by facile hydrothermal process. The structure and morphology of the NiO/Co 3 O 4 core/shell composites were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results indicated that the NiO hollow spheres were decorated by Co 3 O 4 nanowires, and the nanowires were composed of nanoparticles. Electrochemical properties were characterized by cyclic voltammetry, galvanostatic charge/discharge measurements, and electrochemical impedance spectroscopy. The results suggested that the NiO/Co 3 O 4 core/shell composites had good electrochemical reversibility and displayed superior capacitive performance with large capacitance (510 F g −1 ). Moreover, NiO/Co 3 O 4 core/shell composites showed excellent cyclic performanceafter 1000 cycles

Silver-coated LiVPO4F composite with improved electrochemical performance as cathode material for lithium-ion batteries

Science.gov (United States)

Yang, Bo; Yang, Lin

2015-12-01

Nano-structured LiVPO4F/Ag composite cathode material has been successfully synthesized via a sol-gel route. The structural and physical properties, as well as the electrochemical performance of the material are compared with those of the pristine LiVPO4F. X-ray diffraction (XRD) and scanning electron microscopy (SEM) reveal that Ag particles are uniformly dispersed on the surface of LiVPO4F without destroying the crystal structure of the bulk material. An analysis of the electrochemical measurements show that the Ag-modified LiVPO4F material exhibits high discharge capacity, good cycle performance (108.5 mAh g-1 after 50th cycles at 0.1 C, 93% of initial discharge capacity) and excellent rate behavior (81.8 mAh g-1 for initial discharge capacity at 5 C). The electrochemical impedance spectroscopy (EIS) results reveal that the adding of Ag decreases the charge-transfer resistance (Rct) of LiVPO4F cathode. This study demonstrates that Ag-coating is a promising way to improve the electrochemical performance of the pristine LiVPO4F for lithium-ion batteries cathode material.

Enhanced electrochemical performance of porous activated carbon by forming composite with graphene as high-performance supercapacitor electrode material

International Nuclear Information System (INIS)

Wang, Zhi-Hang; Yang, Jia-Ying; Wu, Xiong-Wei; Chen, Xiao-Qing; Yu, Jin-Gang; Wu, Yu-Ping

2017-01-01

In this work, a novel activated carbon containing graphene composite was developed using a fast, simple, and green ultrasonic-assisted method. Graphene is more likely a framework which provides support for activated carbon (AC) particles to form hierarchical microstructure of carbon composite. Scanning electron microscope (SEM), transmission electron microscope (TEM), Brunauer–Emmett–Teller (BET) surface area measurement, thermogravimetric analysis (TGA), Raman spectra analysis, XRD, and XPS were used to analyze the morphology and surface structure of the composite. The electrochemical properties of the supercapacitor electrode based on the as-prepared carbon composite were investigated by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), charge/discharge, and cycling performance measurements. It exhibited better electrochemical performance including higher specific capacitance (284 F g"−"1 at a current density of 0.5 A g"−"1), better rate behavior (70.7% retention), and more stable cycling performance (no capacitance fading even after 2000 cycles). It is easier for us to find that the composite produced by our method was superior to pristine AC in terms of electrochemical performance due to the unique conductive network between graphene and AC.

Electrochemical behaviour and nanoscale characteristics of CNT-based fibers as new substrate for cell growth

Energy Technology Data Exchange (ETDEWEB)

Polizu, S.; Yahia, L.H. [Ecole Polytechnique de Montreal, PQ (Canada). Laboratoire d' innovation et d' analyse de la bioperformance; Savadogo, O. [Ecole Polytechnique de Montreal, Montreal, PQ (Canada). Laboratoire de nouveaux materiaux pour l' energie et l' electrochimie; Maugey, M.; Poulin, P. [Centre de Recherche Paul Pascal, CNRS, Bordeaux (France); Rouabhia, M. [Laval Univ., Quebec City, PQ (Canada). Faculty of Medicine

2008-07-01

This paper reported on a study in which carbon nanotube (CNT) macroscopic fibers were formulated by a newly developed non-covalent method for fabricating fibrous substrate. The covalent and noncovalent chemistry of CNTs has been widely used in the development of CNT-based biomaterials as active substrates for living cells. Time of Flight Mass Spectroscopy (TOF-SIMS) analysis was used to determine the surface characteristics of the CNT-based fibers produced by wet spinning method. The structure and texture of fibers were imaged using Low-Vacuum Scanning Electron Microscopy (LV-SEM) equipped with an Energy Dispersive Spectrometer (EDS) for microanalysis. Atomic Force Microscopy (AFM) imaging revealed the structure of fibers. Cyclic Voltametry (CV) measurements were performed to examine the electrochemical behaviour of fibers. Sulfuric acid and a cell culture medium was used as the 2 different electrolytes. The influences of environmental parameters on the electrochemical phenomena taking place were identified. The intrinsic electrochemical characteristics of fibers were revealed through measurements in acid environment. The cell culture medium simulated the physiological conditions. It was concluded that the newly developed wet spinning method is very efficient for making CNT-based fibers as electroactive biomaterials. The structural nanoscale details evidenced a good alignment of nanotubes in the thread and the critical role it plays in electrochemical interactions. The differences induced by the variation of electrolytes suggest that a relationship could be established between the fiber chemistry and the electrochemical response. This correlation has considerably potential for the design of new biomedical devices. 2 refs.

Electrochemical corrosion study of Mg–Al–Zn–Mn alloy in aqueous ethylene glycol containing chloride ions

Directory of Open Access Journals (Sweden)

Harish Medhashree

2017-01-01

Full Text Available Nowadays most of the automobiles use magnesium alloys in the components of the engine coolant systems. These engine coolants used are mainly composed of aqueous ethylene glycol along with some inhibitors. Generally the engine coolants are contaminated by environmental anions like chlorides, which would enhance the rate of corrosion of the alloys used in the coolant system. In the present study, the corrosion behavior of Mg–Al–Zn–Mn alloy in 30% (v/v aqueous ethylene glycol containing chloride anions at neutral pH was investigated. Electrochemical techniques, such as potentiodynamic polarization method, cyclic polarization and electrochemical impedance spectroscopy (EIS were used to study the corrosion behavior of Mg–Al–Zn–Mn alloy. The surface morphology, microstructure and surface composition of the alloy were studied by using the scanning electron microscopy (SEM, optical microscopy and energy dispersion X-ray (EDX analysis, respectively. Electrochemical investigations show that the rate of corrosion increases with the increase in chloride ion concentration and also with the increase in medium temperature.

Preparation and electrochemical characterization of polyaniline/activated carbon composites as an electrode material for supercapacitors.

Science.gov (United States)

Oh, Misoon; Kim, Seok

2012-01-01

Polyaniline (PANI)/activated carbon (AC) composites were prepared by a chemical oxidation polymerization. To find an optimum ratio between PANI and AC which shows superior electrochemical properties, the preparation was carried out in changing the amount of added aniline monomers. The morphology of prepared composites was investigated by scanning electron microscopy (SEM) and transmission electron microscope (TEM). The structural and thermal properties were investigated by Fourier transform infrared spectra (FT-IR) and thermal gravimetric analysis (TGA), respectively. The electrochemical properties were characterized by cyclic voltammetry (CV). Composites showed a summation of capacitances that consisted of two origins. One is double-layer capacitance by ACs and the other is faradic capacitance by redox reaction of PANI. Fiber-like PANIs are coated on the surface of ACs and they contribute to the large surface for redox reaction. The vacancy among fibers provided the better diffusion and accessibility of ion. High capacitances of composites were originated from the network structure having vacancy made by PANI fibers. It was found that the composite prepared with 5 ml of aniline monomer and 0.25 g of AC showed the highest capacitance. Capacitance of 771 F/g was obtained at a scan rate of 5 mV/s.

Electrochemical Sensors for Clinic Analysis

Directory of Open Access Journals (Sweden)

Guang Li

2008-03-01

Full Text Available Demanded by modern medical diagnosis, advances in microfabrication technology have led to the development of fast, sensitive and selective electrochemical sensors for clinic analysis. This review addresses the principles behind electrochemical sensor design and fabrication, and introduces recent progress in the application of electrochemical sensors to analysis of clinical chemicals such as blood gases, electrolytes, metabolites, DNA and antibodies, including basic and applied research. Miniaturized commercial electrochemical biosensors will form the basis of inexpensive and easy to use devices for acquiring chemical information to bring sophisticated analytical capabilities to the non-specialist and general public alike in the future.

Electrochemical biosensors for hormone analyses.

Science.gov (United States)

Bahadır, Elif Burcu; Sezgintürk, Mustafa Kemal

2015-06-15

Electrochemical biosensors have a unique place in determination of hormones due to simplicity, sensitivity, portability and ease of operation. Unlike chromatographic techniques, electrochemical techniques used do not require pre-treatment. Electrochemical biosensors are based on amperometric, potentiometric, impedimetric, and conductometric principle. Amperometric technique is a commonly used one. Although electrochemical biosensors offer a great selectivity and sensitivity for early clinical analysis, the poor reproducible results, difficult regeneration steps remain primary challenges to the commercialization of these biosensors. This review summarizes electrochemical (amperometric, potentiometric, impedimetric and conductometric) biosensors for hormone detection for the first time in the literature. After a brief description of the hormones, the immobilization steps and analytical performance of these biosensors are summarized. Linear ranges, LODs, reproducibilities, regenerations of developed biosensors are compared. Future outlooks in this area are also discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

Growth, characterization and electrochemical properties of hierarchical CuO nanostructures for supercapacitor applications

Energy Technology Data Exchange (ETDEWEB)

Krishnamoorthy, Karthikeyan [Nanomaterials and System Laboratory, Department of Mechanical Engineering, Jeju National University, Jeju 690 756 (Korea, Republic of); Kim, Sang-Jae, E-mail: kimsangj@jejunu.ac.kr [Nanomaterials and System Laboratory, Department of Mechanical Engineering, Jeju National University, Jeju 690 756 (Korea, Republic of); Department of Mechatronics Engineering, Jeju National University, Jeju 690 756 (Korea, Republic of)

2013-09-01

Graphical abstract: - Highlights: • Hierarchical CuO nanostructures were grown on Cu foil. • Monoclinic phase of CuO was grown. • XPS analysis revealed the presence of Cu(2p{sub 3/2}) and Cu(2p{sub 1/2}) on the surfaces. • Specific capacitance of 94 F/g was achieved for the CuO using cyclic voltammetry. • Impedance spectra show their pseudo capacitor applications. - Abstract: In this paper, we have investigated the electrochemical properties of hierarchical CuO nanostructures for pseudo-supercapacitor device applications. Moreover, the CuO nanostructures were formed on Cu substrate by in situ crystallization process. The as-grown CuO nanostructures were characterized using X-ray diffraction (XRD), Fourier transform-infra red spectroscopy (FT-IR), X-ray photoelectron spectroscopy and field emission-scanning electron microscope (FE-SEM) analysis. The XRD and FT-IR analysis confirm the formation of monoclinic CuO nanostructures. FE-SEM analysis shows the formation of leave like hierarchical structures of CuO with high uniformity and controlled density. The electrochemical analysis such as cyclic voltammetry and electrochemical impedance spectroscopy studies confirms the pseudo-capacitive behavior of the CuO nanostructures. Our experimental results suggest that CuO nanostructures will create promising applications of CuO toward pseudo-supercapacitors.

Growth, characterization and electrochemical properties of hierarchical CuO nanostructures for supercapacitor applications

International Nuclear Information System (INIS)

Krishnamoorthy, Karthikeyan; Kim, Sang-Jae

2013-01-01

Graphical abstract: - Highlights: • Hierarchical CuO nanostructures were grown on Cu foil. • Monoclinic phase of CuO was grown. • XPS analysis revealed the presence of Cu(2p 3/2 ) and Cu(2p 1/2 ) on the surfaces. • Specific capacitance of 94 F/g was achieved for the CuO using cyclic voltammetry. • Impedance spectra show their pseudo capacitor applications. - Abstract: In this paper, we have investigated the electrochemical properties of hierarchical CuO nanostructures for pseudo-supercapacitor device applications. Moreover, the CuO nanostructures were formed on Cu substrate by in situ crystallization process. The as-grown CuO nanostructures were characterized using X-ray diffraction (XRD), Fourier transform-infra red spectroscopy (FT-IR), X-ray photoelectron spectroscopy and field emission-scanning electron microscope (FE-SEM) analysis. The XRD and FT-IR analysis confirm the formation of monoclinic CuO nanostructures. FE-SEM analysis shows the formation of leave like hierarchical structures of CuO with high uniformity and controlled density. The electrochemical analysis such as cyclic voltammetry and electrochemical impedance spectroscopy studies confirms the pseudo-capacitive behavior of the CuO nanostructures. Our experimental results suggest that CuO nanostructures will create promising applications of CuO toward pseudo-supercapacitors

Electrodeposition synthesis and electrochemical properties of nanostructured {gamma}-MnO{sub 2} films

Energy Technology Data Exchange (ETDEWEB)

Chou, Shulei; Cheng, Fangyi; Chen, Jun [Institute of New Energy Material Chemistry, Nankai University, Tianjin 300071 (China)

2006-11-08

The thin films of carambola-like {gamma}-MnO{sub 2} nanoflakes with about 20nm in thickness and at least 200nm in width were prepared on nickel sheets by combination of potentiostatic and cyclic voltammetric electrodeposition techniques. The as-prepared MnO{sub 2} nanomaterials, which were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS), were used as the active material of the positive electrode for primary alkaline Zn/MnO{sub 2} batteries and electrochemical supercapacitors. Electrochemical measurements showed that the MnO{sub 2} nanoflake films displayed high potential plateau (around 1.0V versus Zn) in primary Zn/MnO{sub 2} batteries at the discharge current density of 500mAg{sup -1} and high specific capacitance of 240Fg{sup -1} at the current density of 1mAcm{sup -2}. This indicated the potential application of carambola-like {gamma}-MnO{sub 2} nanoflakes in high-power batteries and electrochemical supercapacitors. The growth process for the one- and three-dimensional nanostructured MnO{sub 2} was discussed on the basis of potentiostatic and cyclic voltammetric techniques. The present synthesis method can be extended to the preparation of other nanostructured metal-oxide films. (author)

Probing the electrochemical behaviour of SWCNT-cobalt nanoparticles and their electrocatalytic activities towards the detection of nitrite at acidic and physiological pH conditions

CSIR Research Space (South Africa)

Adekunle, AS

2010-05-01

Full Text Available was confirmed by field emission scanning electron microscopy (FESEM), AFM and EDX techniques. The electron transfer behavior of the modified electrodes was investigated in [Fe (CN)6]3-/4- redox probe using cyclic voltammetry (CV) and electrochemical impedance...

Highly Selective Polypyrrole MIP-Based Gravimetric and Electrochemical Sensors for Picomolar Detection of Glyphosate

Directory of Open Access Journals (Sweden)

Zouhour Mazouz

2017-11-01

Full Text Available There is a global debate and concern about the use of glyphosate (Gly as an herbicide. New toxicological studies will determine its use in the future under new strict conditions or its replacement by alternative synthetic or natural herbicides. In this context, we designed biomimetic polymer sensing layers for the selective molecular recognition of Gly. Towards this end, complementary surface acoustic wave (SAW and electrochemical sensors were functionalized with polypyrrole (PPy-imprinted polymer for the selective detection of Gly. Their corresponding limits of detection were on the order of 1 pM, which are among the lowest values ever reported in literature. The relevant dissociation constants between PPy and Gly were estimated at [Kd1 = (0.7 ± 0.3 pM and Kd2 = (1.6 ± 1.4 µM] and [Kd1 = (2.4 ± 0.9 pM and Kd2 = (0.3 ± 0.1 µM] for electrochemical and gravimetric measurements, respectively. Quantum chemical calculations permitted to estimate the interaction energy between Gly and PPy film: ΔE = −145 kJ/mol. Selectivity and competitivity tests were investigated with the most common pesticides. This work conclusively shows that gravimetric and electrochemical results indicate that both MIP-based sensors are perfectly able to detect and distinguish glyphosate without any ambiguity.

Preparation and characterization of a new carbonaceous material for electrochemical systems

Directory of Open Access Journals (Sweden)

ZI JI LIN

2010-02-01

Full Text Available A new carbonaceous material was successfully prepared by the py-rolysis of scrap tire rubber at 600 °C under a nitrogen atmosphere. The physical characteristics of the prepared carbonaceous material were studied by scanning electron microscopy (SEM, X-ray powder diffraction (XRD and X-ray photoelectron spectroscopy (XPS. It was proved that the carbonaceous material had a disordered structure and spherical morphology with an average particle size about 100 nm. The prepared carbonaceous material was also used as electrodes in electrochemical systems to examine its electrochemical performances. It was demonstrated that it delivered a lithium insertion capacity of 658 mA h g-1 during the first cycle with a coulombic efficiency of 68 %. Cyclic voltammograms test results showed that a redox reaction occurred during the cycles. The chemical diffusion coefficient based on the impedance diagram was about 10-10 cm2 s-1. The pyrolytic carbonaceous material derived from scrap tire rubber is therefore considered to be a potential anode material in lithium secondary batteries or capacitors. Furthermore, it is advantageous for environmental protection.

Pencil It in: Exploring the Feasibility of Hand-Drawn Pencil Electrochemical Sensors and Their Direct Comparison to Screen-Printed Electrodes

Directory of Open Access Journals (Sweden)

Elena Bernalte

2016-08-01

Full Text Available We explore the fabrication, physicochemical characterisation (SEM, Raman, EDX and XPS and electrochemical application of hand-drawn pencil electrodes (PDEs upon an ultra-flexible polyester substrate; investigating the number of draws (used for their fabrication, the pencil grade utilised (HB to 9B and the electrochemical properties of an array of batches (i.e, pencil boxes. Electrochemical characterisation of the PDEs, using different batches of HB grade pencils, is undertaken using several inner- and outer-sphere redox probes and is critically compared to screen-printed electrodes (SPEs. Proof-of-concept is demonstrated for the electrochemical sensing of dopamine and acetaminophen using PDEs, which are found to exhibit competitive limits of detection (3σ upon comparison to SPEs. Nonetheless, it is important to note that a clear lack of reproducibility was demonstrated when utilising these PDEs fabricated using the HB pencils from different batches. We also explore the suitability and feasibility of a pencil-drawn reference electrode compared to screen-printed alternatives, to see if one can draw the entire sensing platform. This article reports a critical assessment of these PDEs against that of its screen-printed competitors, questioning the overall feasibility of PDEs’ implementation as a sensing platform.

Note: Automated electrochemical etching and polishing of silver scanning tunneling microscope tips.

Science.gov (United States)

Sasaki, Stephen S; Perdue, Shawn M; Rodriguez Perez, Alejandro; Tallarida, Nicholas; Majors, Julia H; Apkarian, V Ara; Lee, Joonhee

2013-09-01

Fabrication of sharp and smooth Ag tips is crucial in optical scanning probe microscope experiments. To ensure reproducible tip profiles, the polishing process is fully automated using a closed-loop laminar flow system to deliver the electrolytic solution to moving electrodes mounted on a motorized translational stage. The repetitive translational motion is controlled precisely on the μm scale with a stepper motor and screw-thread mechanism. The automated setup allows reproducible control over the tip profile and improves smoothness and sharpness of tips (radius 27 ± 18 nm), as measured by ultrafast field emission.

Soft landing of bare PtRu nanoparticles for electrochemical reduction of oxygen.

Science.gov (United States)

Johnson, Grant E; Colby, Robert; Engelhard, Mark; Moon, Daewon; Laskin, Julia

2015-08-07

Magnetron sputtering of two independent Pt and Ru targets coupled with inert gas aggregation in a modified commercial source has been combined with soft landing of mass-selected ions to prepare bare 4.5 nm diameter PtRu nanoparticles on glassy carbon electrodes with controlled size and morphology for electrochemical reduction of oxygen in solution. Employing atomic force microscopy (AFM) it is shown that the nanoparticles bind randomly to the glassy carbon electrode at a relatively low coverage of 7 × 10(4) ions μm(-2) and that their average height is centered at 4.5 nm. Scanning transmission electron microscopy images obtained in the high-angle annular dark field mode (HAADF-STEM) further confirm that the soft-landed PtRu nanoparticles are uniform in size. Wide-area scans of the electrodes using X-ray photoelectron spectroscopy (XPS) reveal the presence of both Pt and Ru in atomic concentrations of ∼9% and ∼33%, respectively. Deconvolution of the high energy resolution XPS spectra in the Pt 4f and Ru 3d regions indicates the presence of both oxidized Pt and Ru. The substantially higher loading of Ru compared to Pt and enrichment of Pt at the surface of the nanoparticles is confirmed by wide-area analysis of the electrodes using time-of-flight medium energy ion scattering (TOF-MEIS) employing both 80 keV He(+) and O(+) ions. The activity of electrodes containing 7 × 10(4) ions μm(-2) of bare 4.5 nm PtRu nanoparticles toward the electrochemical reduction of oxygen was evaluated employing cyclic voltammetry (CV) in 0.1 M HClO4 and 0.5 M H2SO4 solutions. In both electrolytes a pronounced reduction peak was observed during O2 purging of the solution that was not evident during purging with Ar. Repeated electrochemical cycling of the electrodes revealed little evolution in the shape or position of the voltammograms indicating high stability of the nanoparticles supported on glassy carbon. The reproducibility of the nanoparticle synthesis and deposition was

Effect of Amine Adlayer on Electrochemical Uric Acid Sensor Conducted on Electrochemically Reduced Graphene Oxide

Energy Technology Data Exchange (ETDEWEB)

Park, Sumi; Kim, Kyuwon [Incheon National University, Incheon (Korea, Republic of)

2016-03-15

The electrochemical biosensing efficiency of uric acid (UA) detection on an electrochemically reduced graphene oxide (ERGO)-decorated electrode surface was studied by using various amine linkers used to immobilize ERGO. The amine linkers aminoethylphenyldiazonium , 2,2'-(ethylenedioxy)bis(ethylamine), 3-aminopro-pyltriethoxysilane, and polyethyleneimine were coated on indium-tin-oxide electrode surfaces through chemical or electrochemical deposition methods. ERGO-decorated surfaces were prepared by the electrochemical reduction of graphene oxide (GO), which was immobilized on the amine-coated electrode surfaces through the electrostatic interaction between GO and the ammonium ion of the linker on the surface. We monitored the sensing results of electrochemical UA detection with differential pulse voltammetry. The ERGO-modified surface presented electrocatalytic oxidation of UA and ascorbic acid. Among the different amines tested, 3-aminopropyltriethoxysilane provided the best biosensing performance in terms of sensitivity and reproducibility.

Effect of Amine Adlayer on Electrochemical Uric Acid Sensor Conducted on Electrochemically Reduced Graphene Oxide

International Nuclear Information System (INIS)

Park, Sumi; Kim, Kyuwon

2016-01-01

The electrochemical biosensing efficiency of uric acid (UA) detection on an electrochemically reduced graphene oxide (ERGO)-decorated electrode surface was studied by using various amine linkers used to immobilize ERGO. The amine linkers aminoethylphenyldiazonium , 2,2'-(ethylenedioxy)bis(ethylamine), 3-aminopro-pyltriethoxysilane, and polyethyleneimine were coated on indium-tin-oxide electrode surfaces through chemical or electrochemical deposition methods. ERGO-decorated surfaces were prepared by the electrochemical reduction of graphene oxide (GO), which was immobilized on the amine-coated electrode surfaces through the electrostatic interaction between GO and the ammonium ion of the linker on the surface. We monitored the sensing results of electrochemical UA detection with differential pulse voltammetry. The ERGO-modified surface presented electrocatalytic oxidation of UA and ascorbic acid. Among the different amines tested, 3-aminopropyltriethoxysilane provided the best biosensing performance in terms of sensitivity and reproducibility.

One-step electrochemical deposition of a graphene-ZrO₂ nanocomposite: Preparation, characterization and application for detection of organophosphorus agents

Energy Technology Data Exchange (ETDEWEB)

Du, Dan; Liu, Juan; Zhang, Xiao-Yan; Cui, Xiao-Li; Lin, Yuehe

2011-04-27

This paper described the preparation, characterization, and electrochemical properties of a graphene-ZrO₂ nanocomposite (GZN) and its application for both the enrichment and detection of methyl parathion (MP). GZN was fabricated using electrochemical deposition and characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), which showed the successful formation of nanocomposites. Due to the strong affinity to the phosphoric group and the fast electron-transfer kinetics of GZN, both the extraction and electrochemical detection of organophosphorus (OP) agents at the same GZN modified electrochemical sensor was possible. The combination of solid-phase extraction and stripping voltammetric analysis allowed fast, sensitive, and selective determination of MP in garlic samples. The stripping response was highly linear over the MP concentrations ranging from 0.5 ng mL^-1 to 100 ng mL^-1, with a detection limit of 0.1 ng mL^-1. This new nanocomposite-based electrochemical sensor provides an opportunity to develop a field-deployable, sensitive, and quantitative method for monitoring exposure to OPs.

Activated carbon and single-walled carbon nanotube based electrochemical capacitor in 1 M LiPF6 electrolyte

International Nuclear Information System (INIS)

Azam, M.A.; Jantan, N.H.; Dorah, N.; Seman, R.N.A.R.; Manaf, N.S.A.; Kudin, T.I.T.; Yahya, M.Z.A.

2015-01-01

Highlights: • Activated carbon and single-walled CNT based electrochemical capacitor. • Electrochemical analysis by means of CV, charge/discharge and impedance. • 1 M LiPF 6 non-aqueous solution as an electrolyte. • AC/SWCNT electrode exhibits a maximum capacitance of 60.97 F g −1 . - Abstract: Carbon nanotubes have been extensively studied because of their wide range of potential application such as in nanoscale electric circuits, textiles, transportation, health, and the environment. Carbon nanotubes feature extraordinary properties, such as electrical conductivities higher than those of copper, hardness and thermal conductivity higher than those of diamond, and strength surpassing that of steel, among others. This research focuses on the fabrication of an energy storage device, namely, an electrochemical capacitor, by using carbon materials, i.e., activated carbon and single-walled carbon nanotubes, of a specific weight ratio as electrode materials. The electrolyte functioning as an ion carrier is 1 M lithium hexafluorophosphate. Variations in the electrochemical performance of the device, including its capacitance, charge/discharge characteristics, and impedance, are reported in this paper. The electrode proposed in this work exhibits a maximum capacitance of 60.97 F g −1 at a scan rate of 1 mV s −1

A disposable electrochemical immunosensor based on carbon screen-printed electrodes for the detection of prostate specific antigen.

Science.gov (United States)

Yan, Mei; Zang, Dejin; Ge, Shenguang; Ge, Lei; Yu, Jinghua

2012-01-01

A novel screen-printed electrode (SPEs) on sheets of vegetable parchment was prepared. The obtained SPEs were stable, convenient, inexpensive and suitable for large-area screen-printing. With these SPEs, we explored the fabrication of a novel, disposable and highly sensitive electro-analytical immunosensor using graphene nanosheets (GS) and horseradish peroxidase (HRP)-labeled signal antibody functionalized with gold nanoparticles (HRP-Ab(2)/Au NPs). GS was used to increase the conductivity and stability of this immunosensor due to its fast electron transportation and good biocompatibility. Au NPs could not only provide a large surface area for the immobilization of HRP-Ab(2) but also enhance the electroreduction between HRP and H(2)O(2) to amplify the electrochemical signal on the sandwich immuno-complexes modified SPEs. The proposed SPEs were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electrochemical methods involving cyclic voltammetry (CV), and electrochemical impedence method. Using prostate specific antigen (PSA) as a model analyte, this immunosensor showed a wide linear range over 6 orders of magnitude with the minimum value down to 2 pg mL(-1). In addition, this immunosensor could avoid the need of deoxygenation for the electrochemical immunoassay. Thus, it provided a promising potential in clinical applications. Copyright © 2012 Elsevier B.V. All rights reserved.

A high-performance flexible fibre-shaped electrochemical capacitor based on electrochemically reduced graphene oxide.

Science.gov (United States)

Li, Yingru; Sheng, Kaixuan; Yuan, Wenjing; Shi, Gaoquan

2013-01-11

A fibre-shaped solid electrochemical capacitor based on electrochemically reduced graphene oxide has been fabricated, exhibiting high specific capacitance and rate capability, long cycling life and attractive flexibility.

A Miniaturized Impedimetric Immunosensor for the Competitive Detection of Adrenocorticotropic Hormone

Directory of Open Access Journals (Sweden)

Nan Li

2017-12-01

Full Text Available Adrenocorticotropic hormone (ACTH plays an essential role in regulating corticosteroid hormone production, which has important functions in a myriad of critical physiological functions. In this proof-of-concept study, a miniaturized immunosensor was developed for the highly sensitive detection of ACTH using electrochemical impedance spectroscopy (EIS in connection with disposable screen-printed gold electrodes (SPGEs. A film of 3,3′-dithiobis[sulfosuccinimidylpropionate] (DTSSP was prepared to immobilize anti-ACTH antibodies covalently on the nanostructured SPGE surface. The surface-immobilized anti-ACTH antibodies captured the biotinylated ACTH (biotin-ACTH and non-labelled ACTH for the competitive immunoassay. After coupling of a streptavidin-alkaline phosphatase conjugate (Streptavidin-ALP, the bio-catalysed precipitation of an insoluble and insulating product onto the sensing interface changed the charge transfer resistance (Rct characteristics significantly. The detection limit of 100 fg/mL was determined for ACTH in a 5 μL sample volume, which indicated that this versatile platform can be easily adapted for miniaturized electrochemical immunosensing of cancer marker biomolecules. High selectivity and sensitivity of our immunoassay to detect ACTH in real samples demonstrated its promising potential for future development and applications using clinical samples.

Flexible all-solid-state high-performance supercapacitor based on electrochemically synthesized carbon quantum dots/polypyrrole composite electrode

International Nuclear Information System (INIS)

Jian, Xuan; Yang, Hui-min; Li, Jia-gang; Zhang, Er-hui; Cao, Le-le; Liang, Zhen-hai

2017-01-01

Highlights: • Porous nanostructure carbon quantum dots/polypyrrole composite film was successfully synthesized by direct electrochemical method. • A flexible all-solid-state supercapacitor device was fabricated using the carbon quantum dots/polypyrrole composite electrode. • The flexible supercapacitor exhibits high specific capacitance, excellent reliability and long cycling life. - Abstract: Recently, carbon quantum dots (CQDs) as a new zero-dimensional carbon nanomaterial have become a focus in electrochemical energy storage. In this paper, flexible all-solid-state supercapacitors (ASSSs) were electrochemically synthesized by on-step co-deposition of appropriate amounts of pyrrole monomer and CQDs in aqueous solution. The different electrodeposition time plays an important role in controlling morphologies of stainless steel wire meshes (SSWM)-supported CQDs/PPy composite film. The morphologies and compositions of the obtained CQDs/PPy composite electrodes were characterized by scanning electron microscope (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), Raman spectrum and X-ray photoelectron spectroscopy (XPS). Furthermore, a novel flexible ASSS device was fabricated using CQDs/PPy composite as the electrode and separated by polyvinyl alcohol/LiCl gel electrolyte. Benefiting from superior electrochemical properties of CQDs and PPy, the as-prepared CQDs/PPy composite ASSSs exhibit outstanding electrochemical performance with the areal capacitance 315 mF cm −2 (corresponding to specific capacitance of 308 F g −1 ) at a current density of 0.2 mA cm −2 and long cycle life with 85.7% capacitance retention after 2 000 cycles.

Influence of Fenton's reagent treatment on electrochemical properties of graphite felt for all vanadium redox flow battery

International Nuclear Information System (INIS)

Gao, Chao; Wang, NanFang; Peng, Sui; Liu, SuQin; Lei, Ying; Liang, XinXing; Zeng, ShanShan; Zi, HuiFang

2013-01-01

Highlights: ► Highly hydroxyl-functionalized graphite felt has been obtained through Fenton's reagent treatment. ► Fenton's reagent treatment involves only one step, works under ambient conditions and will never produce any toxic gas. ► The treated graphite felt exhibits superior electrochemical performance in comparison to the untreated one. -- Abstract: An environmental, economic and highly effective method for carbon fiber hydroxylated-functionalization based on Fenton's reagent treatment is used to improve the electrochemical activity of graphite felt (GF) as the positive electrode in all vanadium redox flow battery (VRFB). The effect of H 2 O 2 content in Fenton's reagent on the structure and electrochemical properties of GF is investigated. The scanning electron microscope (SEM) indicates that the surface of the treated GF is etched increasingly with the content of H 2 O 2 . The Fourier transformation infrared (FTIR) spectroscopy shows that the peak intensity of hydroxyl groups on the treated felt is increased with the H 2 O 2 concentration, which is further verified by X-ray photoelectron spectroscopy (XPS). Cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) show that the treated sample exhibits a higher electrochemical activity. A VRFB with the treated GF as electrodes exhibits higher coulombic, voltage and energy efficiency (98.8%, 75.1% and 74.2%) than that with the untreated GF (93.9%, 72.1% and 67.7%) at 60 mA cm −2 , and this method is even superior when compared with the reported methods

Photoinducedly electrochemical preparation of Prussian blue film and electrochemical modification of the film with cetyltrimethylammonium cation

Energy Technology Data Exchange (ETDEWEB)

Liu Shouqing, E-mail: shouqing_liu@hotmail.co [Key Laboratory of Environmental Functional Materials of Jiangsu Province, College of Chemistry and Bioengineering, Suzhou University of Science and Technology, Suzhou 215009 (China); Li Hua; Sun Weihui; Wang Xiaomei; Chen Zhigang [Key Laboratory of Environmental Functional Materials of Jiangsu Province, College of Chemistry and Bioengineering, Suzhou University of Science and Technology, Suzhou 215009 (China); Xu Jingjuan; Ju Huangxian; Chen Hongyuan [Key Laboratory of Analytical Chemistry for Life Science, Ministry of Education, Nanjing University, Nanjing 210093 (China)

2011-04-15

Research highlights: {yields} Cetyltrimethylammonium cations work as counter ions in Prussian blue film was observed and confirmed by cyclic voltammetry, Fourier transform infrared spectroscopy, X-ray powder diffraction measurements, scanning electronic microscopy and transmission electron microscope for the first time. {yields} Because the cetyltrimethylammonium cations in Prussian blue film are hydrophobic, the Prussian blue film is very stable even in alkali solution, which provides a technical basis for fabrication of stable biosensors. - Abstract: This work presents a photoinducedly electrochemical preparation of Prussian blue from a single sodium nitroprusside and insertion of cetyltrimethylammonium cations into Prussian blue as counter ions. The product of photoinducedly electrochemical reactions has a couple of voltammetric peaks at E{sup o} = 0.266 V in 0.2 mol l{sup -1} KCl solution, the measurements of X-ray powder diffraction and FT-IR spectroscopy show that it is Prussian blue (PB). The formation mechanism of a pre-photochemical reaction and subsequent electrochemical reaction is suggested. The cyclic voltammetric treatment of the freshly as-prepared PB film in 1.0 mmol l{sup -1} cetyltrimethylammonium (CTA) bromide solution leads to the insertion of cetyltrimethylammonium cations into the channels of Prussian blue, which substitutes for potassium ions as counter ions in Prussian blue. The Prussian blue containing CTA counter ions shows two couples of voltammetric peaks at E{sup o} = -0.106 V and E{sup o} = 0.249 V in 0.2 mol l{sup -1} KCl solution containing 1.0 mmol l{sup -1} cetyltrimethylammonium bromide. Compared with the electrochemical behaviors of KFeFe(CN){sub 6} in 0.1 mol l{sup -1} KOH alkali solution, CTAFeFe(CN){sub 6} shows relatively durable voltammetric currents due to the hydrophobic effects of cetyltrimethylammonium. The diffusion coefficients for CTA and potassium cations were estimated to be D{sub CTA} 1.25 x 10{sup -12} cm{sup 2} s

Electro-chemical deposition of zinc oxide nanostructures by using two electrodes

Directory of Open Access Journals (Sweden)

B. A. Taleatu

2011-09-01

Full Text Available One of the most viable ways to grow nanostructures is electro deposition. However, most electrodeposited samples are obtained by three-electrode electrochemical cell. We successfully use a much simpler two-electrode cell to grow different ZnO nanostructures from common chemical reagents. Concentration, pH of the electrolytes and growth parameters like potentials at the electrodes, are tailored to allow fast growth without complexity. Morphology and surface roughness are investigated by Scanning Electron and Air Force Microscopy (SEM and AFM respectively, crystal structure by X-Ray Diffraction measurements (XRD and ZnO stoichiometry by core level photoemission spectroscopy (XPS.

Nanoporous gold microelectrode prepared from potential modulated electrochemical alloying–dealloying in ionic liquid

International Nuclear Information System (INIS)

Jiang, Junhua; Wang, Xinying; Zhang, Lei

2013-01-01

Highlights: • A green chemistry method for producing nanoporous gold microelectrode was studied. • An ionic liquid plating bath was utilized for electrochemical alloying–dealloying. • Nanostructures of gold surface layers can be tuned by modulating potential. • Nanoporous gold microelectrode has high surface area and merit of a microelectrode. • Nitrite oxidation and reduction on nanoporous gold microelectrode were studied. -- Abstract: Nanoporous gold (NPG) microelectrodes with high surface area and open pore network were successfully prepared by applying modulated potential to a polycrystalline Au-disk microelectrode in ionic liquid electrolyte containing ZnCl 2 at elevated temperature. During cathodic process, Zn is electrodeposited and interacted with Au microdisk substrate to form a AuZn alloy phase. During subsequent anodic process, Zn is selectively dissolved from the alloy phase, leading to the formation of a NPG layer which can grow with repetitive potential modulation. Scanning-electron microscope and energy dispersive X-ray microscope measurements show that the NPG microelectrodes possessing nanoporous structures can be tuned via potential modulation, and chemically contain a small amount of Zn whose presence has no obvious influence on electrochemical responses of the electrodes. Steady-state and cyclic voltammetric studies suggest that the NPG microelectrodes have high surface area and keep diffusional properties of a microelectrode. Electrochemical nitrite reduction and oxidation are studied as model reactions to demonstrate potential applications of the NPG microelectrodes in electrocatalysis and electroanalysis. These facts suggest that the potential-modulated electrochemical alloying/dealloying in ionic liquid electrolyte offers a convenient green-chemistry method for the preparation of nanoporous microelectrodes

EDITORIAL: Physics competitions Physics competitions

Science.gov (United States)

Jordens, H.; Mathelitsch, L.

2009-11-01

1. Physics competitions: aims and realizations One aim of physics competitions is to increase the interest of young students, primarily at upper secondary level, to physics and natural sciences in general. A competition has motivational aspects known usually from sports events or games—comparing one's own ability with others, of course with the desire to be better and to win. If competitions reach nationwide and even international levels, additional stimulation is created. Competitions provide greatest attraction to possible winners, to the group of gifted people in a particular field. This implies that science contests are excellent tools for the promotion of talented students. Traditional teaching has been shown to have problems in supporting this group of students. Very often teachers are overstretched with the demands of teaching both low- and high-level students. Extracurricular activities are therefore a good chance to relieve the teacher, and to give talented students the opportunity for appropriate training and challenge. The competitions, however, have a broader impact and address more young people than one might guess from the statements above. Training courses and selection at school level give a larger group of students extra and, to some extent, complimentary education in physics. The degree of complexity of the tasks corresponds very often to the standards of the next level of education in the school system. Interestingly, many physics competitions have their origin in countries beyond the former Iron Curtain. They started as regional and national tournaments, were joined by neighbouring countries and have grown, in some cases, to events with participants from more than 80 countries. Although the features mentioned above are common to the different competitions, there are distinct differences between them [1]. The International Physics Olympiad (IPhO) is the oldest international physics competition for students at upper secondary level [2]. It dates

High-performance symmetric electrochemical capacitor based on graphene foam and nanostructured manganese oxide

Directory of Open Access Journals (Sweden)

Abdulhakeem Bello

2013-08-01

Full Text Available We have fabricated a symmetric electrochemical capacitor with high energy and power densities based on a composite of graphene foam (GF with ∼80 wt% of manganese oxide (MnO2 deposited by hydrothermal synthesis. Raman spectroscopy and X-ray diffraction measurements showed the presence of nanocrystalline MnO2 on the GF, while scanning and transmission electron microscopies showed needle-like manganese oxide coated and anchored onto the surface of graphene. Electrochemical measurements of the composite electrode gave a specific capacitance of 240 Fg−1 at a current density of 0.1 Ag−1 for symmetric supercapacitors using a two-electrode configuration. A maximum energy density of 8.3 Whkg−1 was obtained, with power density of 20 kWkg−1 and no capacitance loss after 1000 cycles. GF is an excellent support for pseudo-capacitive oxide materials such as MnO2, and the composite electrode provided a high energy density due to a combination of double-layer and redox capacitance mechanisms.

Synthesis and electrochemical performance of polyaniline-MnO2 nanowire composites for supercapacitors

Science.gov (United States)

Chen, Ling; Song, Zhaoxia; Liu, Guichang; Qiu, Jieshan; Yu, Chang; Qin, Jiwei; Ma, Lin; Tian, Fengqin; Liu, Wei

2013-02-01

Polyaniline-MnO2 nanowire (PANI-MNW) composites were prepared by in situ chemical oxidative polymerization of aniline monomer in a suspension of MnO2 nanowires. The structure and morphology of the PANI-MNW composites were characterized by powder X-ray diffraction (XRD) and scanning electron microscopy (SEM). Their electrochemical properties were investigated using cyclic voltammetry, galvanostatic charge-discharge and electrochemical impedance spectroscopy in 1 mol/L KOH electrolyte. The PANI-MNW composites show significantly better specific capacity and redox performance in comparison to the untreated MnO2 nanowires. The enhanced properties can be mainly attributed to the composite structure wherein high porosity is created between MnO2 nanowires and PANI during the process of fabricating the PANI-MNW nanocomposites. A specific capacitance as high as 256 F/g is obtained at a current density of 1 A/g for PANI-MNW-5, and the composite also shows a good cyclic performance and coulomb efficiency.

Application of electrochemical plasma techniques in surface engineering of iron based structural materials

International Nuclear Information System (INIS)

Coaca, E.; Rusu, O.; Mihalache, M.; Minca, M.; Tacica, M.; Florea, S.; Oncioiu, G.; Andrei, V.

2013-01-01

The surface of austenitic stainless steels 304 L and 316 L was modified by various complex surface treatments: - plasma electrolytic carbo-nitriding by means of Plasma electrolytic saturation (PES); the saturation of cathodic surfaces with C, N was performed using suitable electrolytes (aqueous solutions of inorganic acids, appropriate salts containing the desired elements and certain organic compounds); -electrodeposition of Al from ChCl based Ionic Liquid. The coatings obtained in various experimental conditions have been investigated by means of electron spectroscopy, scanning electron microscopy, energy dispersion x-ray spectrometry, electrochemical techniques, and the properties of the thin films have been correlated with the microstructure and the composition of the surface layers which are strongly dependents of the different regimes of diffusion treatments. The preliminary results on Electrochemical Plasma Technology (EPT) treatments demonstrate that we can select the processing parameters for essential improvement of corrosion behaviour in some aggressive medium and high values of microhardness. (authors)

Electrochemical preparation of iron cuboid nanoparticles and their catalytic properties for nitrite reduction

International Nuclear Information System (INIS)

Chen Yanxin; Chen Shengpei; Chen Qingsong; Zhou Zhiyou; Sun Shigang

2008-01-01

Iron cuboid nanoparticles supported on glassy carbon (denoted nm-Fe/GC) were prepared by electrochemical deposition under cyclic voltammetric (CV) conditions. The structure and composition of the Fe nanomaterials were characterized by scanning electron microscopy (SEM), selected area electron diffraction (SAED), X-ray diffraction (XRD) and energy dispersive X-ray analysis (EDX). The results demonstrated that the Fe cuboid nanoparticles are dispersed discretely on GC substrate with an average size ca. 171 nm, and confirmed that the electrochemical synthesized nanocubes are single crystals of pure Fe. The catalytic properties of the Fe cuboid nanoparticles towards nitrite electroreduction were investigated, and enhanced electrocatalytic activity of the Fe nanocubes has been determined. In comparison with the data obtained on a bulk-Fe electrode, the onset potential of nitrite reduction on nm-Fe/GC is positively sifted by 100 mV, and the steady reduction current density is enhanced about 2.4-3.2 times

Disposable screen printed graphite electrode for the direct electrochemical determination of ibuprofen in surface water

KAUST Repository

Amin, Sidra; Soomro, M. Tahir; Memon, Najma; Solangi, Amber R.; Sirajuddin; Qureshi, Tahira; Behzad, Ali Reza

2014-01-01

The potential of square wave voltammetry (SWV) for the determination of ibuprofen in aqueous solution, applying baseline correction, is reported. A screen printed graphite electrodes (SPGEs), especially pretreated for this purpose, were used to investigate the electrochemical oxidation and detection of ibuprofen. After optimization of SWV parameters, measurements were carried out at 200 Hz modulation frequency, 4 mV step potential and 40 mV pulse amplitude for the determination of ibuprofen. The surfaces of both untreated and pretreated SPGEs were characterized by scanning electron microscopy (SEM) and electrochemical impedance spectroscopy (EIS). The electro-catalytic properties of both the electrodes were correlated with the surface treatment. The pretreated screen printed graphite electrode exhibited a high sensitivity toward ibuprofen even in low concentration. The developed method was found rapid, cost-effective and reproducible for in-field ibuprofen detection.

Disposable screen printed graphite electrode for the direct electrochemical determination of ibuprofen in surface water

KAUST Repository

Amin, Sidra

2014-08-01

The potential of square wave voltammetry (SWV) for the determination of ibuprofen in aqueous solution, applying baseline correction, is reported. A screen printed graphite electrodes (SPGEs), especially pretreated for this purpose, were used to investigate the electrochemical oxidation and detection of ibuprofen. After optimization of SWV parameters, measurements were carried out at 200 Hz modulation frequency, 4 mV step potential and 40 mV pulse amplitude for the determination of ibuprofen. The surfaces of both untreated and pretreated SPGEs were characterized by scanning electron microscopy (SEM) and electrochemical impedance spectroscopy (EIS). The electro-catalytic properties of both the electrodes were correlated with the surface treatment. The pretreated screen printed graphite electrode exhibited a high sensitivity toward ibuprofen even in low concentration. The developed method was found rapid, cost-effective and reproducible for in-field ibuprofen detection.

Electrochemical migration of tin in electronics and microstructure of the dendrites

Energy Technology Data Exchange (ETDEWEB)

Minzari, Daniel, E-mail: dmin@mek.dtu.d [Section for Materials and Surface Technology, Department for Mechanical Engineering, Technical University of Denmark (Denmark); Grumsen, Flemming Bjerg; Jellesen, Morten S.; Moller, Per; Ambat, Rajan [Section for Materials and Surface Technology, Department for Mechanical Engineering, Technical University of Denmark (Denmark)

2011-05-15

Graphical abstract: The electrochemical migration of tin in electronics forms dendritic structures, consisting of a metallic tin core, which is surrounded by oxide layers having various thickness. Display Omitted Research highlights: Electrochemical migration occurs if two conductors are connected by condensed moisture. Metallic ions are dissolved and grow in a dendritic structure that short circuit the electrodes. The dendrite consists of a metallic tin core with oxide layers of various thickness surrounding. Detailed microstructure of dendrites is investigated using electron microscopy. The dendrite microstructure is heterogeneous along the growth direction. - Abstract: The macro-, micro-, and nano-scale morphology and structure of tin dendrites, formed by electrochemical migration on a surface mount ceramic chip resistor having electrodes consisting of tin with small amounts of Pb ({approx}2 wt.%) was investigated by scanning electron microscopy and transmission electron microscopy including Energy dispersive X-ray spectroscopy and electron diffraction. The tin dendrites were formed under 5 or 12 V potential bias in 10 ppm by weight NaCl electrolyte as a micro-droplet on the resistor during electrochemical migration experiments. The dendrites formed were found to have heterogeneous microstructure along the growth direction, which is attributed to unstable growth conditions inside the micro-volume of electrolyte. Selected area electron diffraction showed that the dendrites are metallic tin having sections of single crystal orientation and lead containing intermetallic particles embedded in the structure. At certain areas, the dendrite structure was found to be surrounded by an oxide crust, which is believed to be due to unstable growth conditions during the dendrite formation. The oxide layer was found to be of nanocrystalline structure, which is expected to be formed by the dehydration of the hydrated oxide originally formed in solution ex-situ in ambient air.

Observation of Dynamic Interfacial Layers in Li-Ion and Li-O_2 Batteries by Scanning Electrochemical Microscopy

International Nuclear Information System (INIS)

Bülter, Heinz; Schwager, Patrick; Fenske, Daniela; Wittstock, Gunther

2016-01-01

Highlights: • Imaging changes of solid electrolyte interphases on rinsed lithiated graphite. • Strongly non-uniform changes of SEI passivation properties. • In situ imaging of clogged gas diffusion electrodes of Li/O_2 batteries. - Abstract: The requirements of high energy density in modern batteries dictate the use of very high (oxidizing) or very low (reducing) potential for negative and positive electrode materials. These extreme potentials can cause molecular compounds to undergo electron transfer reactions at the interfaces. This is well documented for lithium-ion batteries, where a solid electrolyte interphase (SEI) between the lithiated graphite electrode and the electrolyte is formed by the decomposition of electrolyte components mainly during the first charging process. Characterization of the SEI is a challenge because of the variety of chemically similar components and enclosed electrolyte species. Furthermore, ex situ analysis of the SEI requires separation and isolation of the SEI, which may change the content and the structure of the SEI. Scanning electrochemical microscopy (SECM) provides in situ analysis of passivating layers formed at battery electrodes. Such approaches must deal with continuous changes of the studied interfaces. This is illustrated for the in situ investigation of the electron transport at SEI-covered lithiated graphite using 2,5-di-tert-butyl-1,4-dimethoxy benzene as SECM mediator in an inert atmosphere. With this setup, the influence of rinsing protocols on the passivating properties of the SEI was studied. An extensive rinsing compared to our previous studies [DOI 10.1002/anie.201403935] leads to much higher local variation of the SEI passivation properties which continue over the entire observation time of 54 h. The second example uses a SECM generation-collection experiment to detect gas permeation through a gas-diffusion electrode (GDE) of a Li-O_2 cell into a Li"+-containing organic electrolyte. The passivation of the

One-step electrochemical synthesis and photoelectric conversion of a ZnO/Se/RGO composite

International Nuclear Information System (INIS)

Wang, Lei; Zhang, Chunyan; Zhang, Shengyi; Niu, Helin; Song, Jiming; Mao, Changjie; Jin, Baokang; Tian, Yupeng

2015-01-01

Using Zn(NO 3 ) 2 , H 2 SeO 3 and graphene oxide as precursors, the zinc oxide/selenium/reduced graphene oxide (ZnO/Se/RGO) composite was facilely electrodeposited on the surface of indium tin oxide glass. The conditions for electrochemical synthesis such as electrodeposition potential and electrolyte composition were studied. The morphology and crystallization of the products as-prepared were characterized using scanning electron microscopy (SEM) and x-ray diffractometry (XRD) respectively. The light absorption and conductivity of the products were studied by UV-visible spectroscopy (UV-vis) and electrochemical impedance spectroscopy (EIS). Based on a series of experimental results, the photoelectrical conversion mechanism and effect factors of the products were explored. By means of synergistic action of n-type ZnO, p-type Se and conductive RGO, the ZnO/Se/RGO composite showed excellent photoelectric conversion under visible light irradiation. (paper)

Electrochemical Determination of Uric Acid at CdTe Quantum Dot Modified Glassy Carbon Electrodes.

Science.gov (United States)

Pan, Deng; Rong, Shengzhong; Zhang, Guangteng; Zhang, Yannan; Zhou, Qiang; Liu, Fenghai; Li, Miaojing; Chang, Dong; Pan, Hongzhi

2015-01-01

Cyclic voltammetry and differential pulse voltammetry were used to investigate the electrochemical behavior of uric acid (UA) at a CdTe quantum dot (QD) modified the glassy carbon electrode (GCE). CdTe QDs, as new semiconductor nanocrystals, can greatly improve the peak current of UA. The anodic peak current of UA was linear with its concentration between 1.0×10(-6) and 4.0×10(-4) M in 0.1 M pH 5.0 phosphate buffer solution. The LOD for UA at the CdTe electrode (1.0×10(-7) M) was superior to that of the GCE. In addition, we also determined the effects of scan rate, pH, and interferences of UA for the voltammetric behavior and detection. The results indicated that modified electrode possessed excellent reproducibility and stability. Finally, a new and efficient electrochemical sensor for detecting UA was developed.

COMPETITIVENESS AND COMPETITIVE ORIENTATIONS: EVALUATION OF STUDENTS

Directory of Open Access Journals (Sweden)

G. Z. Efimova

2017-01-01

Full Text Available Introduction. Education of a competitive student is a strategically significant problem of the system of higher education in modern social and economic conditions. Personal competitiveness and competitive orientations – priority quality of future expert for successful future professional experience.The aim of the present research is to study factors of competitive orientations formation and criteria for evaluation of competitiveness of student’s youth in the Russian society.Methodology and research methods. Results of theoretical researches of Russian and foreign researchers are generalized; secondary analysis of data based on results of sociological researches and analysis of official statistical data are carried out. The results of the sociological survey undertaken in 2017 on the basis of statistical methods were processed and studied by the instrumentality of IBM SPSS Statistics 23 program; 1196 students of institutions of higher and secondary vocational education of the Tyumen region took part.Results and scientific novelty. It is stated that senior students feel themselves more competitive. It is revealed that a quarter of students who took part in the survey, generally men, count themselves competitive. A continuous distance of goal-setting is recorded among these respondents; in every third case they have plans of professional growth for five and more years that allows them to build attractive competitive strategy.The level of the competitiveness is directly connected with such indicators as “social stratum”, “overall life satisfaction”, “self-esteem of health”, “tendency to lead a healthy lifestyle” and “the level of trust in the surrounding people”. Mostly the students oriented on competition look into the future with confidence and optimism.Respondents focused on the competitiveness were more tend to demonstrate their abilities and cause admiration, have a creative approach towards work, be ready for surprises

The Aqueous Electrochemical Response of TiC–Stainless Steel Cermets

Directory of Open Access Journals (Sweden)

Chukwuma Onuoha

2018-05-01

Full Text Available A family of TiC–stainless steel ceramic–metal composites, or cermets, has been developed in the present study, using steel grades of 304 L, 316 L, or 410 L as the binder phase. Melt infiltration was used to prepare the cermets, with the steel binder contents varying between 10–30 vol. %. The corrosion behaviour was evaluated using a range of electrochemical techniques in an aqueous solution containing 3.5 wt. % NaCl. The test methods included potentiodynamic, cyclic, and potentiostatic polarisation. The corroded samples were subsequently characterised using scanning electron microscopy (SEM and energy dispersive X-ray spectroscopy (EDS, while the post-corrosion solutions were analysed using inductively coupled plasma optical emission spectroscopy (ICP-OES to determine the residual ionic and particulate material removed from the cermets during electrochemical testing. It was demonstrated that the corrosion resistance was enhanced through decreasing the steel binder content, which arises due to the preferential dissolution of the binder phase, while the TiC ceramic remains largely unaffected. Increasing corrosion resistance was observed in the sequence TiC-304 L > TiC-316 L > TiC-410 L.

In Vivo Electrochemical Analysis of a PEDOT/MWCNT Neural Electrode Coating

Directory of Open Access Journals (Sweden)

Nicolas A. Alba

2015-10-01

Full Text Available Neural electrodes hold tremendous potential for improving understanding of brain function and restoring lost neurological functions. Multi-walled carbon nanotube (MWCNT and dexamethasone (Dex-doped poly(3,4-ethylenedioxythiophene (PEDOT coatings have shown promise to improve chronic neural electrode performance. Here, we employ electrochemical techniques to characterize the coating in vivo. Coated and uncoated electrode arrays were implanted into rat visual cortex and subjected to daily cyclic voltammetry (CV and electrochemical impedance spectroscopy (EIS for 11 days. Coated electrodes experienced a significant decrease in 1 kHz impedance within the first two days of implantation followed by an increase between days 4 and 7. Equivalent circuit analysis showed that the impedance increase is the result of surface capacitance reduction, likely due to protein and cellular processes encapsulating the porous coating. Coating’s charge storage capacity remained consistently higher than uncoated electrodes, demonstrating its in vivo electrochemical stability. To decouple the PEDOT/MWCNT material property changes from the tissue response, in vitro characterization was conducted by soaking the coated electrodes in PBS for 11 days. Some coated electrodes exhibited steady impedance while others exhibiting large increases associated with large decreases in charge storage capacity suggesting delamination in PBS. This was not observed in vivo, as scanning electron microscopy of explants verified the integrity of the coating with no sign of delamination or cracking. Despite the impedance increase, coated electrodes successfully recorded neural activity throughout the implantation period.

Electrochemical oxidation of organic waste

International Nuclear Information System (INIS)

Almon, A.C.; Buchanan, B.R.

1990-01-01

Both silver catalyzed and direct electrochemical oxidation of organic species are examined in analytical detail. This paper describes the mechanisms, reaction rates, products, intermediates, capabilities, limitations, and optimal reaction conditions of the electrochemical destruction of organic waste. A small bench-top electrocell being tested for the treatment of small quantities of laboratory waste is described. The 200-mL electrochemical cell used has a processing capacity of 50 mL per day, and can treat both radioactive and nonradioactive waste. In the silver catalyzed process, Ag(I) is electrochemically oxidized to Ag(II), which attacks organic species such as tributylphosphate (TBP), tetraphenylborate (TPB), and benzene. In direct electrochemical oxidation, the organic species are destroyed at the surface of the working electrode without the use of silver as an electron transfer agent. This paper focuses on the destruction of tributylphosphate (TBP), although several organic species have been destroyed using this process. The organic species are converted to carbon dioxide, water, and inorganic acids

Electrochemical, morphological and microstructural characterization of carbon film resistor electrodes for application in electrochemical sensors

International Nuclear Information System (INIS)

Gouveia-Caridade, Carla; Soares, David M.; Liess, Hans-Dieter; Brett, Christopher M.A.

2008-01-01

The electrochemical and microstructural properties of carbon film electrodes made from carbon film electrical resistors of 1.5, 15, 140 Ω and 2.0 kΩ nominal resistance have been investigated before and after electrochemical pre-treatment at +0.9 V vs SCE, in order to assess the potential use of these carbon film electrodes as electrochemical sensors and as substrates for sensors and biosensors. The results obtained are compared with those at electrodes made from previously investigated 2 Ω carbon film resistors. Cyclic voltammetry was performed in acetate buffer and phosphate buffer saline electrolytes and the kinetic parameters of the model redox system Fe(CN) 6 3-/4- obtained. The 1.5 Ω resistor electrodes show the best properties for sensor development with wide potential windows, similar electrochemical behaviour to those of 2 Ω and close-to-reversible kinetic parameters after electrochemical pre-treatment. The 15 and 140 Ω resistor electrodes show wide potential windows although with slower kinetics, whereas the 2.0 kΩ resistor electrodes show poor cyclic voltammetric profiles even after pre-treatment. Electrochemical impedance spectroscopy related these findings to the interfacial properties of the electrodes. Microstructural and morphological studies were carried out using contact mode Atomic Force Microscopy (AFM), Confocal Raman spectroscopy and X-ray diffraction. AFM showed more homogeneity of the films with lower nominal resistances, related to better electrochemical characteristics. X-ray diffraction and Confocal Raman spectroscopy indicate the existence of a graphitic structure in the carbon films

High-performance lithium-rich layered oxide materials: Effects of chelating agents on microstructure and electrochemical properties

International Nuclear Information System (INIS)

Li, Lingjun; Xu, Ming; Chen, Zhaoyong; Zhou, Xiang; Zhang, Qiaobao; Zhu, Huali; Wu, Chun; Zhang, Kaili

2015-01-01

The mechanisms and effects of three typical chelating agents, namely glucose, citric acid and sucrose on the sol-gel synthesis process, electrochemical degradation and structural evolution of 0.5Li 2 MnO 3 ·0.5LiNi 0.5 Co 0.2 Mn 0.3 O 2 (LLMO) materials are systematically compared for the first time. X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy and high-resolution transmission electron microscopy analysis indicate that the sample synthesized from sucrose owns well structure, homogenous distribution, low Ni 3+ concentration and good surface structural stability during cycling, respectively. Electrochemical tests further prove that the LLMO material obtained from sucrose maintains 258.4 mAh g −1 with 94.8% capacity retention after 100 cycles at 0.2 C. The superior electrochemical performance can be ascribed to the exceptional complexing mechanism of sucrose, compared to those of the glucose and citric acid. Namely, one mole sucrose can be hydrolyzed into two different monosaccharides and further chelates three M (Li, Ni, Co and Mn) ions to form a more uniform ion-chelated matrix during sol-gel process. This discovery is an important step towards understanding the selection criterion of chelating agents for sol-gel method, that chelating agent with excellent complexing capability is beneficial to the distribution, structural stability and electrochemical properties of advanced lithium-rich layered materials

Rapid extraction and quantitative detection of the herbicide diuron in surface water by a hapten-functionalized carbon nanotubes based electrochemical analyzer.

Science.gov (United States)

Sharma, Priyanka; Bhalla, Vijayender; Tuteja, Satish; Kukkar, Manil; Suri, C Raman

2012-05-21

A solid phase extraction micro-cartridge containing a non-polar polystyrene absorbent matrix was coupled with an electrochemical immunoassay analyzer (EIA) and used for the ultra-sensitive detection of the phenyl urea herbicide diuron in real samples. The EIA was fabricated by using carboxylated carbon nanotubes (CNTs) functionalized with a hapten molecule (an amine functionalized diuron derivative). Screen printed electrodes (SPE) were modified with these haptenized CNTs and specific in-house generated anti diuron antibodies were used for bio-interface development. The immunodetection was realized in a competitive electrochemical immunoassay format using alkaline phosphatase labeled secondary anti-IgG antibody. The addition of 1-naphthyl phosphate substrate resulted in the production of an electrochemically active product, 1-naphthol, which was monitored by using differential pulse voltammetry (DPV). The assay exhibited excellent sensitivity and specificity having a dynamic response range of 0.01 pg mL(-1) to 10 μg mL(-1) for diuron with a limit of detection of around 0.1 pg mL(-1) (n = 3) in standard water samples. The micro-cartridge coupled hapten-CNTs modified SPE provided an effective and efficient electrochemical immunoassay for the real-time monitoring of pesticides samples with a very high degree of sensitivity.

An electrochemical approach: Switching Structures of rare earth metal Praseodymium hexacyanoferrate and its application to sulfite sensor in Red Wine

International Nuclear Information System (INIS)

Devadas, Balamurugan; Sivakumar, Mani; Chen, Shen Ming; Cheemalapati, Srikanth

2015-01-01

Graphical abstract: Nucleation and growth of PrHCF and its application to sulfite oxidation in wine samples. - Highlights: • Electrochemical synthesis of PrHCF. • Switching structures of PrHCF. • Sulfite electrochemical sensor. • Wide linear range and low limit of detection. • Real sample application. - Abstract: Herein, we report a shape-controlled preparation of Praseodymium hexacyanoferrate (PrHCF) using a simple electrochemical technique. The electrochemically fabricated PrHCF modified glassy carbon electrodes (GCE) shows an excellent electrocatalytic activity towards sulfite oxidation. The morphology of PrHCF particles were controlled by carefully changing various synthesis conditions including electrochemical technique (cyclic voltammetry, amperometry and chemical), cations in the supporting electrolyte (K + , Na + , Li + and H + ), deposition cycles, molar ratio of precursors, and applied potential (-.2,0 and 0.2 V). The morphologies of the PrHCF was elucidated using scanning electron microscopy (SEM). The as-synthesized PrHCF was characterized using X-ray diffraction pattern (XRD), Infra-red (IR) and energy dispersive X-ray spectroscopy (EDX). The electrochemical oxidation of sulfite on PrHCF modified GCE was investigated using cyclic voltammetry (CV) and linear sweep voltammetry (LSV). The sensitivity of the as-developed sulfite sensor was determined to be 0.036 μA μM −1 cm −2 . The low limit of detection was determined to be 2.15 μM. The real time application of PrHCF modified GCE was confirmed through the determination of sulfite from red wine and tap water samples

Morphological reason for enhancement of electrochemical double layer capacitances of various acetylene blacks by electrochemical polarization

International Nuclear Information System (INIS)

Kim, Taegon; Ham, Chulho; Rhee, Choong Kyun; Yoon, Seong-Ho; Tsuji, Masaharu; Mochida, Isao

2008-01-01

Enhancement of electrochemical capacitance and morphological variations of various acetylene blacks caused by electrochemical polarization are presented. Acetylene blacks of different mean particle diameters were modified by air-oxidation and heat treatment to diversify the morphologies of the acetylene blacks before electrochemical polarization. The various acetylene blacks were electrochemically oxidized at 1.6 V (vs. Ag/AgCl) for 10 s and the polarization step was repeated until the capacitance values did not change any longer. These polarization steps enhanced the capacitances of the acetylene blacks and the specific enhancement factors range from 2 to 5.5. Such an enhancement is strongly related to morphological modification as revealed by transmission electron microscopic observations. The electrochemical polarization resulted in formation of tiny graphene sheets on the wide graphitic carbon surfaces, which were most responsible for the observed capacitive enhancement. Although the pseudo-capacitance increased after polarization by forming oxygenated species on the surfaces, its contribution to the total capacitance was less than 10%. The mechanism of the formation of the tiny graphene sheets during the electrochemical oxidation is described schematically

Investigation of the electrochemically active surface area and lithium diffusion in graphite anodes by a novel OsO4 staining method

Science.gov (United States)

Pfaffmann, Lukas; Birkenmaier, Claudia; Müller, Marcus; Bauer, Werner; Mitsch, Tim; Feinauer, Julian; Krämer, Yvonne; Scheiba, Frieder; Hintennach, Andreas; Schleid, Thomas; Schmidt, Volker; Ehrenberg, Helmut

2016-03-01

Negative electrodes of lithium-ion batteries generally consist of graphite-based active materials. In order to realize batteries with a high current density and therefore accelerated charging processes, the intercalation of lithium and the diffusion processes of these carbonaceous materials must be understood. In this paper, we visualized the electrochemical active surface area for three different anode materials using a novel OsO4 staining method in combination with scanning electron microscopy techniques. The diffusion behavior of these three anode materials is investigated by potentiostatic intermittent titration technique measurements. From those we determine the diffusion coefficient with and without consideration of the electrochemical active surface area.

Electron transport determines the electrochemical properties of tetrahedral amorphous carbon (ta-C) thin films

International Nuclear Information System (INIS)

Palomäki, Tommi; Wester, Niklas; Caro, Miguel A.; Sainio, Sami; Protopopova, Vera; Koskinen, Jari; Laurila, Tomi

2017-01-01

Amorphous carbon based electrodes are very promising for electrochemical sensing applications. In order to better understand their structure-function relationship, the effect of film thickness on the electrochemical properties of tetrahedral amorphous carbon (ta-C) electrodes was investigated. ta-C thin films of 7, 15, 30, 50 and 100 nm were characterized in detail with Raman spectroscopy, transmission electron microscopy (TEM), conductive atomic force microscopy (c-AFM), scanning tunneling spectroscopy (STS) and X-ray absorption spectroscopy (XAS) to assess (i) the surface properties of the films, (ii) the effect of film thickness on their structure and electrical properties and (iii) the subsequent correlation with their electrochemistry. The electrochemical properties were investigated by cyclic voltammetry (CV) using two different outer-sphere redox probes, Ru(NH 3 ) 6 3+/2+ and FcMeOH, and by electrochemical impedance spectroscopy (EIS). Computational simulations using density functional theory (DFT) were carried out to rationalize the experimental findings. The characterization results showed that the sp 2 /sp 3 ratio increased with decreasing ta-C film thickness. This correlated with a decrease in mobility gap value and an increase in the average current through the films, which was also consistent with the computational results. XAS indicated that the surface of the ta-C films was always identical and composed of a sp 2 -rich layer. The CV measurements indicated reversible reaction kinetics for both outer-sphere redox probes at 7 and 15 nm ta-C films with a change to quasi-reversible behavior at a thickness of around 30 nm. The charge transfer resistance, obtained from EIS measurements, decreased with decreasing film thickness in accordance with the CV results. Based on the characterization and electrochemical results, we conclude that the reaction kinetics in the case of outer-sphere redox systems is determined mainly by the electron transport through the

Fabrication of highly sensitive gold nanourchins based electrochemical sensor for nanomolar determination of primaquine

International Nuclear Information System (INIS)

Thapliyal, Neeta Bachheti; Chiwunze, Tirivashe Elton; Karpoormath, Rajshekhar; Cherukupalli, Srinivasulu

2017-01-01

A gold nanourchins modified glassy carbon electrode (AuNu/GCE) was developed for the determination of antimalarial drug, primaquine (PQ). The surface of AuNu/GCE was characterized by electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and cyclic voltammetry (CV). EIS results indicated that the electron transfer process at AuNu/GCE was faster as compared to the bare electrode. The SEM and TEM image confirmed the presence and uniform dispersion of gold nanourchins on the GCE surface. Upon investigating the electrochemical behavior of PQ at AuNu/GCE, the developed sensor was found to exhibit high electrocatalytic activity towards the oxidation of PQ. Under optimal experimental conditions, the sensor showed fast and sensitive current response to PQ over a linear concentration range of 0.01–1 μM and 0.001–1 μM with a detection limit of 3.5 nM and 0.9 nM using differential pulse voltammetry (DPV) and square wave voltammetry (SWV), respectively. The AuNu/GCE showed good selectivity, reproducibility and stability. Further, the developed sensor was successfully applied to determine the drug in human urine samples and pharmaceutical formulations demonstrating its analytical applicability in clinical analysis as well as quality control. The proposed method thus provides a promising alternative in routine sensing of PQ as well as promotes the application of gold nanourchins in electrochemical sensors. - Graphical abstract: A gold nanourchins modified glassy carbon electrode was fabricated and used as an electrochemical sensing platform for the determination of primaquine. Display Omitted - Highlights: • Gold nanourchins based electrochemical sensor for determination of primaquine • A detection limit of 0.9 nM was obtained using square wave voltammetry. • Proposed method was applied to quantify the drug in tablet and human urine samples. • Fast, simple and low-cost method for trace analysis of

Fabrication of highly sensitive gold nanourchins based electrochemical sensor for nanomolar determination of primaquine

Energy Technology Data Exchange (ETDEWEB)

Thapliyal, Neeta Bachheti, E-mail: thapliyaln@ukzn.ac.za; Chiwunze, Tirivashe Elton; Karpoormath, Rajshekhar, E-mail: karpoormath@ukzn.ac.za; Cherukupalli, Srinivasulu

2017-05-01

A gold nanourchins modified glassy carbon electrode (AuNu/GCE) was developed for the determination of antimalarial drug, primaquine (PQ). The surface of AuNu/GCE was characterized by electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and cyclic voltammetry (CV). EIS results indicated that the electron transfer process at AuNu/GCE was faster as compared to the bare electrode. The SEM and TEM image confirmed the presence and uniform dispersion of gold nanourchins on the GCE surface. Upon investigating the electrochemical behavior of PQ at AuNu/GCE, the developed sensor was found to exhibit high electrocatalytic activity towards the oxidation of PQ. Under optimal experimental conditions, the sensor showed fast and sensitive current response to PQ over a linear concentration range of 0.01–1 μM and 0.001–1 μM with a detection limit of 3.5 nM and 0.9 nM using differential pulse voltammetry (DPV) and square wave voltammetry (SWV), respectively. The AuNu/GCE showed good selectivity, reproducibility and stability. Further, the developed sensor was successfully applied to determine the drug in human urine samples and pharmaceutical formulations demonstrating its analytical applicability in clinical analysis as well as quality control. The proposed method thus provides a promising alternative in routine sensing of PQ as well as promotes the application of gold nanourchins in electrochemical sensors. - Graphical abstract: A gold nanourchins modified glassy carbon electrode was fabricated and used as an electrochemical sensing platform for the determination of primaquine. Display Omitted - Highlights: • Gold nanourchins based electrochemical sensor for determination of primaquine • A detection limit of 0.9 nM was obtained using square wave voltammetry. • Proposed method was applied to quantify the drug in tablet and human urine samples. • Fast, simple and low-cost method for trace analysis of

Effect of graphene oxide nanoplatelets on electrochemical properties of steel substrate in saline media

International Nuclear Information System (INIS)

Chaudhry, A.U.; Mittal, Vikas; Mishra, Brajendra

2015-01-01

There has been increased interest in using graphene oxide (GO) in various industrial applications such as working fluids, lubricants, oil and gas fields, heavy metal removal from water, anticorrosion paints and coatings etc. We studied electrochemical properties of steel in the presence of suspended GO in saline media. GO suspension has been characterized using Transmission electron microscopy (TEM) and X-ray diffractometer (XRD). We measured the effect of the GO concentration (0–15 ppm) on electrochemical properties of steel using different techniques: open circuit potential (OCP), electrochemical impedance spectroscopy (EIS), linear polarization resistance (LPR) and potentiodynamic (PD) methods. Results indicate that the suppression of corrosion is directly proportional to increasing GO concentrations in saline environments. Surface morphology of corroded samples was examined using Scanning Electron Microscopy (SEM). Identification of the elements at accumulated layer was estimated from peaks of energy dispersive x-ray spectroscopy (EDX) and XRD. Increased protection abilities with increasing GO concentration have been attributed to the domination of salt layer presence at the surface of steel which occurs via precipitation of sodium chloride. Surface analysis confirm that there is no direct effect of GO on the protection behavior of steel. The presence of GO in the solution can enhance the precipitation of NaCl due to the decreased solubility NaCl which further slows down the corrosion. The pourbaix diagram shows that GO forms an anionic compound with sodium which may enhance the precipitation at working electrode. - Graphical abstract: Display Omitted - Highlights: • Electrochemical properties of steel in saline media containing nano graphene oxide. • Effect of concentration of graphene oxide on electrochemical properties. • Mechanism of corrosion reduction due to the presence of graphene oxide

Characterization by acoustic emission and electrochemical impedance spectroscopy of the cathodic disbonding of Zn coating

International Nuclear Information System (INIS)

Amami, Souhail; Lemaitre, Christian; Laksimi, Abdelouahed; Benmedakhene, Salim

2010-01-01

Galvanized steel has been tested in a synthetic sea water solution under different cathodic overprotection conditions. The generated hydrogen flux caused the damage of the metal-zinc interface and led to a progressive coating detachment. Scanning electron microscopy, electrochemical impedance spectroscopy and acoustic emission technique were used to characterize the damage chronology under different cathodic potentials. A damage mechanism was proposed and the acoustic signature related to the coating degradation was statistically identified using clustering techniques.

Characterization by acoustic emission and electrochemical impedance spectroscopy of the cathodic disbonding of Zn coating

Energy Technology Data Exchange (ETDEWEB)

Amami, Souhail [Universite de Technologie de Compiegne, Departement de Genie Mecanique, Laboratoire Roberval, UMR 6066 du CNRS, B.P. 20529, 60206 Compiegne Cedex (France)], E-mail: souhail.amami@utc.fr; Lemaitre, Christian; Laksimi, Abdelouahed; Benmedakhene, Salim [Universite de Technologie de Compiegne, Departement de Genie Mecanique, Laboratoire Roberval, UMR 6066 du CNRS, B.P. 20529, 60206 Compiegne Cedex (France)

2010-05-15

Galvanized steel has been tested in a synthetic sea water solution under different cathodic overprotection conditions. The generated hydrogen flux caused the damage of the metal-zinc interface and led to a progressive coating detachment. Scanning electron microscopy, electrochemical impedance spectroscopy and acoustic emission technique were used to characterize the damage chronology under different cathodic potentials. A damage mechanism was proposed and the acoustic signature related to the coating degradation was statistically identified using clustering techniques.

Electrochemical synthesis of polypyrrole on ferrous and non-ferrous metals from sweet aqueous electrolytic medium

International Nuclear Information System (INIS)

Bazzaoui, M.; Martins, J.I.; Reis, T.C.; Bazzaoui, E.A.; Nunes, M.C.; Martins, L.

2005-01-01

The electrodeposition of polypyrrole (PPy) on oxidizable metals such as aluminum and iron has been achieved in aqueous medium of saccharin and pyrrole. Scanning electron microscopy and X-ray photoelectron spectroscopy analysis reveal a good homogeneity of the obtained PPy film. The electrochemical synthesis of PPy coating has been achieved successfully under potentiodynamic, galvanostatic and potentiostatic techniques. The corrosion experiments performed in HCl show that the PPy coating increases the corrosion potential and decreases the corrosion current density

Synthesis, spectroscopic and electrochemical performance of pasted β-nickel hydroxide electrode in alkaline electrolyte

Science.gov (United States)

Shruthi, B.; Bheema Raju, V.; Madhu, B. J.

2015-01-01

β-Nickel hydroxide (β-Ni(OH)2) was successfully synthesized using precipitation method. The structure and property of the β-Ni(OH)2 were characterized by X-ray diffraction (XRD), Fourier Transform infra-red (FT-IR), Raman spectra and thermal gravimetric-differential thermal analysis (TG-DTA). The results of the FTIR spectroscopy and TG-DTA studies indicate that the β-Ni(OH)2 contains water molecules and anions. The microstructural and composition studies have been performed using Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray (EDX) analysis. A pasted-type electrode is prepared using β-Ni(OH)2 powder as the active material on a nickel sheet as a current collector. Cyclic voltammetry (CV) and Electrochemical impedance spectroscopy (EIS) studies were performed to evaluate the electrochemical performance of the β-Ni(OH)2 electrode in 6 M KOH electrolyte. CV curves showed a pair of strong redox peaks as a result of the Faradaic redox reactions of β-Ni(OH)2. The proton diffusion coefficient (D) for the present β-Ni(OH)2 electrode material is found to be 1.44 × 10-12 cm2 s-1. Further, electrochemical impedance studies confirmed that the β-Ni(OH)2 electrode reaction processes are diffusion controlled.

Modified glassy carbon electrodes based on carbon nanostructures for ultrasensitive electrochemical determination of furazolidone

Energy Technology Data Exchange (ETDEWEB)

Shahrokhian, Saeed, E-mail: shahrokhian@sharif.edu [Department of Chemistry, Sharif University of Technology, Tehran 11155-9516 (Iran, Islamic Republic of); Institute for Nanoscience and Nanotechnology, Sharif University of Technology, Tehran (Iran, Islamic Republic of); Naderi, Leila [Department of Chemistry, Sharif University of Technology, Tehran 11155-9516 (Iran, Islamic Republic of); Ghalkhani, Masoumeh [Department of Chemistry, Faculty of Science, Shahid Rajaee Teacher Training University, Lavizan, Tehran (Iran, Islamic Republic of); Institute for advanced technology, Shahid Rajaee Teacher Training University, Lavizan, Tehran, 16788 (Iran, Islamic Republic of)

2016-04-01

The electrochemical behavior of Furazolidone (Fu) was investigated on the surface of the glassy carbon electrode modified with different carbon nanomaterials, including carbon nanotubes (CNTs), carbon nanoparticles (CNPs), nanodiamond-graphite (NDG), graphene oxide (GO), reduced graphene oxide (RGO) and RGO-CNT hybrids (various ratios) using linear sweep voltammetry (LSV). The results of voltammetric studies exhibited a considerable increase in the cathodic peak current of Fu at the RGO modified GCE, compared to other modified electrodes and also bare GCE. The surface morphology and nature of the RGO film was thoroughly characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV) techniques. The modified electrode showed two linear dynamic ranges of 0.001–2.0 μM and 2.0–10.0 μM with a detection limit of 0.3 nM for the voltammetric determination of Fu. This sensor was used successfully for Fu determination in pharmaceutical and clinical preparations. - Highlights: • The electrochemical behavior of Furazolidone (Fu) was investigated on the surface of the modified electrode with different carbon nanomaterials by Linear sweep voltammetry. • Two linear dynamic ranges and a low detection limit were obtained. • The modified electrode was applied for the detection of Fu in pharmaceutical and clinical preparations.

Solid-state electrochemistry on the nanometer and atomic scales: the scanning probe microscopy approach

Science.gov (United States)

Strelcov, Evgheni; Yang, Sang Mo; Jesse, Stephen; Balke, Nina; Vasudevan, Rama K.; Kalinin, Sergei V.

2016-01-01

Energy technologies of the 21st century require understanding and precise control over ion transport and electrochemistry at all length scales – from single atoms to macroscopic devices. This short review provides a summary of recent works dedicated to methods of advanced scanning probe microscopy for probing electrochemical transformations in solids at the meso-, nano- and atomic scales. Discussion presents advantages and limitations of several techniques and a wealth of examples highlighting peculiarities of nanoscale electrochemistry. PMID:27146961

Activated carbon and single-walled carbon nanotube based electrochemical capacitor in 1 M LiPF{sub 6} electrolyte

Energy Technology Data Exchange (ETDEWEB)

Azam, M.A., E-mail: asyadi@utem.edu.my [Carbon Research Technology Research Group, Faculty of Manufacturing Engineering, Universiti Teknikal Malaysia Melaka, Hang Tuah Jaya, 76100 Durian Tunggal, Melaka (Malaysia); Jantan, N.H.; Dorah, N.; Seman, R.N.A.R.; Manaf, N.S.A. [Carbon Research Technology Research Group, Faculty of Manufacturing Engineering, Universiti Teknikal Malaysia Melaka, Hang Tuah Jaya, 76100 Durian Tunggal, Melaka (Malaysia); Kudin, T.I.T. [Ionics Materials & Devices Research Laboratory, Faculty of Applied Sciences, Universiti Teknologi MARA, Shah Alam, Selangor (Malaysia); Yahya, M.Z.A. [Ionics Materials & Devices Research Laboratory, Faculty of Applied Sciences, Universiti Teknologi MARA, Shah Alam, Selangor (Malaysia); National Defence University of Malaysia, Kem Sungai Besi, 57000 Kuala Lumpur (Malaysia)

2015-09-15

Highlights: • Activated carbon and single-walled CNT based electrochemical capacitor. • Electrochemical analysis by means of CV, charge/discharge and impedance. • 1 M LiPF{sub 6} non-aqueous solution as an electrolyte. • AC/SWCNT electrode exhibits a maximum capacitance of 60.97 F g{sup −1}. - Abstract: Carbon nanotubes have been extensively studied because of their wide range of potential application such as in nanoscale electric circuits, textiles, transportation, health, and the environment. Carbon nanotubes feature extraordinary properties, such as electrical conductivities higher than those of copper, hardness and thermal conductivity higher than those of diamond, and strength surpassing that of steel, among others. This research focuses on the fabrication of an energy storage device, namely, an electrochemical capacitor, by using carbon materials, i.e., activated carbon and single-walled carbon nanotubes, of a specific weight ratio as electrode materials. The electrolyte functioning as an ion carrier is 1 M lithium hexafluorophosphate. Variations in the electrochemical performance of the device, including its capacitance, charge/discharge characteristics, and impedance, are reported in this paper. The electrode proposed in this work exhibits a maximum capacitance of 60.97 F g{sup −1} at a scan rate of 1 mV s{sup −1}.

Electrochemical impedance spectroscopy study of the metal hydride alloy/electrolyte junction

International Nuclear Information System (INIS)

Khaldi, Chokri; Mathlouthi, Hamadi; Lamloumi, Jilani

2009-01-01

The behaviour of the LaNi 3.55 Mn 0.4 Al 0.3 Co 0.75 alloy, used as a negative electrode in the Ni-MH batteries, was studied by the electrochemical impedance spectroscopy (EIS), measured at different potentials. The modeling of the EIS spectra allows us to model the interface electrolyte/Ni-MH electrode by a succession of interfaces electrolyte/corrosion film/alloy particles. The various processes and the physics parameters of each interface are discussed and evaluated. When the potential shifts to more negative values, two reactions are in competition: the hydrogen molecular evolution and the hydrogen atomic absorption. The hydrogen diffuses in the bulk of the alloy and the diffusion is not the limiting factor for the hydrogen absorption.

Passivation Dynamics in the Anisotropic Deposition and Stripping of Bulk Magnesium Electrodes During Electrochemical Cycling.

Science.gov (United States)

Wetzel, David J; Malone, Marvin A; Haasch, Richard T; Meng, Yifei; Vieker, Henning; Hahn, Nathan T; Gölzhäuser, Armin; Zuo, Jian-Min; Zavadil, Kevin R; Gewirth, Andrew A; Nuzzo, Ralph G

2015-08-26

Although rechargeable magnesium (Mg) batteries show promise for use as a next generation technology for high-density energy storage, little is known about the Mg anode solid electrolyte interphase and its implications for the performance and durability of a Mg-based battery. We explore in this report passivation effects engendered during the electrochemical cycling of a bulk Mg anode, characterizing their influences during metal deposition and dissolution in a simple, nonaqueous, Grignard electrolyte solution (ethylmagnesium bromide, EtMgBr, in tetrahydrofuran). Scanning electron microscopy images of Mg foil working electrodes after electrochemical polarization to dissolution potentials show the formation of corrosion pits. The pit densities so evidenced are markedly potential-dependent. When the Mg working electrode is cycled both potentiostatically and galvanostatically in EtMgBr these pits, formed due to passive layer breakdown, act as the foci for subsequent electrochemical activity. Detailed microscopy, diffraction, and spectroscopic data show that further passivation and corrosion results in the anisotropic stripping of the Mg {0001} plane, leaving thin oxide-comprising passivated side wall structures that demark the {0001} fiber texture of the etched Mg grains. Upon long-term cycling, oxide side walls formed due to the pronounced crystallographic anisotropy of the anodic stripping processes, leading to complex overlay anisotropic, columnar structures, exceeding 50 μm in height. The passive responses mediating the growth of these structures appear to be an intrinsic feature of the electrochemical growth and dissolution of Mg using this electrolyte.

Uniform β-Co(OH)2 disc-like nanostructures prepared by low-temperature electrochemical rout as an electrode material for supercapacitors

Science.gov (United States)

Aghazadeh, Mustafa; Shiri, Hamid Mohammad; Barmi, Abbas-Ali Malek

2013-05-01

Uniform nanostructures of cobalt hydroxide were successfully prepared by a low-temperature electrochemical method via galvanostatically deposition from a 0.005 M Co(NO3)3 bath at 10 °C. The XRD and FT-IR analyses showed that the prepared sample has a single crystalline hexagonal phase of the brucite-like Co(OH)2. Morphological characterization by SEM and TEM revealed that the prepared β-Co(OH)2 was composed of uniform compact disc-like nanostructures with diameters of 40-50 nm. The electrochemical performance of the prepared β-Co(OH)2 was evaluated using cyclic voltammetry and charge-discharge tests. A maximum specific capacitance of 736.5 F g-1 was obtained in aqueous 1 M KOH with the potential range of -0.2-0.5 V (vs. Ag/AgCl) at the scan rate of 10 mV s-1, suggesting the potential application of the prepared nanostructures as an electrode material in electrochemical supercapacitors. The results of this work showed that the low-temperature cathodic electrodeposition method can be recognized as a new and facile route for the synthesis of cobalt hydroxide nanodiscs as a promising candidate for the electrochemical supercapacitors.

Electrochemical determination of paraquat in citric fruit based on electrodeposition of silver particles onto carbon paste electrode

OpenAIRE

Abdelfettah Farahi; Mounia Achak; Laila El Gaini; Moulay Abderrahim El Mhammedi; Mina Bakasse

2015-01-01

Carbon paste electrodes (CPEs) modified with silver particles present an interesting tool in the determination of paraquat (PQ) using square wave voltammetry. Metallic silver particle deposits have been obtained via electrochemical deposition in acidic media using cyclic voltammetry. Scanning electron microscopy and X-ray diffraction measurements show that the silver particles are deposited onto carbon surfaces in aggregate form. The response of PQ with modified electrode (Ag-CPE) related to ...

Preparing cuprous oxide nanomaterials by electrochemical method for non-enzymatic glucose biosensor

Science.gov (United States)

Nguyen, Thu-Thuy; Huy, Bui The; Hwang, Seo-Young; Vuong, Nguyen Minh; Pham, Quoc-Thai; Nghia, Nguyen Ngoc; Kirtland, Aaron; Lee, Yong-Ill

2018-05-01

Cuprous oxide (Cu2O) nanostructure has been synthesized using an electrochemical method with a two-electrode system. Cu foils were used as electrodes and NH2(OH) was utilized as the reducing agent. The effects of pH and applied voltages on the morphology of the product were investigated. The morphology and optical properties of Cu2O particles were characterized using scanning electron microscopy, x-ray diffraction, and diffuse reflectance spectra. The synthesized Cu2O nanostructures that formed in the vicinity of the anode at 2 V and pH = 11 showed high uniform distribution, small size, and good electrochemical sensing. These Cu2O nanoparticles were coated on an Indium tin oxide substrate and applied to detect non-enzyme glucose as excellent biosensors. The non-enzyme glucose biosensors exhibited good performance with high response, good selectivity, wide linear detection range, and a low detection limit at 0.4 μM. Synthesized Cu2O nanostructures are potential materials for a non-enzyme glucose biosensor.

Metal-based anode for high performance bioelectrochemical systems through photo-electrochemical interaction

Science.gov (United States)

Liang, Yuxiang; Feng, Huajun; Shen, Dongsheng; Long, Yuyang; Li, Na; Zhou, Yuyang; Ying, Xianbin; Gu, Yuan; Wang, Yanfeng

2016-08-01

This paper introduces a novel composite anode that uses light to enhance current generation and accelerate biofilm formation in bioelectrochemical systems. The composite anode is composed of 316L stainless steel substrate and a nanostructured α-Fe2O3 photocatalyst (PSS). The electrode properties, current generation, and biofilm properties of the anode are investigated. In terms of photocurrent, the optimal deposition and heat-treatment times are found to be 30 min and 2 min, respectively, which result in a maximum photocurrent of 0.6 A m-2. The start-up time of the PSS is 1.2 days and the maximum current density is 2.8 A m-2, twice and 25 times that of unmodified anode, respectively. The current density of the PSS remains stable during 20 days of illumination. Confocal laser scanning microscope images show that the PSS could benefit biofilm formation, while electrochemical impedance spectroscopy indicates that the PSS reduce the charge-transfer resistance of the anode. Our findings show that photo-electrochemical interaction is a promising way to enhance the biocompatibility of metal anodes for bioelectrochemical systems.

Hydrothermal synthesis and electrochemical characterization of VO2 (B) with controlled crystal structures

International Nuclear Information System (INIS)

Jiang Wentao; Ni Juan; Yu Ke; Zhu Ziqiang

2011-01-01

Three different VO 2 (B) nanostructures, including urchin-like VO 2 (B), VO 2 (B) honeycombs and VO 2 (B) nanorods have been successfully fabricated through hydrothermal process by adjusting the concentrations of the oxalic acid. The microstructure and morphology of the VO 2 nanostructures were evaluated by using X-ray diffraction and scanning and transmission electron microscopies. Electrochemical properties measurements of urchin-like VO 2 (B) and VO 2 (B) honeycombs showed excellent cycling performance, especially the urchin-like VO 2 (B) exhibited higher discharge capacity and better capacity retention.

Investigations of AB{sub 5}-type negative electrode for nickel-metal hydride cell with regard to electrochemical and microstructural characteristics

Energy Technology Data Exchange (ETDEWEB)

Srivastava, Sumita [Department of Physics, Govt. P.G. College, Uttarkashi, Uttarakhand 249193 (India); Upadhyay, R.K. [Department of Physics, Govt. P.G. College, Rishikesh 249201 (India)

2010-05-01

In the present investigation, AB{sub 5}-type hydrogen storage alloys with compositions Mm{sub 0.8}La{sub 0.2}Ni{sub 3.7}Al{sub 0.38}Co{sub 0.3}Mn{sub 0.5}Mo{sub 0.02} and Mm{sub 0.75}Ti{sub 0.05}La{sub 0.2}Ni{sub 3.7}Al{sub 0.38}Co{sub 0.3}Mn{sub 0.5}Mo{sub 0.02} are synthesized by radio-frequency induction melting. The electrochemical properties are studied through the measurements of discharge capacity, activation process, rate capability, self-discharge rate and cyclic stability of both the electrodes. Pressure-composition isotherms are plotted by converting the electrode potential into the hydrogen pressure following the Nernst equation. The structural and microstructural characterizations are performed by means of X-ray diffraction phase analysis and scanning electron microscopy of as-fabricated and electrochemically tested electrodes. An attempt is made to correlate the observed electrochemical properties with the structural-microstructural characteristics. (author)

Competitive balance in national European soccer competitions

NARCIS (Netherlands)

Haan, M.A.; Koning, R.H.; van Witteloostuijn, A.; Albert, Jim; Koning, Ruud H.

2007-01-01

According to popular belief, competitive balance in national soccer competitions in Europe has decreased due to the Bosman ruling and the introduction of the Champions League. We test this hypothesis using data from 7 national competitions, for a host of indicators. We find some evidence for

Towards a carbon independent and CO2-free electrochemical membrane process for NH3 synthesis.

Science.gov (United States)

Kugler, K; Ohs, B; Scholz, M; Wessling, M

2014-04-07

Ammonia is exclusively synthesized by the Haber-Bosch process starting from precious carbon resources such as coal or CH4. With H2O, H2 is produced and with N2, NH3 can be synthesized at high pressures and temperatures. Regrettably, the carbon is not incorporated into NH3 but emitted as CO2. Valuable carbon sources are consumed which could be used otherwise when carbon sources become scarce. We suggest an alternative process concept using an electrochemical membrane reactor (ecMR). A complete synthesis process with N2 production and downstream product separation is presented and evaluated in a multi-scale model to quantify its energy consumption. A new micro-scale ecMR model integrates mass, species, heat and energy balances with electrochemical conversions allowing further integration into a macro-scale process flow sheet. For the anodic oxidation reaction H2O was chosen as a ubiquitous H2 source. Nitrogen was obtained by air separation which combines with protons from H2O to give NH3 using a hypothetical catalyst recently suggested from DFT calculations. The energy demand of the whole electrochemical process is up to 20% lower than the Haber-Bosch process using coal as a H2 source. In the case of natural gas, the ecMR process is not competitive under today's energy and resource conditions. In future however, the electrochemical NH3 synthesis might be the technology-of-choice when coal is easily accessible over natural gas or limited carbon sources have to be used otherwise but for the synthesis of the carbon free product NH3.

Noncovalent Pi-Pi Stacking at the Carbon-Electrolyte Interface: Controlling the Voltage Window of Electrochemical Supercapacitors.

Science.gov (United States)

Li, Mengya; Westover, Andrew S; Carter, Rachel; Oakes, Landon; Muralidharan, Nitin; Boire, Timothy C; Sung, Hak-Joon; Pint, Cary L

2016-08-03

A key parameter in the operation of an electrochemical double-layer capacitor is the voltage window, which dictates the device energy density and power density. Here we demonstrate experimental evidence that π-π stacking at a carbon-ionic liquid interface can modify the operation voltage of a supercapacitor device by up to 30%, and this can be recovered by steric hindrance at the electrode-electrolyte interface introduced by poly(ethylene oxide) polymer electrolyte additives. This observation is supported by Raman spectroscopy, electrochemical impedance spectroscopy, and differential scanning calorimetry that each independently elucidates the signature of π-π stacking between imidazole groups in the ionic liquid and the carbon surface and the role this plays to lower the energy barrier for charge transfer at the electrode-electrolyte interface. This effect is further observed universally across two separate ionic liquid electrolyte systems and is validated by control experiments showing an invariant electrochemical window in the absence of a carbon-ionic liquid electrode-electrolyte interface. As interfacial or noncovalent interactions are usually neglected in the mechanistic picture of double-layer capacitors, this work highlights the importance of understanding chemical properties at supercapacitor interfaces to engineer voltage and energy capability.

Effect of Ce addition on the mechanical and electrochemical properties of a lithium battery shell alloy

International Nuclear Information System (INIS)

Zhang, Junchao; Ding, Dongyan; Xu, Xinglong; Gao, Yongjin; Chen, Guozhen; Chen, Weigao; You, Xiaohua; Huang, Yuanwei; Tang, Jinsong

2014-01-01

Highlights: • Fabrication of Ce-free and Ce-containing Al–Cu–Mn–Fe–Mg alloy. • TEM, tensile and electrochemical characterization of the alloys. • Ce element greatly affects the precipitation of the alloy. • Ce element had great impact on the tensile strength and corrosion potential of the alloys. - Abstract: Due to severe application environment lithium battery shell of new-energy automotives requires increasing demands for using high performance aluminum alloys. In the present work, effect of Ce addition on the microstructure, tensile and electrochemical properties of an Al–Cu–Mn–Mg–Fe alloy were investigated through using X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), tensile tests and electrochemical tests. The experimental results indicated that the addition of Ce element could promote the precipitation of second phases. With addition of 0.36% Ce, high melting point Al 8 Cu 4 Ce phase and many Al 20 Cu 2 Mn 3 particles could be found. In addition, the precipitation of conventionally dominant phase of Al 2 Cu could be suppressed in alloy. The Ce addition was found to result in enhanced tensile strength and improved corrosion resistance