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.

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

Imaging by Electrochemical Scanning Tunneling Microscopy and Deconvolution Resolving More Details of Surfaces Nanomorphology

DEFF Research Database (Denmark)

Andersen, Jens Enevold Thaulov

observed in high-resolution images of metallic nanocrystallites may be effectively deconvoluted, as to resolve more details of the crystalline morphology (see figure). Images of surface-crystalline metals indicate that more than a single atomic layer is involved in mediating the tunneling current......Upon imaging, electrochemical scanning tunneling microscopy (ESTM), scanning electrochemical micro-scopy (SECM) and in situ STM resolve information on electronic structures and on surface topography. At very high resolution, imaging processing is required, as to obtain information that relates...... to crystallographic-surface structures. Within the wide range of new technologies, those images surface features, the electrochemical scanning tunneling microscope (ESTM) provides means of atomic resolution where the tip participates actively in the process of imaging. Two metallic surfaces influence ions trapped...

Modelization of the SECM in molten salts environment

International Nuclear Information System (INIS)

Lucas, M.; Slim, C.; Di Caprio, D.; Delpech, S.; Stafiej, J.

2013-01-01

We develop a cellular automata simulation of SECM (Scanning Electrochemical Microscopy)experiments to study corrosion in molten salt media for generation IV nuclear reactors. The electrodes used in these experiments are cylindrical glass tips with a coaxial metal wire inside. As the result of simulations we obtain the current approach curves of the electrodes with geometries characterized by several values of the ratios of glass to metal area at the tip. We compare these results with predictions of the known analytic expressions, solutions of partial differential equations for flat uniform geometry of the substrate. We present also the results for other, more complicated substrate surface geometries e. g. regular saw modulated surface, or surface obtained by an Eden model process. We show that with a simple cellular automata model we can reasonably well simulate the results of SECM setup. The stochastic resolution of the diffusion equations is made possible by the parallel code implemented on GPU

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.

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.

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.

Tunneling Mode of Scanning Electrochemical Microscopy: Probing Electrochemical Processes at Single Nanoparticles.

Science.gov (United States)

Sun, Tong; Wang, Dengchao; Mirkin, Michael V

2018-06-18

Electrochemical experiments at individual nanoparticles (NPs) can provide new insights into their structure-activity relationships. By using small nanoelectrodes as tips in a scanning electrochemical microscope (SECM), we recently imaged individual surface-bound 10-50 nm metal NPs. Herein, we introduce a new mode of SECM operation based on tunneling between the tip and a nanoparticle immobilized on the insulating surface. The obtained current vs. distance curves show the transition from the conventional feedback response to electron tunneling between the tip and the NP at separation distances of less than about 3 nm. In addition to high-resolution imaging of the NP topography, the tunneling mode enables measurement of the heterogeneous kinetics at a single NP without making an ohmic contact with it. The developed method should be useful for studying the effects of nanoparticle size and geometry on electrocatalytic activity in real-world applications. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ultramicrosensors based on transition metal hexacyanoferrates for scanning electrochemical microscopy

Directory of Open Access Journals (Sweden)

Maria A. Komkova

2013-10-01

Full Text Available We report here a way for improving the stability of ultramicroelectrodes (UME based on hexacyanoferrate-modified metals for the detection of hydrogen peroxide. The most stable sensors were obtained by electrochemical deposition of six layers of hexacyanoferrates (HCF, more specifically, an alternating pattern of three layers of Prussian Blue and three layers of Ni–HCF. The microelectrodes modified with mixed layers were continuously monitored in 1 mM hydrogen peroxide and proved to be stable for more than 5 h under these conditions. The mixed layer microelectrodes exhibited a stability which is five times as high as the stability of conventional Prussian Blue-modified UMEs. The sensitivity of the mixed layer sensor was 0.32 A·M−1·cm−2, and the detection limit was 10 µM. The mixed layer-based UMEs were used as sensors in scanning electrochemical microscopy (SECM experiments for imaging of hydrogen peroxide evolution.

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

Directory of Open Access Journals (Sweden)

Sanju Gupta

2015-10-01

Full Text Available 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/ErGO1, (PPy/ErGO1, (PAni/GO1 and (PPy/GO1. 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 (reactivity of surface ion

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

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.

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.

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.

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.

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.

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.

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.

Electrochemical monitoring of intracellular enzyme activity of single living mammalian cells by using a double-mediator system

International Nuclear Information System (INIS)

Matsumae, Yoshiharu; Takahashi, Yasufumi; Ino, Kosuke; Shiku, Hitoshi; Matsue, Tomokazu

2014-01-01

Graphical abstract: NAD(P)H:quinone oxidoreductase (NQO) activity of single HeLa cells were evaluated by using the menadione–ferrocyanide double mediator system combined with scanning electrochemical microscopy (SECM). - Highlights: • NAD(P)H:quinone oxidoreductase activity of single cells were evaluated with SECM. • Fe(CN) 6 3− /menadione concentrations were optimized for long-term SECM monitoring. • Menadione affect the intracellular levels of reactive oxygen species and GSH. • At 100 μM menadione, the Fe(CN) 6 3− generation rate decreased rapidly within 30 min. - Abstract: We evaluated the intracellular NAD(P)H:quinone oxidoreductase (NQO) activity of single HeLa cells by using the menadione–ferrocyanide double-mediator system combined with scanning electrochemical microscopy (SECM). The double-mediator system was used to amplify the current response from the intracellular NQO activity and to reduce menadione-induced cell damage. The electron shuttle between the electrode and menadione was mediated by the ferrocyanide/ferricyanide redox couple. Generation of ferrocyanide was observed immediately after the addition of a lower concentration (10 μM) of menadione. The ferrocyanide generation rate was constant for 120 min. At a higher menadione concentration (100 μM), the ferrocyanide generation rate decreased within 30 min because of the cytotoxic effect of menadione. We also investigated the relationship between intracellular reactive oxygen species or glutathione levels and exposure to different menadione concentrations to determine the optimal condition for SECM with minimal invasiveness. The present study clearly demonstrates that SECM is useful for the analysis of intracellular enzymatic activities in single cells with a double-mediator system

Electrochemical monitoring of intracellular enzyme activity of single living mammalian cells by using a double-mediator system

Energy Technology Data Exchange (ETDEWEB)

Matsumae, Yoshiharu [Graduate School of Environmental Studies, Tohoku University, Aramaki 6-6-11-605, Aoba, Sendai 980-8579 (Japan); Takahashi, Yasufumi [Advanced Institute for Materials Research, Tohoku University, Katahira 2-1-1, Aoba, Sendai 980-8577 (Japan); Ino, Kosuke [Graduate School of Environmental Studies, Tohoku University, Aramaki 6-6-11-605, Aoba, Sendai 980-8579 (Japan); Shiku, Hitoshi, E-mail: shiku@bioinfo.che.tohoku.ac.jp [Graduate School of Environmental Studies, Tohoku University, Aramaki 6-6-11-605, Aoba, Sendai 980-8579 (Japan); Matsue, Tomokazu, E-mail: matsue@bioinfo.che.tohoku.ac.jp [Graduate School of Environmental Studies, Tohoku University, Aramaki 6-6-11-605, Aoba, Sendai 980-8579 (Japan); Advanced Institute for Materials Research, Tohoku University, Katahira 2-1-1, Aoba, Sendai 980-8577 (Japan)

2014-09-09

Graphical abstract: NAD(P)H:quinone oxidoreductase (NQO) activity of single HeLa cells were evaluated by using the menadione–ferrocyanide double mediator system combined with scanning electrochemical microscopy (SECM). - Highlights: • NAD(P)H:quinone oxidoreductase activity of single cells were evaluated with SECM. • Fe(CN){sub 6}{sup 3−}/menadione concentrations were optimized for long-term SECM monitoring. • Menadione affect the intracellular levels of reactive oxygen species and GSH. • At 100 μM menadione, the Fe(CN){sub 6}{sup 3−} generation rate decreased rapidly within 30 min. - Abstract: We evaluated the intracellular NAD(P)H:quinone oxidoreductase (NQO) activity of single HeLa cells by using the menadione–ferrocyanide double-mediator system combined with scanning electrochemical microscopy (SECM). The double-mediator system was used to amplify the current response from the intracellular NQO activity and to reduce menadione-induced cell damage. The electron shuttle between the electrode and menadione was mediated by the ferrocyanide/ferricyanide redox couple. Generation of ferrocyanide was observed immediately after the addition of a lower concentration (10 μM) of menadione. The ferrocyanide generation rate was constant for 120 min. At a higher menadione concentration (100 μM), the ferrocyanide generation rate decreased within 30 min because of the cytotoxic effect of menadione. We also investigated the relationship between intracellular reactive oxygen species or glutathione levels and exposure to different menadione concentrations to determine the optimal condition for SECM with minimal invasiveness. The present study clearly demonstrates that SECM is useful for the analysis of intracellular enzymatic activities in single cells with a double-mediator system.

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.

Development of scanning electrochemical microscopy for the investigation of photocatalysis at semiconductor surfaces

International Nuclear Information System (INIS)

Fonseca, Sofia Margarida Martins Costa da

2002-01-01

This thesis is concerned with the development and application of scanning electrochemical microscopy (SECM) to investigate interfacial photoelectrochemical processes occurring at supported TiO 2 surfaces. The new SECM approach, involving both amperometric and potentiometric electrodes, was used to monitor interfacial photoprocesses with high spatial resolution. A new in situ photoelectrochemical approach to chemical actinometry has been developed and used to determine the light flux through a quartz fibre employed in the SECM system. In this system an ultramicroelectrode (UME) probe is positioned with high precision at a known distance close to a TiO 2 -coated fibre and used to detect reactants or products of the ongoing photodegradation process. The microelectrochemical actinometry approach was developed using the well-known liquid phase potassium ferrioxalate actinometer. The approach involved recording the steady-state current for Fe(lll) reduction at an SECM tip positioned close to the fibre. A step function in the light flux (off-on) was then applied and the resulting chronoamperometric behaviour due to the reduction of Fe(lll) at the UME was recorded as a function of tip-fibre separation distance. A theoretical model has been developed to simulate experimental current-time profiles, which allowed the light flux through the quartz fibre to be quantified. An experimental approach to investigating the photoelectrochemical reduction of oxygen at UV-illuminated TiO 2 surfaces, in aqueous aerated and oxygenated electrolyte solutions, in the absence and presence of hole scavengers, has been developed. In this new approach the chronoamperometric behaviour for oxygen reduction was recorded at an UME tip after stepping the light flux at a back-illuminated TiO 2 film on and off. The kinetics of the reduction process were interpreted through various theoretical models proposed in the literature. This experimental approach demonstrated a significant depletion of the

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.

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 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.

A study of ion exchange at the poly(butyl viologen)-electrolyte interface by SECM

Energy Technology Data Exchange (ETDEWEB)

Hsu, Chih-Yu.; Vasantha, V.S. [Department of Chemical Engineering, National Taiwan University, Taipei 10617 (China); Ho, Kuo-Chuan [Department of Chemical Engineering, National Taiwan University, Taipei 10617 (China); Institute of Polymer Science and Engineering, National Taiwan University, Taipei 10617 (China)

2008-09-01

In this work, the ion exchange characteristics of poly(butyl viologen) (PBV) thin films on a platinum electrode has been investigated by cyclic voltammetric (CV) scans. Since ferrocyanide anions (Fe(CN){sub 6}{sup 4-}) were added during the polymerization of the PBV thin-film for its stability, Fe(CN){sub 6}{sup 4-} could form charge transfer complex with monomer and co-deposited with polymer. Scanning electrochemical microscopy (SECM) was used to probe the released Fe(CN){sub 6}{sup 4-} ions from PBV film with Os(bpy){sub 3}Cl{sub 2} as a mediator for the approaching process in 0.5 M KCl medium. Mass changes during the redox process of the film were also monitored in-situ by electrochemical quartz crystal microbalance (EQCM). The ion exchange and transport behavior was observed during CV cycling of the film of the SECM and EQCM. The insertion and extraction of anions were found to be potential-dependence. Moreover, the decrease in tip current of released Fe(CN){sub 6}{sup 4-} with increasing cycle number accounted for the ion exchange between Fe(CN){sub 6}{sup 4-} and Cl{sup -} in the KCl electrolyte. However, the Fe(CN){sub 6}{sup 4-}/Fe(CN){sub 6}{sup 3-} redox couple was found to be highly stable between 0.0 and 0.5 V (vs. Ag/AgCl/saturated KCl) in the phosphate buffer solution. Therefore, the electrochemical property of Fe(CN){sub 6}{sup 4-}/Fe(CN){sub 6}{sup 3-} redox couple was studied at different scan rates using CV technique. The peak currents were directly proportional to the scan rate as predicted for a surface confined diffusionless system. The surface coverage ({gamma}) and the concentration of Fe(CN){sub 6}{sup 4-} were determined to be 1.88 x 10{sup -8} mol/cm{sup 2} and 0.641 mol/dm{sup 3}, respectively. By neglecting cations incorporation during redox reaction of the PBV film and also based on the results obtained from energy-dispersive X-ray spectroscopy for the films of as-deposited, reduced and oxidized states, an ion exchange mechanism was

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.

Inhibition of the MRP1-mediated transport of the menadione-glutathione conjugate (thiodione) in HeLa cells as studied by SECM.

Science.gov (United States)

Koley, Dipankar; Bard, Allen J

2012-07-17

Oxidative stress induced in live HeLa cells by menadione (2-methyl-1,4-napthaquinone) was studied in real time by scanning electrochemical microscopy (SECM). The hydrophobic molecule menadione diffuses through a living cell membrane where it is toxic to the cell. However, in the cell it is conjugated with glutathione to form thiodione. Thiodione is then recognized and transported across the cell membrane via the ATP-driven MRP1 pump. In the extracellular environment, thiodione was detected by the SECM tip at levels of 140, 70, and 35 µM upon exposure of the cells to menadione concentrations of 500, 250, and 125 µM, respectively. With the aid of finite element modeling, the kinetics of thiodione transport was determined to be 1.6 10(-7) m/s, about 10 times faster than menadione uptake. Selective inhibition of these MRP1 pumps inside live HeLa cells by MK571 produced a lower thiodione concentration of 50 µM in presence of 500 µM menadione and 50 µM MK571. A similar reduced (50% drop) thiodione efflux was observed in the presence of monoclonal antibody QCRL-4, a selective blocking agent of the MRP1 pumps. The reduced thiodione flux confirmed that thiodione was transported by MRP1, and that glutathione is an essential substrate for MRP1-mediated transport. This finding demonstrates the usefulness of SECM in quantitative studies of MRP1 inhibitors and suggests that monoclonal antibodies can be a useful tool in inhibiting the transport of these MDR pumps, and thereby aiding in overcoming multidrug resistance.

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.

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

Development of electrochemical reporter assay using HeLa cells transfected with vector plasmids encoding various responsive elements

Energy Technology Data Exchange (ETDEWEB)

Shiku, Hitoshi, E-mail: shiku@bioinfo.che.tohoku.ac.jp [Graduate School of Environmental Studies, Tohoku University, 6-6-11-604 Aramaki-Aoba, Sendai 980-8579 (Japan); Takeda, Michiaki; Murata, Tatsuya [Graduate School of Environmental Studies, Tohoku University, 6-6-11-604 Aramaki-Aoba, Sendai 980-8579 (Japan); Akiba, Uichi; Hamada, Fumio [Graduate School of Engineering and Resource Science, Akita University, 1-1 Tegata gakuen-machi, Akita 010-8502 (Japan); Matsue, Tomokazu, E-mail: matsue@bioinfo.che.tohoku.ac.jp [Graduate School of Environmental Studies, Tohoku University, 6-6-11-604 Aramaki-Aoba, Sendai 980-8579 (Japan)

2009-04-27

Electrochemical assay using HeLa cell lines transfected with various plasmid vectors encoding SEAP (secreted alkaline phosphatase) as the reporter has been performed by using SECM (scanning electrochemical microscopy). The plasmid vector contains different responsive elements that include GRE (glucocorticoid response elements), CRE (cAMP responsive elements), or {kappa}B (binding site for NF{kappa}B (nuclear factor kappa B)) upstream of the SEAP sequence. The transfected HeLa cells were patterned on a culture dish in a 4 x 4 array of circles of diameter 300 {mu}m by using the PDMS (poly(dimethylsiloxane)) stencil technique. The cellular array was first exposed to 100 ng mL{sup -1} dexamethasone, 10 ng mL{sup -1} forskolin, or 100 ng mL{sup -1} TNF-{alpha} (tumor necrosis factor {alpha}) after which it was further cultured in an RPMI culture medium for 6 h. After incubation, the cellular array was soaked in a measuring solution containing 4.7 mM PAPP (p-aminophenylphosphate) at pH 9.5, following which electrochemical measurements were performed immediately within 40 min. The SECM method allows parallel evaluation of different cell lines transfected with pGRE-SEAP, pCRE-SEAP, and pNF{kappa}B-SEAP patterned on the same solid support for detection of the oxidation current of PAP (p-aminophenol) flux produced from only 300 HeLa cells in each stencil pattern. The results of the SECM method were highly sensitive as compared to those obtained from the conventional CL (chemiluminescence) protocol with at least 5 x 10{sup 4} cells per well.

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

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.

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.

Study of the ion-channel behavior on glassy carbon electrode supported bilayer lipid membranes stimulated by perchlorate anion

Energy Technology Data Exchange (ETDEWEB)

Zhang, Zhiquan; Shi, Jun; Huang, Weimin, E-mail: huangwm@jlu.edu.cn

2015-10-01

In this paper, a kind of didodecyldimethylammonium bromide (DDAB) layer membranes was supported on a glassy carbon electrode (GCE). We studied the ion channel behavior of the supported bilayer lipid membrane by scanning electrochemical microscopy (SCEM) in tris(2,2′-bipyridine) ruthenium(II) solution. Perchlorate anion was used as a presence of stimulus and ruthenium(II) complex cations as the probing ions for the measurement of SECM, the lipid membrane channel was opened and exhibited the behavior of distinct SECM positive feedback curve. The channel was in a closed state in the absence of perchlorate anions while reflected the behavior of SECM negative feedback curve. The rates of electron transfer reaction in the lipid membranes surface were detected and it was dependant on the potential of SECM. - Highlights: • The rates of electron transfer reaction in the lipid membranes surface were detected. • Dynamic investigations of ion-channel behavior of supported bilayer lipid membranes by scanning electrochemical microscopy • A novel way to explore the interaction between molecules and supported bilayer lipid membranes.

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...

Kelvin probe force microscopy in liquid using electrochemical force microscopy

Directory of Open Access Journals (Sweden)

Liam Collins

2015-01-01

Full Text Available Conventional closed loop-Kelvin probe force microscopy (KPFM has emerged as a powerful technique for probing electric and transport phenomena at the solid–gas interface. The extension of KPFM capabilities to probe electrostatic and electrochemical phenomena at the solid–liquid interface is of interest for a broad range of applications from energy storage to biological systems. However, the operation of KPFM implicitly relies on the presence of a linear lossless dielectric in the probe–sample gap, a condition which is violated for ionically-active liquids (e.g., when diffuse charge dynamics are present. Here, electrostatic and electrochemical measurements are demonstrated in ionically-active (polar isopropanol, milli-Q water and aqueous NaCl and ionically-inactive (non-polar decane liquids by electrochemical force microscopy (EcFM, a multidimensional (i.e., bias- and time-resolved spectroscopy method. In the absence of mobile charges (ambient and non-polar liquids, KPFM and EcFM are both feasible, yielding comparable contact potential difference (CPD values. In ionically-active liquids, KPFM is not possible and EcFM can be used to measure the dynamic CPD and a rich spectrum of information pertaining to charge screening, ion diffusion, and electrochemical processes (e.g., Faradaic reactions. EcFM measurements conducted in isopropanol and milli-Q water over Au and highly ordered pyrolytic graphite electrodes demonstrate both sample- and solvent-dependent features. Finally, the feasibility of using EcFM as a local force-based mapping technique of material-dependent electrostatic and electrochemical response is investigated. The resultant high dimensional dataset is visualized using a purely statistical approach that does not require a priori physical models, allowing for qualitative mapping of electrostatic and electrochemical material properties at the solid–liquid interface.

Menadione metabolism to thiodione in hepatoblastoma by scanning electrochemical microscopy

Science.gov (United States)

Mauzeroll, Janine; Bard, Allen J.; Owhadian, Omeed; Monks, Terrence J.

2004-01-01

The cytotoxicity of menadione on hepatocytes was studied by using the substrate generation/tip collection mode of scanning electrochemical microscopy by exposing the cells to menadione and detecting the menadione-S-glutathione conjugate (thiodione) that is formed during the cellular detoxication process and is exported from the cell by an ATP-dependent pump. This efflux was electrochemically detected and allowed scanning electrochemical microscopy monitoring and imaging of single cells and groups of highly confluent live cells. Based on a constant flux model, ≈6 × 106 molecules of thiodione per cell per second are exported from monolayer cultures of Hep G2 cells. PMID:15601769

Establishing the SECME model in the District of Columbia. Quarterly report, 1 January 1994--31 March 1994

Energy Technology Data Exchange (ETDEWEB)

Vikers, R.G.

1994-05-01

During this quarter, many program activities were held to help SECME teachers and counselors implement, improve and strengthen SECME school programs in the District of Columbia. Teachers were actively engaged in enhanced instructional techniques, ideas, processes and resources to help them enrich their students` learning experience. Students are busily participating in hands-on instructional activities and preparing for the SECME competition where they are learning to excel in a competitive environment designed to help them make the most of their school experience.

1993-1994 Final technical report for establishing the SECME Model in the District of Columbia

Energy Technology Data Exchange (ETDEWEB)

Vickers, R.G.

1995-12-31

This is the final report for a program to establish the SECME Model in the District of Columbia. This program has seen the development of a partnership between the District of Columbia Public Schools, the University of the District of Columbia, the Department of Energy, and SECME. This partnership has demonstrated positive achievement in mathematics and science education and learning in students within the District of Columbia.

1993-1994 Final technical report for establishing the SECME Model in the District of Columbia

International Nuclear Information System (INIS)

Vickers, R.G.

1995-01-01

This is the final report for a program to establish the SECME Model in the District of Columbia. This program has seen the development of a partnership between the District of Columbia Public Schools, the University of the District of Columbia, the Department of Energy, and SECME. This partnership has demonstrated positive achievement in mathematics and science education and learning in students within the District of Columbia

Porphyrins as Corrosion Inhibitors for N80 Steel in 3.5% NaCl Solution: Electrochemical, Quantum Chemical, QSAR and Monte Carlo Simulations Studies

Directory of Open Access Journals (Sweden)

Ambrish Singh

2015-08-01

Full Text Available The inhibition of the corrosion of N80 steel in 3.5 wt. % NaCl solution saturated with CO2 by four porphyrins, namely 5,10,15,20-tetrakis(4-hydroxyphenyl-21H,23H-porphyrin (HPTB, 5,10,15,20-tetra(4-pyridyl-21H,23H-porphyrin (T4PP, 4,4′,4″,4‴-(porphyrin-5,10,15,20-tetrayltetrakis(benzoic acid (THP and 5,10,15,20-tetraphenyl-21H,23H-porphyrin (TPP was studied using electrochemical impedance spectroscopy (EIS, potentiodynamic polarization, scanning electrochemical microscopy (SECM and scanning electron microscopy (SEM techniques. The results showed that the inhibition efficiency, η% increases with increasing concentration of the inhibitors. The EIS results revealed that the N80 steel surface with adsorbed porphyrins exhibited non-ideal capacitive behaviour with reduced charge transfer activity. Potentiodynamic polarization measurements indicated that the studied porphyrins acted as mixed type inhibitors. The SECM results confirmed the adsorption of the porphyrins on N80 steel thereby forming a relatively insulated surface. The SEM also confirmed the formation of protective films of the porphyrins on N80 steel surface thereby protecting the surface from direct acid attack. Quantum chemical calculations, quantitative structure activity relationship (QSAR were also carried out on the studied porphyrins and the results showed that the corrosion inhibition performances of the porphyrins could be related to their EHOMO, ELUMO, ω, and μ values. Monte Carlo simulation studies showed that THP has the highest adsorption energy, while T4PP has the least adsorption energy in agreement with the values of σ from quantum chemical calculations.

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.

AFSC/ABL: Southeast Coastal Monitoring Survey (SECM)-juvenile salmon and associated epipelagic ichthyofauna in the marine waters of Southeast Alaska

Data.gov (United States)

National Oceanic and Atmospheric Administration, Department of Commerce — SECM research was initiated in the spring of 1997, just prior to the onset of a strong El Nio event, and has continued annually. SECM sampling occurs around Icy...

Carbon-Based Solid-State Calcium Ion-Selective Microelectrode and Scanning Electrochemical Microscopy: A Quantitative Study of pH-Dependent Release of Calcium Ions from Bioactive Glass.

Science.gov (United States)

Ummadi, Jyothir Ganesh; Downs, Corey J; Joshi, Vrushali S; Ferracane, Jack L; Koley, Dipankar

2016-03-15

Solid-state ion-selective electrodes are used as scanning electrochemical microscope (SECM) probes because of their inherent fast response time and ease of miniaturization. In this study, we report the development of a solid-state, low-poly(vinyl chloride), carbon-based calcium ion-selective microelectrode (Ca(2+)-ISME), 25 μm in diameter, capable of performing an amperometric approach curve and serving as a potentiometric sensor. The Ca(2+)-ISME has a broad linear response range of 5 μM to 200 mM with a near Nernstian slope of 28 mV/log[a(Ca(2+))]. The calculated detection limit for Ca(2+)-ISME is 1 μM. The selectivity coefficients of this Ca(2+)-ISME are log K(Ca(2+),A) = -5.88, -5.54, and -6.31 for Mg(2+), Na(+), and K(+), respectively. We used this new type of Ca(2+)-ISME as an SECM probe to quantitatively map the chemical microenvironment produced by a model substrate, bioactive glass (BAG). In acidic conditions (pH 4.5), BAG was found to increase the calcium ion concentration from 0.7 mM ([Ca(2+)] in artificial saliva) to 1.4 mM at 20 μm above the surface. In addition, a solid-state dual SECM pH probe was used to correlate the release of calcium ions with the change in local pH. Three-dimensional pH and calcium ion distribution mapping were also obtained by using these solid-state probes. The quantitative mapping of pH and Ca(2+) above the BAG elucidates the effectiveness of BAG in neutralizing and releasing calcium ions in acidic conditions.

Corrosion mitigation of J55 steel in 3.5% NaCl solution by a macrocyclic inhibitor

Energy Technology Data Exchange (ETDEWEB)

Singh, Ambrish [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); Obot, I.B. [Centre of Research Excellence in Corrosion, Research Institute, King Fahd University of Petroleum and Minerals, Dhahran 31261 (Saudi Arabia); Ebenso, Eno E. [Department of Chemistry, School of Mathematical & Physical Sciences, North-West University (Mafikeng Campus), Private Bag X2046, Mmabatho 2735 (South Africa); Material Science Innovation & Modelling (MaSIM) Focus Area, Faculty of Agriculture, Science and Technology, North-West University (Mafikeng Campus), Private Bag X2046, Mmabatho 2735 (South Africa); Ansari, K.R.; Quraishi, M.A. [Department of Applied Chemistry, Indian Institute of Technology, Banaras Hindu University, Varanasi 221005, Uttar Pradesh (India)

2015-11-30

Graphical abstract: SECM studies revealed decrease of steady current in the presence of inhibitor while it increased for 3.5% NaCl solution that acted as the conductor. - Highlights: • J55 steel protection in 3.5% NaCl solution saturated with CO{sub 2} by HPT. • Potentiodynamic polarization curves reveal that the actions of HPT are mixed type. • The adsorption of HPT obeys the Langmuir adsorption isotherm. • Scanning electrochemical microscopy is used to discuss the insulated and conductive surface. - Abstract: 1,2,4,7,9,10-Hexaazacyclo-pentadeca-10,15-dien-3,5,6,8-tetraone (HPT) a macrocyclic compound has been studied using electrochemical methods and scanning electrochemical microscopy (SECM) techniques. The R{sub ct} values increased and C{sub dl} values decreased with the increase in concentration of the inhibitor. The corrosion inhibition of J55 steel in 3.5 wt.% NaCl solution saturated with CO{sub 2} by polarization studies revealed that HPT acted as a mixed type inhibitor. The adsorption of HPT on the J55 steel surface obeyed the Langmuir adsorption isotherm. The thermodynamic parameters (K{sub ads}, ΔG°{sub ads}) were also computed and discussed.

Corrosion mitigation of J55 steel in 3.5% NaCl solution by a macrocyclic inhibitor

International Nuclear Information System (INIS)

Singh, Ambrish; Lin, Yuanhua; Obot, I.B.; Ebenso, Eno E.; Ansari, K.R.; Quraishi, M.A.

2015-01-01

Graphical abstract: SECM studies revealed decrease of steady current in the presence of inhibitor while it increased for 3.5% NaCl solution that acted as the conductor. - Highlights: • J55 steel protection in 3.5% NaCl solution saturated with CO 2 by HPT. • Potentiodynamic polarization curves reveal that the actions of HPT are mixed type. • The adsorption of HPT obeys the Langmuir adsorption isotherm. • Scanning electrochemical microscopy is used to discuss the insulated and conductive surface. - Abstract: 1,2,4,7,9,10-Hexaazacyclo-pentadeca-10,15-dien-3,5,6,8-tetraone (HPT) a macrocyclic compound has been studied using electrochemical methods and scanning electrochemical microscopy (SECM) techniques. The R ct values increased and C dl values decreased with the increase in concentration of the inhibitor. The corrosion inhibition of J55 steel in 3.5 wt.% NaCl solution saturated with CO 2 by polarization studies revealed that HPT acted as a mixed type inhibitor. The adsorption of HPT on the J55 steel surface obeyed the Langmuir adsorption isotherm. The thermodynamic parameters (K ads , ΔG° ads ) were also computed and discussed.

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 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.

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.

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

Chemical, electrical and electrochemical characterization of hybrid organic/inorganic polypyrrole/PW{sub 12}O{sub 40}{sup 3-} coating deposited on polyester fabrics

Energy Technology Data Exchange (ETDEWEB)

Molina, J.; Fernandez, J.; Rio, A.I. del; Bonastre, J. [Departamento de Ingenieria Textil y Papelera, EPS de Alcoy, Universitat Politecnica de Valencia, Plaza Ferrandiz y Carbonell s/n, 03801 Alcoy (Spain); Cases, F., E-mail: fjcases@txp.upv.es [Departamento de Ingenieria Textil y Papelera, EPS de Alcoy, Universitat Politecnica de Valencia, Plaza Ferrandiz y Carbonell s/n, 03801 Alcoy (Spain)

2011-09-15

A study of the stability of conducting fabrics of polyester (PES) coated with polypyrrole/PW{sub 12}O{sub 40}{sup 3-} (organic/inorganic hybrid material) in different pH solutions (1, 7, 13) has been done. Washing tests were also done in views of its possible application in electronic textiles such as antistatic clothing. X-ray photoelectron spectroscopy (XPS) studies have been done to quantify the amount of counter ion that remains in the polymer matrix and determine the doping ratio (N{sup +}/N) after the different tests. Scanning electron microscopy (SEM) was also used to observe morphological differences after the different tests. Surface resistivity changes were measured by means of electrochemical impedance spectroscopy (EIS). Scanning electrochemical microscopy (SECM) was employed to measure changes in electroactivity after the different tests. Higher pHs caused a decrease of the doping ratio (N{sup +}/N), the loss of part of the counter ions and the decrease of its conducting and electrocatalytic properties. The stability in acid media and neutral media and after the washing test was good. Only at pH 13 the loss of the counter ion was widespread and there was a decrease of its conducting and catalytic properties; although the fabrics continued acting mainly as a conducting material.

Electrocatalytic activity mapping of model fuel cell catalyst films using scanning electrochemical microscopy

International Nuclear Information System (INIS)

Nicholson, P.G.; Zhou, S.; Hinds, G.; Wain, A.J.; Turnbull, A.

2009-01-01

Scanning electrochemical microscopy has been employed to spatially map the electrocatalytic activity of model proton exchange membrane fuel cell (PEMFC) catalyst films towards the hydrogen oxidation reaction (the PEMFC anode reaction). The catalyst films were composed of platinum-loaded carbon nanoparticles, similar to those typically used in PEMFCs. The electrochemical characterisation was correlated with a detailed physical characterisation using dynamic light scattering, transmission electron microscopy and field-emission scanning electron microscopy. The nanoparticles were found to be reasonably mono-dispersed, with a tendency to agglomerate into porous bead-type structures when spun-cast. The number of carbon nanoparticles with little or no platinum was surprisingly higher than would be expected based on the platinum-carbon mass ratio. Furthermore, the platinum-rich carbon particles tended to agglomerate and the clusters formed were non-uniformly distributed. This morphology was reflected in a high degree of heterogeneity in the film activity towards the hydrogen oxidation reaction.

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

A glassy carbon electrode modified with an iron N4-macrocycle and reduced graphene oxide for voltammetric sensing of dissolved oxygen

International Nuclear Information System (INIS)

Silva, Saimon M.; Aguiar, Lucas F.; Carvalho, Rita M. S.; Tanaka, Auro A.; Damos, Flavio S.; Luz, Rita C. S.

2016-01-01

The authors describe a platform for the electrochemical reduction of oxygen. It is based on the use of a glassy carbon electrode (GCE) that was modified in a single-step microwave assisted reaction with a N4-macrocycle containing iron(III) (FeN4) and with reduced graphene oxide. The FeN4/rGO composite was characterized by cyclic voltammetry, differential pulse voltammetry, and scanning electrochemical microscopy (SECM). Cyclic voltammetry showed the composite to enable efficient reduction of O_2 at a very low overpotential (−0.05 V vs. Ag/AgCl). SECM measurements were carried out to map (in the redox competition mode) the activity of a GCE microelectrode modified with FeN4/rGO. Under optimized conditions, the response to dissolved O_2 ranges from 0.8 up to 25 mg⋅L"-"1, and the limit of detection is 0.2 mg⋅L"-"1. (author)

Single-step electrochemical method for producing very sharp Au scanning tunneling microscopy tips

International Nuclear Information System (INIS)

Gingery, David; Buehlmann, Philippe

2007-01-01

A single-step electrochemical method for making sharp gold scanning tunneling microscopy tips is described. 3.0M NaCl in 1% perchloric acid is compared to several previously reported etchants. The addition of perchloric acid to sodium chloride solutions drastically shortens etching times and is shown by transmission electron microscopy to produce very sharp tips with a mean radius of curvature of 15 nm

Electrocatalytic reduction of nitrite on tetraruthenated metalloporphyrins/Nafion glassy carbon modified electrode

Energy Technology Data Exchange (ETDEWEB)

Calfuman, Karla [Facultad de Ciencias, Departamento de Quimica, Universidad de Chile, Las Palmeras 3425, Casilla 653, Nunoa, Santiago (Chile); Aguirre, Maria Jesus [Facultad de Quimica y Biologia, Departamento de Quimica de los Materiales, Universidad de Santiago de Chile, Santiago (Chile); Canete-Rosales, Paulina; Bollo, Soledad [Facultad de Ciencias Quimicas y Farmaceuticas, Departamento de Quimica Farmacologica y Toxicologica, Universidad de Chile, Santiago (Chile); Llusar, Rosa [Departamento de Quimica Fisica y Analitica, Universidad de Jaume I, Castellon (Spain); Isaacs, Mauricio, E-mail: misaacs@uchile.cl [Facultad de Ciencias, Departamento de Quimica, Universidad de Chile, Las Palmeras 3425, Casilla 653, Nunoa, Santiago (Chile)

2011-10-01

Highlights: > Preparation and characterization of modified electrodes with M(II) Tetraruthenated porphyrins onto a Nafion film. > The electrodes were characterized by SEM, TEM, AFM and SECM techniques. > The modified electrodes are active in the electrochemical reduction of nitrite at -660 mV vs Ag/AgCl. > GC/Nf/CoTRP modified electrode is more electrochemically active than their Ni and Zn analogues. - Abstract: This paper describes the electrochemical reduction of nitrite ion in neutral aqueous solution mediated by tetraruthenated metalloporphyrins (Co(II), Ni(II) and Zn(II)) electrostatically assembled onto a Nafion film previously adsorbed on glassy carbon or ITO electrodes. Scanning electron microscope (SEM-EDX) and transmission electron microscopy (TEM) results have shown that on ITO electrodes the macrocycles forms multiple layers with a disordered stacking orientation over the Nafion film occupying hydrophobic and hydrophilic sites in the polyelectrolyte. Atomic force microscopy (AFM) results demonstrated that the Nafion film is 35 nm thick and tetraruthenated metalloporphyrins layers 190 nm thick presenting a thin but compacted morphology. Scanning electrochemical microscopy (SECM) images shows that the Co(II) tetraruthenated porphyrins/Nf/GC modified electrode is more electrochemically active than their Ni and Zn analogues. These modified electrodes are able to reduce nitrite at -660 mV showing enhanced reduction current and a decrease in the required overpotential compared to bare glassy carbon electrode. Controlled potential electrolysis experiments verify the production of ammonia, hydrazine and hydroxylamine at potentials where reduction of solvent is plausible demonstrating some selectivity toward the nitrite ion. Rotating disc electrode voltammetry shows that the factor that governs the kinetics of nitrite reduction is the charge propagation in the film.

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.

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.

Scanning electrochemical microscopy of menadione-glutathione conjugate export from yeast cells

Science.gov (United States)

Mauzeroll, Janine; Bard, Allen J.

2004-01-01

The uptake of menadione (2-methyl-1,4-naphthoquinone), which is toxic to yeast cells, and its expulsion as a glutathione complex were studied by scanning electrochemical microscopy. The progression of the in vitro reaction between menadione and glutathione was monitored electrochemically by cyclic voltammetry and correlated with the spectroscopic (UV–visible) behavior. By observing the scanning electrochemical microscope tip current of yeast cells suspended in a menadione-containing solution, the export of the conjugate from the cells with time could be measured. Similar experiments were performed on immobilized yeast cell aggregates stressed by a menadione solution. From the export of the menadione-glutathione conjugate detected at a 1-μm-diameter electrode situated 10 μm from the cells, a flux of about 30,000 thiodione molecules per second per cell was extracted. Numerical simulations based on an explicit finite difference method further revealed that the observation of a constant efflux of thiodione from the cells suggested the rate was limited by the uptake of menadione and that the efflux through the glutathione-conjugate pump was at least an order of magnitude faster. PMID:15148374

Development of novel tungsten processing technologies for electro-chemical machining (ECM) of plasma facing components

International Nuclear Information System (INIS)

Holstein, Nils; Krauss, Wolfgang; Konys, Juergen

2011-01-01

Plasma facing components for fusion applications must exhibit long-term stability under extreme conditions, and therefore material imperfections cannot be tolerated due to a high risk of technical failures. To prevent or abolish defects in refractory metals components during the manufacturing process, some methods of electro-chemical machining as S-ECM and C-ECM were developed, enabling both the processing of smooth plain defect-free surfaces of different geometry and the removal of bulk material for the shaping of three-dimensional structures, also without cracks. It is discussed, that tungsten ablation with accurate electro-chemical molding is very sensitive to the kind of electric current, and therefore current investigations focused also on the effects of frequency profiles on the sharpness of edge rounding.

Effects of solution viscosity on heterogeneous electron transfer across a liquid/liquid interface

Energy Technology Data Exchange (ETDEWEB)

Bai Yamin; Sun Peng; Zhang Meiqin; Gao Zhao; Yang Zhengyu; Shao Yuanhua

2003-10-15

Scanning electrochemical microscopy (SECM) is employed to investigate the effect of solution viscosity on the rate constants of electron transfer (ET) reaction between potassium ferricyanide in water and 7,7,8,8-tetracyanoquinodimethane (TCNQ) in 1,2-dichloroethane. Either tetrabutylammonium (TBA{sup +}) or ClO{sub 4}{sup -} is chosen as the common ion in both phases to control the interfacial potential drop. The rate constant of heterogeneous ET reaction between TCNQ and ferrocyanide produced in-situ, k{sub 12}, is evaluated by SECM and is inversely proportional to the viscosity of the aqueous solution and directly proportional to the diffusion coefficient of K{sub 4}Fe(CN){sub 6} in water when the concentration of TCNQ in the DCE phase is in excess. The k{sub 12} dependence on viscosity is explained in terms of the longitudinal relaxation time of the solution. The rate constant of the heterogeneous ET reaction between TCNQ{sup -} and ferricyanide, k{sub 21}, is also obtained by SECM and these results cannot be explained by the same manner.

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 activation of Li2MnO3 at elevated temperature investigated by in situ Raman microscopy

International Nuclear Information System (INIS)

Lanz, Patrick; Villevieille, Claire; Novák, Petr

2013-01-01

Layered-layered oxides of the type xLi 2 MnO 3 ·(1 − x)LiMO 2 (M = Mn, Ni, Co) have been postulated to contain Li 2 MnO 3 domains which, upon electrochemical activation, give rise to a characteristic potential plateau at 4.5 V vs. Li + /Li. To improve our understanding of the complex reaction mechanisms at play, we applied in situ Raman microscopy to investigate the constituent Li 2 MnO 3 . Li 2 MnO 3 synthesised via a two-step solid-state reaction was characterised by scanning electron microscopy and X-ray diffraction. Preliminary electrochemical tests and ex situ Raman microscopy showed the need for elevated temperatures to achieve activation. For the first time, in situ Raman microscopy (at 50 °C) confirmed the activation of Li 2 MnO 3 . The main signal at 615 cm −1 shifted to higher wavenumbers upon charging. After reaching 4.4 V vs. Li + /Li, this shift grew significantly, which is in good agreement with the onset of the potential plateau in both Li 2 MnO 3 and xLi 2 MnO 3 ·(1 − x)LiMO 2 , and is assigned to the partial formation of a spinel-like phase

In Situ Formation of Decavanadate-Intercalated Layered Double Hydroxide Films on AA2024 and their Anti-Corrosive Properties when Combined with Hybrid Sol Gel Films

Directory of Open Access Journals (Sweden)

Junsheng Wu

2017-04-01

Full Text Available A layered double hydroxide (LDH film was formed in situ on aluminum alloy 2024 through a urea hydrolysis method, and a decavanadate-intercalated LDH (LDH-V film fabricated through the dip coating method. The microstructural and morphological characteristics were investigated by scanning electron microscopy (SEM. The corrosion-resistant performance was analyzed by electrochemical impedance spectroscopy (EIS, scanning electrochemical microscopy (SECM, and a salt-spray test (SST.The SEM results showed that a complete and defect-free surface was formed on the LDH-VS film. The anticorrosion results revealed that the LDH-VS film had better corrosion-resistant properties than the LDH-S film, especially long-term corrosion resistance. The mechanism of corrosion protection was proposed to consist of the self-healing effect of the decavanadate intercalation and the shielding effect of the sol-gel film.

Scanning electrochemical microscopy determination of hydrogen flux at liquid|liquid interface with potentiometric probe

OpenAIRE

Jedraszko, Justyna; Nogala, Wojciech; Adamiak, Wojciech; Girault, Hubert H.; Opallo, Marcin

2014-01-01

Scanning electrochemical microscopy potentiometric determination of local hydrogen concentration and its flux next to the liquid|liquid interface was demonstrated. This method is based on the shift of open circuit potential of Pt-based reversible hydrogen electrode. The detection system was verified with a system generating hydrogen under galvanostatic conditions. Then, it was applied to aqueous|1,2-dichloroethane interface where hydrogen is produced with decamethylferrocene as electron donor.

The study of optimal conditions of electrochemical etching of tunnel electron microscopy tungsten tips

International Nuclear Information System (INIS)

Anguiano, E.; Aguilar, M.; Olivar, A.I.

1996-01-01

We present the experimental results obtained during the study made in the electrochemical etching of tunneling electron microscopy tungsten tips. The experiments was made using DC and two usual electrolytes: KOH and NaOH. For the tip preparation we used a electrochemical cell with stainless steel cathode and the tungsten wire as anode. the electrodes was introduced in a glass recipient containing the electrolytic solution. We study the effects of applied voltage, polish time, tip length and electrolyte concentration as process relevant parameters. The best condition for tip preparation was obtained with a metallurgical microscope and with a SEM.EDX and Auger analysis was made. The results shown the better tips was made with KOH as electrolyte with a limited concentration range (2-4 normal) and applied voltage (2-6 volts) (Author) 20 refs

Discussion meet on electroanalytical techniques and their applications

International Nuclear Information System (INIS)

Aggarwal, S.K.; Gopinath, N.; Govindan, R.

2008-02-01

Electrochemistry is truly an interdisciplinary science and plays an important role in different branches of science and technology. The present Discussion Meet on ElectroAnalytical Techniques (DM- ELANTE-2008) is focused on the update of various electroanalytical techniques which have brought out a substantial change in electroanalytical chemistry. The aim of this Discussion Meet is to provide a forum to all the electroanalytical scientists to discuss their recent findings and information, learn from the mutual experiences and interests, and to promote cooperation both nationally and internationally. It is proposed to have tutorial lectures as well as invited talks during the Discussion Meet on various electroanalytical techniques including Electrochemical Impedance Spectroscopy (EIS), Spectro-electrochemistry, Scanning Electrochemical Microscopy (SECM), Electrochemical Quartz Crystal Microbalance (EQCM), Surface Plasmon Resonance (SPR) etc. Papers relevant to INIS are indexed separately

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.

Electrochemomechanics with flexoelectricity and modelling of electrochemical strain microscopy in mixed ionic-electronic conductors

Energy Technology Data Exchange (ETDEWEB)

Yu, Pengfei; Hu, Shuling; Shen, Shengping, E-mail: sshen@mail.xjtu.edu.cn [State Key Laboratory for Strength and Vibration of Mechanical Structures, School of Aerospace, Xi' an Jiaotong University, Xi' an 710049 (China)

2016-08-14

Recently, a new scanning probe microscopy approach, referred to as electrochemical strain microscopy (ESM), for probing local ionic flows and electrochemical reactions in solids based on the bias-strain coupling was proposed by Morozovska et al. Then, a series of theoretical papers for analyzing the image formation and spectroscopic mechanism of ESM were published within the framework of Fermi-Dirac statistics, the Vegard law, the direct flexoelectric coupling effect, the electrostriction effect, and so on. However, most of the models in these papers are limited to the partial coupling or particular process, and numerically solved by using decoupling approximation. In this paper, to model the ESM measurement with the coupling electrical-chemical-mechanical process, the chemical Gibbs function variational principle for the thermal electrical chemical mechanical fully coupling problem is proposed. The fully coupling governing equations are derived from the variational principle. When the tip concentrates the electric field within a small volume of the material, the inhomogeneous electric field is induced. So, both direct and inverse flexoelectric effects should be taken into account. Here, the bulk defect electrochemical reactions are also taken into account, which are usually omitted in the existing works. This theory can be used to deal with coupling problems in solids, including conductors, semiconductors, and piezoelectric and non-piezoelectric dielectrics. As an application of this work, a developed initial-boundary value problem is solved numerically in a mixed ion-electronic conductor. Numerical results show that it is meaningful and necessary to consider the bulk defect chemical reaction. Besides, the chemical reaction and the flexoelectric effect have an interactive influence on each other. This work can provide theoretical basis for the ESM as well as investigating the bulk chemical reaction process in solids.

Graphenated tantalum(IV) oxide and poly(4-styrene sulphonic acid)-doped polyaniline nanocomposite as cathode material in an electrochemical capacitor

International Nuclear Information System (INIS)

Njomo, Njagi; Waryo, Tesfaye; Masikini, Milua; Ikpo, Chinwe O.; Mailu, Stephen; Tovide, Oluwakemi; Ross, Natasha; Williams, Avril; Matinise, Nolubabalo; Sunday, Christopher E.; Mayedwa, Noluthando; Baker, Priscilla G.L.; Ozoemena, Kenneth I.; Iwuoha, Emmanuel I.

2014-01-01

Nanostructured poly(4-styrene sulphonic acid) and tantalum (IV) oxide-doped polyaniline nanocomposite were synthesised and their electro-conductive properties were determined. The oxide was synthesized using a modified sol-gel method and then dispersed in acidic media through sonication and entrapped in-situ into the polymeric matrix during the oxidative chemical polymerization of aniline doped with poly(4-styrene sulphonic acid). The oxides and novel polymeric nanocomposite were characterised with TEM, SEM, EDX, XRD, FTIR, UV-visible to ascertain elemental and phase composition, successful polymerization, doping, morphology and entrapment of the metal oxide nanoparticles. The electro-conductivity of the nanomaterial was interrogated using scanning electrochemical microscopy (SECM) and cyclic voltammetry (CV). The material was then anchored on activated graphitic carbon and used in the design of an asymmetric supercapacitor cell using 6 M KOH aqueous electrolyte. Characteristically high specific capacitance values of 318.4 F/g with a corresponding energy and power densities of 1.57 kWh/kg and 0.435 kW/kg, respectively, were demonstrated. The cell also showed high coulombic efficiency of 94.9% with a long cycle life and good cycle stability making the nanomaterial suitable for constructing supercapacitor cell electrodes

Improved L-cysteine electrocatalysis through a sequential drop dry technique using multi-walled carbon nanotubes and cobalt tetraaminophthalocyanine conjugates

International Nuclear Information System (INIS)

Nyoni, Stephen; Mugadza, Tawanda; Nyokong, Tebello

2014-01-01

Graphical abstract: A sequential drop dry modification of a glassy carbon electrode where by multiwalled carbon nanotubes are first placed on to the electrode followed by cobalt tetraaminophthalocyanine gave a better catalytic response towards the oxidation of L-cysteine than when the two components were mixed, due to the higher catalytic activity of the former as judged by scanning electrochemical microscopy. - Highlights: • A glassy carbon electrode modified with multi-walled carbon nanotubes and cobalt tetraaminophthalocyanine by a sequential drop dry method. • The modified surface gave a better catalytic response towards the oxidation of L-cysteine than when the individual components were mixed. • Scanning electrochemical microscopy was employed for surface characterization. - Abstract: Voltammetry, chronoamperometry, scanning electrochemical microscopy and electrochemical impedance spectroscopy methods are used for characterization of a glassy carbon electrode modified with multi-walled carbon nanotubes (MWCNTs)–cobalt tetraaminophthalocyanine (CoTAPc) mixture or sequential drop dry modification technique whereby the MWCNTs are first placed on to the electrode followed by CoTAPc. The sequential drop dry CoTAPc–MWCNTs modified surface gave better catalytic responses with a catalytic rate constant of 2.2 × 10 5 M −1 s −1 , apparent electron transfer rate constant of 0.073 cm s −1 , and a limit of detection of 2.8 × 10 −7 M. Scanning electrochemical microscopy (SECM) surface characterization (topography and reactivity) further gave proof the better catalytic perfomance of the sequential drop dry CoTAPc–MWCNTs modified surface

Accessing the dynamics of end-grafted flexible polymer chains by atomic force-electrochemical microscopy. Theoretical modeling of the approach curves by the elastic bounded diffusion model and Monte Carlo simulations. Evidence for compression-induced lateral chain escape.

Science.gov (United States)

Abbou, Jeremy; Anne, Agnès; Demaille, Christophe

2006-11-16

The dynamics of a molecular layer of linear poly(ethylene glycol) (PEG) chains of molecular weight 3400, bearing at one end a ferrocene (Fc) label and thiol end-grafted at a low surface coverage onto a gold substrate, is probed using combined atomic force-electrochemical microscopy (AFM-SECM), at the scale of approximately 100 molecules. Force and current approach curves are simultaneously recorded as a force-sensing microelectrode (tip) is inserted within the approximately 10 nm thick, redox labeled, PEG chain layer. Whereas the force approach curve gives access to the structure of the compressed PEG layer, the tip-current, resulting from tip-to-substrate redox cycling of the Fc head of the chain, is controlled by chain dynamics. The elastic bounded diffusion model, which considers the motion of the Fc head as diffusion in a conformational field, complemented by Monte Carlo (MC) simulations, from which the chain conformation can be derived for any degree of confinement, allows the theoretical tip-current approach curve to be calculated. The experimental current approach curve can then be very satisfyingly reproduced by theory, down to a tip-substrate separation of approximately 2 nm, using only one adjustable parameter characterizing the chain dynamics: the effective diffusion coefficient of the chain head. At closer tip-substrate separations, an unpredicted peak is observed in the experimental current approach curve, which is shown to find its origin in a compression-induced escape of the chain from within the narrowing tip-substrate gap. MC simulations provide quantitative support for lateral chain elongation as the escape mechanism.

Electrochemical study of bio-corrosion mechanisms at the carbon steel interface in presence of iron-reducing and hydrogenotrophic bacteria in the nuclear waste disposal context

International Nuclear Information System (INIS)

Leite-de-Souza-Moreira, Rebeca

2013-01-01

The safety of deep geological repository for nuclear waste is a very important and topical matter especially for the nuclear industry. Such as nuclear fuel the high level waste have to be stored for time frames of millions of years in metallic containers. Typically these containers should be placed in deep geological clay formations 500 metres underground. Corrosion processes, will take place after the re-saturation of the geological medium and under the prevalent anoxic conditions may lead to the generation of hydrogen. This gas accumulates in clay environment through the years and eventually becomes hazardous for steel containers. In the particular environment of geological repositories does not provide much biodegradable substances. This is the reason that hydrogen represents a new suitable energy source for hydrogenotrophic bacteria. Thereby formed bacterial bio-films on the containers may contribute to a process of fast decay of the steel, the so called bio-corrosion. The aim of this study is to characterize the electrochemical interfaces in order to obtain the mechanisms of bio-corrosion of carbon steels in presence of iron reducing and hydrogenotrophic bacterium Shewanella oneideinsis. The products of corrosion processes, namely hydrogen and iron (III) oxides are used as electron donor and acceptor, respectively. The amount of hydrogen consumed by Shewanella could be estimated with 10"-"4 mol s"-"1 using Scanning Electrochemical Microscopy (SECM) techniques. The influence of the local hydrogen generation was evaluated via chrono-amperometry. When hydrogen was locally generated above a carbon steel substrate an accelerated corrosion process can be observed. Eventually, using Local Electrochemical Impedance Spectroscopy (LEIS) techniques, the mechanism of the generalised corrosion process was demonstrated. (author)

Characterization of azo dyes on Pt and Pt/polyaniline/dispersed Pt electrodes

Energy Technology Data Exchange (ETDEWEB)

Molina, J.; Fernandez, J.; Rio, A.I. del; Bonastre, J. [Departamento de Ingenieria Textil y Papelera, EPS de Alcoy, Universitat Politecnica de Valencia, Plaza Ferrandiz y Carbonell s/n, 03801 Alcoy (Spain); Cases, F., E-mail: fjcases@txp.upv.es [Departamento de Ingenieria Textil y Papelera, EPS de Alcoy, Universitat Politecnica de Valencia, Plaza Ferrandiz y Carbonell s/n, 03801 Alcoy (Spain)

2012-06-15

The electrochemical characterization of two organic dyes (amaranth and procion orange MX-2R) has been performed on Pt electrodes and Pt electrodes coated with polyaniline and dispersed Pt. Electrodes with different Pt loads have been synthesized and characterized obtaining that a load of 300 {mu}g cm{sup -2} was the optimum one. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) was employed to observe the distribution and morphology of the Pt nanoparticles. The electroactivity of the electrodes has also been characterized by means of scanning electrochemical microscopy (SECM). The chemical characterization of Pt dispersed Pani coated Pt electrodes (Pt-Pani-Pt) was performed by means of X-ray photoelectron spectroscopy (XPS). The electrochemical characterization of the dyes has been performed by means of cyclic voltammetry. Voltammograms have shown that the presence of the dyes diminishes characteristic Pt oxidation and reduction peaks. However, redox processes due to the dyes, appeared in the voltammograms. The different species responsible of these redox processes were generated in the vicinity of the electrode and were not adsorbed on the electrode surface since after stirring, the different redox processes disappeared. Characterization with different scan rates showed that redox processes of both dyes were controlled by diffusion.

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.

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).

Thin-film voltammetry and its analytical applications: A review

International Nuclear Information System (INIS)

Tian, Huihui; Li, Yunchao; Shao, Huibo; Yu, Hua-Zhong

2015-01-01

Highlights: • Electrochemistry at immiscible liquid–liquid interfaces is fundamentally important. • Methods for studying redox processes at liquid–liquid interfaces are reviewed. • Thin-film voltammetry is simple in experimental operation and kinetic data analysis. • Thin-film voltammetry’s analytical applications are prevailing and comprehensive. - Abstract: Electrochemical reactions at the interfaces of immiscible electrolyte solutions (ITIES) are of fundamental importance in the fields of chemical, biological and pharmaceutical sciences. Four-electrode cell setup, scanning electrochemical microscopy (SECM) and thin-film voltammetry are the three most frequently used methods for studying the electrochemical processes at these interfaces. The principle, experimental design, advantages and challenges of the three methods are described and compared. The thin-film voltammetry is highlighted for its simplicity in experimental operation and kinetic data analysis. Its versatile analytical applications are discussed in detail, including the study of redox properties of hydrophobic compounds, evaluation of interfacial electron transfer kinetics, synthesis of nanoparticles/nanostructures, and illustration of cross-membrane ion transport phenomena

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.

Optimization of Electrical Methods for Sub -surface Monitoring of Biological Contamination: From Micro-scale to Macroscopic one through Sub-micrometric Topographic and Electrochemical Studies of Oxydation/Reduction Processes Provoked by Bacteria

Science.gov (United States)

Dhahri, S.; Marliere, C.

2012-12-01

The presence of biological matter (bacteria) in deep geological sites for storage of, for instance, radioactive elements or groundwater in aquifers was clearly proved. That biomass triggers physical and chemical processes which greatly modify the durability and the sustainability of the storage sites. These processes, mainly from oxidative/reductive reactions, are poorly understood. This is mainly due to the fact that former studies were done at the macroscopic level far away from the micrometric scale where relevant processes induced by bacteria take place. Investigations at microscopic level are needed. Thus, we developed an experimental set -up based on the combined use of optical microscopy (epifluorescence and transmission), atomic force microscopy (AFM) and scanning electro -chemical microscopy (SECM) in order to get simultaneous information on topographic and electro -chemical processes at different length scales. The first highly sensitive step was to use AFM and optical microscopy with biological samples in liquid environment: We will present a new, non -perturbative method for imaging bacteria in their natural liquid environment using AFM. No immobilization protocol, neither chemical nor mechanical, is needed, contrary to what has been regarded till now as essential. Furthermore we were able to follow the natural gliding movements of bacteria, directly proving their living state during the AFM investigation: we thus directly prove the low impact of these breakthrough AFM observations on the native behavior of the bacteria. The second delicate step was to combine AFM and optical measurements with electrical ones. We mounted a new experimental set-up coupling real -time (i) monitoring of optical properties as the optical density (OD) evolution related to bulk bacterial growth in liquid or as the counting of number of bacteria adhering on the surface of the sample as well and (ii) electrical and electrochemical measurements. We thus will present results on

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

Imaging space charge regions in Sm-doped ceria using electrochemical strain microscopy

International Nuclear Information System (INIS)

Chen, Qian Nataly; Li, Jiangyu; Adler, Stuart B.

2014-01-01

Nanocrystalline ceria exhibits a total conductivity several orders of magnitude higher than microcrystalline ceria in air at high temperature. The most widely accepted theory for this enhancement (based on fitting of conductivity data to various transport and kinetic models) is that relatively immobile positively charged defects and/or impurities accumulate at the grain boundary core, leading to a counterbalancing increase in the number of mobile electrons (small polarons) within a diffuse space charge region adjacent to each grain boundary. In an effort to validate this model, we have applied electrochemical strain microscopy to image the location and relative population of mobile electrons near grain boundaries in polycrystalline Sm-doped ceria in air at 20–200 °C. Our results show the first direct (spatially resolved) evidence that such a diffuse space charge region does exist in ceria, and is localized to both grain boundaries and the gas-exposed surface

Imaging space charge regions in Sm-doped ceria using electrochemical strain microscopy

Energy Technology Data Exchange (ETDEWEB)

Chen, Qian Nataly; Li, Jiangyu, E-mail: jjli@uw.edu [Department of Mechanical Engineering, University of Washington, Seattle, Washington 98195 (United States); Adler, Stuart B., E-mail: stuadler@uw.edu [Department of Chemical Engineering, University of Washington, Seattle, Washington 98195 (United States)

2014-11-17

Nanocrystalline ceria exhibits a total conductivity several orders of magnitude higher than microcrystalline ceria in air at high temperature. The most widely accepted theory for this enhancement (based on fitting of conductivity data to various transport and kinetic models) is that relatively immobile positively charged defects and/or impurities accumulate at the grain boundary core, leading to a counterbalancing increase in the number of mobile electrons (small polarons) within a diffuse space charge region adjacent to each grain boundary. In an effort to validate this model, we have applied electrochemical strain microscopy to image the location and relative population of mobile electrons near grain boundaries in polycrystalline Sm-doped ceria in air at 20–200 °C. Our results show the first direct (spatially resolved) evidence that such a diffuse space charge region does exist in ceria, and is localized to both grain boundaries and the gas-exposed surface.

Diffusion and reaction in microbead agglomerates.

Science.gov (United States)

Nunes Kirchner, Carolina; Träuble, Markus; Wittstock, Gunther

2010-04-01

Scanning electrochemical microscopy has been used to analyze the flux of p-aminonophenol (PAP) produced by agglomerates of polymeric microbeads modified with galactosidase as a model system for the bead-based heterogeneous immunoassays. With the use of mixtures of enzyme-modified and bare beads in defined ratio, agglomerates with different saturation levels of the enzyme modification were produced. The PAP flux depends on the intrinsic kinetics of the galactosidase, the local availability of the substrate p-aminophenyl-beta-D-galactopyranoside (PAPG), and the external mass transport conditions in the surrounding of the agglomerate and the internal mass transport within the bead agglomerate. The internal mass transport is influenced by the diffusional shielding of the modified beads by unmodified beads. SECM in combination with optical microscopy was used to determine experimentally the external flux. These data are in quantitative agreement with boundary element simulation considering the SECM microelectrode as an interacting probe and treating the Michaelis-Menten kinetics of the enzyme as nonlinear boundary conditions with two independent concentration variables [PAP] and [PAPG]. The PAPG concentration at the surface of the bead agglomerate was taken as a boundary condition for the analysis of the internal mass transport condition as a function of the enzyme saturation in the bead agglomerate. The results of this analysis are represented as PAP flux per contributing modified bead and the flux from freely suspended galactosidase-modified beads. These numbers are compared to the same number from the SECM experiments. It is shown that depending on the enzyme saturation level a different situation can arise where either beads located at the outer surface of the agglomerate dominate the contribution to the measured external flux or where the contribution of buried beads cannot be neglected for explaining the measured external flux.

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.

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...

Effect of alternating voltage treatment on corrosion resistance of AZ91D magnesium alloy

Energy Technology Data Exchange (ETDEWEB)

Liu, X. [Corrosion and Protection Laboratory, Key Laboratory of Superlight Materials and Surface Technology (Harbin Engineering University), Ministry of Education, Harbin (China); Zhang, T.; Shao, Y.; Meng, G.; Wang, F. [Corrosion and Protection Laboratory, Key Laboratory of Superlight Materials and Surface Technology (Harbin Engineering University), Ministry of Education, Harbin (China); State Key Laboratory for Corrosion and Protection, Institute of Metal Research, Chinese Academy of Sciences, Shenyang (China)

2012-06-15

AZ91D magnesium alloy was treated by the alternating voltage (AV) treatment technique. The optimal AV-treatment parameters of the alloy were determined by orthogonal experiments. Polarization curve, electrochemical impedance spectroscopy (EIS), and scanning electrochemical microscopy (SECM) were used to understand the effect of AV-treatment on the corrosion resistance of the alloy. AFM, contact angle, and XPS were employed to investigate further the influence of AV-treatment on the properties of the surface film formed on the alloy after AV-treatment. The results showed that a uniform and stable film was formed and the corrosion resistance of AZ91D magnesium alloy was significantly improved after AV-treatment. This was caused by the noticeable change of the chemical structure and semi-conducting properties of the surface film after AV-treatment. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Investigating Nanoscale Electrochemistry with Surface- and Tip-Enhanced Raman Spectroscopy.

Science.gov (United States)

Zaleski, Stephanie; Wilson, Andrew J; Mattei, Michael; Chen, Xu; Goubert, Guillaume; Cardinal, M Fernanda; Willets, Katherine A; Van Duyne, Richard P

2016-09-20

The chemical sensitivity of surface-enhanced Raman spectroscopy (SERS) methodologies allows for the investigation of heterogeneous chemical reactions with high sensitivity. Specifically, SERS methodologies are well-suited to study electron transfer (ET) reactions, which lie at the heart of numerous fundamental processes: electrocatalysis, solar energy conversion, energy storage in batteries, and biological events such as photosynthesis. Heterogeneous ET reactions are commonly monitored by electrochemical methods such as cyclic voltammetry, observing billions of electrochemical events per second. Since the first proof of detecting single molecules by redox cycling, there has been growing interest in examining electrochemistry at the nanoscale and single-molecule levels. Doing so unravels details that would otherwise be obscured by an ensemble experiment. The use of optical spectroscopies, such as SERS, to elucidate nanoscale electrochemical behavior is an attractive alternative to traditional approaches such as scanning electrochemical microscopy (SECM). While techniques such as single-molecule fluorescence or electrogenerated chemiluminescence have been used to optically monitor electrochemical events, SERS methodologies, in particular, have shown great promise for exploring electrochemistry at the nanoscale. SERS is ideally suited to study nanoscale electrochemistry because the Raman-enhancing metallic, nanoscale substrate duly serves as the working electrode material. Moreover, SERS has the ability to directly probe single molecules without redox cycling and can achieve nanoscale spatial resolution in combination with super-resolution or scanning probe microscopies. This Account summarizes the latest progress from the Van Duyne and Willets groups toward understanding nanoelectrochemistry using Raman spectroscopic methodologies. The first half of this Account highlights three techniques that have been recently used to probe few- or single-molecule electrochemical

Investigation of processing effects on the corrosion resistance of Ti20Mo alloy in saline solutions

International Nuclear Information System (INIS)

Bolat, G.; Izquierdo, J.; Gloriant, T.; Chelariu, R.; Mareci, D.; Souto, R.M.

2015-01-01

Graphical abstract: - Highlights: • Alloy fabrication method affects both surface finish and corrosion resistance. • More porous surface finish and higher wettability produced by powder sintering. • Passive layer formed on sintered alloy breaks down in saline solution. • Increase in surface porosity facilitated electron transfer through the oxide film. • More corrosion resistant alloy produced by cold crucible levitation melting. - Abstract: The electrochemical properties of Ti20Mo alloys prepared using different fabrication procedures, namely cold crucible levitation melting (CCLM) and powder sintering, were investigated using linear potentiodynamic polarization and EIS measurements. The surface condition was established using AFM, with the observation of a more porous surface finish in the case of powder sintering. A major effect of surface conditioning on the corrosion resistance of Ti20Mo alloys was observed, where the compact finish exhibits a superior corrosion resistance in chloride-containing saline solutions. Less insulating surfaces towards electron exchange resulted for the more porous finish as revealed by scanning electrochemical microscopy (SECM)

Self-consistent modelling of electrochemical strain microscopy in mixed ionic-electronic conductors: Nonlinear and dynamic regimes

Science.gov (United States)

Varenyk, O. V.; Silibin, M. V.; Kiselev, D. A.; Eliseev, E. A.; Kalinin, S. V.; Morozovska, A. N.

2015-08-01

The frequency dependent Electrochemical Strain Microscopy (ESM) response of mixed ionic-electronic conductors is analyzed within the framework of Fermi-Dirac statistics and the Vegard law, accounting for steric effects from mobile donors. The emergence of dynamic charge waves and nonlinear deformation of the surface in response to bias applied to the tip-surface junction is numerically explored. The 2D maps of the strain and concentration distributions across the mixed ionic-electronic conductor and bias-induced surface displacements are calculated. The obtained numerical results can be applied to quantify the ESM response of Li-based solid electrolytes, materials with resistive switching, and electroactive ferroelectric polymers, which are of potential interest for flexible and high-density non-volatile memory devices.

Self-consistent modelling of electrochemical strain microscopy in mixed ionic-electronic conductors: Nonlinear and dynamic regimes

Energy Technology Data Exchange (ETDEWEB)

Varenyk, O. V.; Morozovska, A. N., E-mail: sergei2@ornl.gov, E-mail: anna.n.morozovska@gmail.com [Institute of Physics, National Academy of Sciences of Ukraine, 46, pr. Nauky, 03028 Kyiv (Ukraine); Silibin, M. V. [National Research University of Electronic Technology “MIET,” 124498 Moscow (Russian Federation); Kiselev, D. A. [National University of Science and Technology “MISiS,” 119049 Moscow, Leninskiy pr. 4 (Russian Federation); Eliseev, E. A. [Institute for Problems of Materials Science, NAS of Ukraine, Krjijanovskogo 3, 03142 Kyiv (Ukraine); Kalinin, S. V., E-mail: sergei2@ornl.gov, E-mail: anna.n.morozovska@gmail.com [The Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831 (United States)

2015-08-21

The frequency dependent Electrochemical Strain Microscopy (ESM) response of mixed ionic-electronic conductors is analyzed within the framework of Fermi-Dirac statistics and the Vegard law, accounting for steric effects from mobile donors. The emergence of dynamic charge waves and nonlinear deformation of the surface in response to bias applied to the tip-surface junction is numerically explored. The 2D maps of the strain and concentration distributions across the mixed ionic-electronic conductor and bias-induced surface displacements are calculated. The obtained numerical results can be applied to quantify the ESM response of Li-based solid electrolytes, materials with resistive switching, and electroactive ferroelectric polymers, which are of potential interest for flexible and high-density non-volatile memory devices.

Evolution of the Corrosion Morphology on AZ31B Tracked Electrochemically and by In Situ Microscopy in Chloride-Containing Media

Science.gov (United States)

Melia, M. A.; Cain, T. W.; Briglia, B. F.; Scully, J. R.; Fitz-Gerald, J. M.

2017-11-01

The evolution of open-circuit corrosion morphology as a function of immersion time for Mg alloy AZ31B in 0.6-M NaCl solution was investigated. Real-time optical microscopy accompanied by simultaneous electrochemical characterization was used to characterize the filiform corrosion (FFC) of AZ31B. Specifically, the behavior of propagating corrosion filaments on the metal surface was observed, and correlations among polarization resistance, filament propagation rates, open-circuit potential, and active coverage of local corrosion sites were revealed. Three distinct stages of corrosion were observed in 0.6-M NaCl. An initial passive region, during which a slow potential rise occurred (termed stage I), a second FFC region (termed stage II) with shallow penetrating, distinct filaments, and a final FFC region (termed stage III) with deeper penetrating filaments, aligned to form a linear front. The electrochemical properties of each stage are discussed, providing insights into the penetration rates and corrosion model.

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

Intermittent contact atomic force microscopy in electrochemical environment

Energy Technology Data Exchange (ETDEWEB)

Haering, P; Koetz, R [Paul Scherrer Inst. (PSI), Villigen (Switzerland); Siegenthaler, H [Bern Univ., Bern (Switzerland)

1997-06-01

In situ measurements with Atomic Force Microscopy may cause surface modifications due to the tip-surface interactions. As an alternative and less destructive method, Intermittent Contact Atomic Force Microscopy (ICAFM) has been tested in an electrolytic environment. In the ICAFM mode the tip is not constantly in contact with the surface under investigation but is tapping onto the surface with a certain frequency. A commercial Park Scientific Instruments Microscopy has been modified to enable in situ experiment with ICAFM. It was possible to image iridium oxide films with ICAFM in the electrolytic environment without any noticeable surface modifications. (author) 3 figs., 4 refs.

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.

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

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.

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.

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.

Corrosion inhibition of powder metallurgy Mg by fluoride treatments.

Science.gov (United States)

Pereda, M D; Alonso, C; Burgos-Asperilla, L; del Valle, J A; Ruano, O A; Perez, P; Fernández Lorenzo de Mele, M A

2010-05-01

Pure Mg has been proposed as a potential degradable biomaterial to avoid both the disadvantages of non-degradable internal fixation implants and the use of alloying elements that may be toxic. However, it shows excessively high corrosion rate and insufficient yield strength. The effects of reinforcing Mg by a powder metallurgy (PM) route and the application of biocompatible corrosion inhibitors (immersion in 0.1 and 1M KF solution treatments, 0.1M FST and 1M FST, respectively) were analyzed in order to improve Mg mechanical and corrosion resistance, respectively. Open circuit potential measurements, polarization techniques (PT), scanning electrochemical microscopy (SECM) and electrochemical impedance spectroscopy (EIS) were performed to evaluate its corrosion behavior. SECM showed that the local current of attacked areas decreased during the F(-) treatments. The corrosion inhibitory action of 0.1M FST and 1M FST in phosphate buffered solution was assessed by PT and EIS. Under the experimental conditions assayed, 0.1M FST revealed better performance. X-ray photoelectron spectroscopy, energy dispersive X-ray and X-ray diffraction analyses of Mg(PM) with 0.1M FST showed the presence of KMgF(3) crystals on the surface while a MgF(2) film was detected for 1M FST. After fluoride inhibition treatments, promising results were observed for Mg(PM) as degradable metallic biomaterial due to its higher yield strength and lower initial corrosion rate than untreated Mg, as well as a progressive loss of the protective characteristics of the F(-)-containing film which ensures the gradual degradation process. Copyright (c) 2009 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

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.

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...

Changes on iron electrode surface during hydrogen permeation in borate buffer solution

International Nuclear Information System (INIS)

Modiano, S.; Carreno, J.A.V.; Fugivara, C.S.; Torresi, R.M.; Vivier, V.; Benedetti, A.V.; Mattos, O.R.

2008-01-01

Hydrogen interaction with oxide films grown on iron electrodes at open circuit potential (E oc ) and in the passive region (+0.30 V ECS ) was studied by chronopotentiometry, chronoamperometry and electrochemical impedance spectroscopy techniques. The results were obtained in deaerated 0.3 mol L -1 H 3 BO 3 + 0.075 mol L -1 Na 2 B 4 O 7 (BB, pH 8.4) solution before, during and after hydrogen permeation. The iron oxide film modification was also investigated by means of in situ X-ray absorption near-edge spectroscopy (XANES) and scanning electrochemical microscopy (SECM) before and during hydrogen permeation. The main conclusion was that the passive film is reduced during the hydrogen diffusion. The hydrogen permeation stabilizes the iron surface at a potential close to the thermodynamic water stability line where hydrogen evolution can occur. The stationary condition required for the determination of the permeation parameters cannot be easily attained on iron surface during hydrogen permeation. Moreover, additional attention must be paid when obtaining the transport parameters using the classical permeation cell

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.

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...

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...

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

Adsorptive stripping voltammetric determination of nitroimidazole derivative on multiwalled carbon nanotube modified electrodes: influence of size and functionalization of nanotubes

Energy Technology Data Exchange (ETDEWEB)

Jara-Ulloa, Paola; Canete-Rosales, Paulina; Nunez-Vergara, Luis J; Squella, Juan A., E-mail: asquella@ciq.uchile.c [University of Chile, Santiago (Chile). Chemical and Pharmaceutical Sciences Faculty. Bioelectrochemistry Lab.

2011-07-01

1-Methyl-4-nitro-2-bromine methylimidazole (4-NimMeBr), was electrochemically reduced on mercury, glassy carbon and multiwalled carbon nanotubes (MWCNT) modified electrodes. 4-NimMeBr was adsorbed on the MWCNT modified electrode thus permitting the implementation of an adsorptive stripping voltammetric (ASV) method. We have used 4-NimMeBr as a prototype electroactive nitro compound to study the effect of both the size of the nanotubes and its functionalization by oxidation. The oxidized MWCNT forms better dispersions than the non-oxidized, producing electrode surface with higher density of MWCNT as was determined by electrochemical mapping using scanning electrochemical microscopy (SECM). Under the optimized conditions, the peak current was proportional to the concentration of 4-NimMeBr in the range of 10{sup -6} mol L{sup -1} to 10{sup -4} mol L{sup -1} with detection and quantification limits of 4.41 x 10{sup -6} mol L{sup -1} and 6.21 x 10{sup -6} mol L{sup -1}, respectively. The sensibility of bare electrode was 0.01 {mu}A per mmol L{sup -1}, which was lower than the value of 5.34 and 6.97 mA per mmol L{sup -1} obtained using short and large oxidized MWCNT, respectively. (author)

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

Bioelectrocatalytic mediatorless dioxygen reduction at carbon ceramic electrodes modified with bilirubin oxidase

International Nuclear Information System (INIS)

Nogala, Wojciech; Celebanska, Anna; Szot, Katarzyna; Wittstock, Gunther; Opallo, Marcin

2010-01-01

Carbon ceramic electrodes were prepared by sol-gel processing of a hydrophobic precursor - methyltrimethoxysilane (MTMOS) - together with dispersed graphite microparticles according to a literature procedure. Bilirubin oxidase (BOx) was adsorbed on this electrode from buffer solution and this process was followed by atomic force microscopy (AFM). The electrodes exhibited efficient mediatorless electrocatalytic activity towards dioxygen reduction. The activity depends on the time of adsorption of the enzyme and the pH. The electrode remains active in neutral solution. The bioelectrocatalytic activity is further increased when a fraction of the carbon microparticles is replaced by sulfonated carbon nanoparticles (CNPs). This additive enhances the electrical communication between the enzyme and the electronic conductor. At pH 7 the carbon ceramic electrode modified with bilirubin oxidase retains ca. half of its highest activity. The role of the modified nanoparticles is confirmed by experiments in which a film embedded in a hydrophobic silicate matrix also exhibited efficient mediatorless biocatalytic dioxygen reduction. Scanning electrochemical microscopy (SECM) of the studied electrodes indicated a rather even distribution of the catalytic activity over the electrode surface.

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…

Electrochemical synthesis of polydiphenylamine nanofibrils through AAO template

International Nuclear Information System (INIS)

Zhao Yanchun; Chen Miao; Liu Xiang; Xu Tao; Liu Weimin

2005-01-01

Highly ordered polydiphenylamine (PDPA) nanofibrils arrays have been fabricated within the pores of porous anodic aluminum oxide (AAO) template membrane by electrochemical polymerization. The morphology of PDPA nanofibrils array was observed using transmission electron microscopy (TEM) and its electrochemical behavior and structure were examined by cyclic voltammetry, UV-vis spectroscopy and Fourier transmission infrared spectrum. The result of TEM revealed that the obtained PDPA nanofibrils had uniform and well-aligned array. The UV-vis spectroscopy and electrochemical experimental result indicated that the spatial restraint in the pores of AAO membrane is sufficient to induce the formation of more ordered PDPA chains in the AAO membrane

Electrochemical synthesis of polydiphenylamine nanofibrils through AAO template

Energy Technology Data Exchange (ETDEWEB)

Yanchun, Zhao [State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000 (China); Miao, Chen [State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000 (China); Xiang, Liu [State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000 (China); Tao, Xu [State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000 (China); Weimin, Liu [State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000 (China)

2005-06-15

Highly ordered polydiphenylamine (PDPA) nanofibrils arrays have been fabricated within the pores of porous anodic aluminum oxide (AAO) template membrane by electrochemical polymerization. The morphology of PDPA nanofibrils array was observed using transmission electron microscopy (TEM) and its electrochemical behavior and structure were examined by cyclic voltammetry, UV-vis spectroscopy and Fourier transmission infrared spectrum. The result of TEM revealed that the obtained PDPA nanofibrils had uniform and well-aligned array. The UV-vis spectroscopy and electrochemical experimental result indicated that the spatial restraint in the pores of AAO membrane is sufficient to induce the formation of more ordered PDPA chains in the AAO membrane.

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.

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.

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.

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...

Impact of the spatial distribution of morphological pattern on the efficiency of electrocatalytic gas evolving reactions

Directory of Open Access Journals (Sweden)

Žerađanin Aleksandar R.

2014-01-01

Full Text Available The efficiency of electrocatalytic gas evolving reactions (hydrogen, chlorine and oxygen evolution is a key challenge for the important industrial processes, such as chlor-alkali electrolysis or water electrolysis. Central issue for the aforementioned electrocatalytic processes is huge power consumption. Experimental results accumulated in the past, as well as some predictive models ("volcano" plots indicate that altering the nature of the electrode material cannot significantly increase the activity of mentioned reactions. Consequently, it is necessary to find a qualitatively different strategy for improving the energy efficiency of electrocatalytic gas evolving reactions. Usually disregarded fact is that the gas evolution is an oscillatory phenomenon. Given the oscillatory behavior, a key parameter of macrokinetics of gas electrode is the frequency of gas-bubble detachment. Bearing in mind that the gas evolution greatly depends on the surface morphology, a methodology is proposed that establishes a rational link between the morphological pattern of electrode with electrode activity and stability. Characterization was performed using advanced analytical tools. Frequency of gas-bubble detachment is obtained in the configuration of scanning electrochemical microscopy (SECM while the corrosion stability is analyzed using miniaturized scanning flow electrochemical cell connected to the mass spectrometer (SFC-ICPMS.

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.

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.

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 Design of Optical Nanoantennas

Directory of Open Access Journals (Sweden)

Vasilchenko V.E.

2015-01-01

Full Text Available Electrochemical techniques for fabricating tapered gold nanoantennas (tips are discussed. In the paper, the tunable design of nanoantennas is demonstrated. Tip parameters such as a tip apex curvature, mesoscopic morphology, aspect ratio and enhancement factor can be varied with etching electrolyte and applied voltage. The low-cost method makes tipehnahced optical spectroscopy and microscopy feasible for routine optical measurements beyond the diffraction limit.

Electrochemically cathodic exfoliation of graphene sheets in room temperature ionic liquids N-butyl, methylpyrrolidinium bis(trifluoromethylsulfonyl)imide and their electrochemical properties

International Nuclear Information System (INIS)

Yang, Yingchang; Lu, Fang; Zhou, Zhou; Song, Weixin; Chen, Qiyuan; Ji, Xiaobo

2013-01-01

Graphical abstract: Electrochemically cathodic exfoliation of graphite into few-layer graphene sheets in room temperature ionic liquids (RTILs) N-butyl, methylpyrrolidinium bis(trifluoromethylsulfonyl)-imide (BMPTF 2 N). -- Highlights: • Few-layer graphene sheets were prepared through electrochemically cathodic exfoliation in room temperature ionic liquids. • The mechanism of cathodic exfoliation in ionic liquids was proposed. • The derived activated graphene sheets show enhanced electrochemical properties. -- Abstract: Electrochemically cathodic exfoliation in room temperature ionic liquids N-butyl, methylpyrrolidinium bis(trifluoromethylsulfonyl)-imide (BMPTF 2 N) has been developed for few-layer graphene sheets, demonstrating low levels of oxygen (2.7 at% of O) with a nearly perfect structure (I D /I G 2 N involves the intercalation of ionic liquids cation [BMP] + under highly negatively charge followed by graphite expansion. Porous activated graphene sheets were also obtained by activation of graphene sheets in KOH. Transmission electron microscopy, X-ray photoelectron spectroscopy and Raman spectroscopy were used to characterize these graphene materials. The electrochemical performances of the graphene sheets and porous activated graphene sheets for lithium-ion battery anode materials were evaluated using cyclic voltammetry, galvanostatic charge–discharge cycling, and electrochemical impedance spectroscopy

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.

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.

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.

Corrosion protection of ENIG surface finishing using electrochemical methods

International Nuclear Information System (INIS)

Bui, Q.V.; Nam, N.D.; Choi, D.H.; Lee, J.B.; Lee, C.Y.; Kar, A.; Kim, J.G.; Jung, S.B.

2010-01-01

Four types of thin film coating were carried out on copper for electronic materials by the electroless plating method at a pH range from 3 to 9. The coating performance was evaluated by electrochemical impedance spectroscopy and potentiodynamic polarization testing in a 3.5 wt.% NaCl solution. In addition, atomic force microscopy and X-ray diffraction were also used to analyze the coating surfaces. The electrochemical behavior of the coatings was improved using the electroless nickel plating solution of pH 5. The electroless nickel/immersion gold on the copper substrate exhibited high protective efficiency, charge transfer resistance and very low porosity, indicating an increase in corrosion resistance. Atomic force microscopy and X-ray diffraction analyses confirmed the surface uniformity and the formation of the crystalline-refined NiP {1 2 2} phase at pH 5.

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.

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)

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.

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.

Boron-doped Diamond Electrodes: Electrochemical, Atomic Force Microscopy and Raman Study towards Corrosion-modifications at Nanoscale

International Nuclear Information System (INIS)

Kavan, Ladislav; Vlckova Zivcova, Zuzana; Petrak, Vaclav; Frank, Otakar; Janda, Pavel; Tarabkova, Hana; Nesladek, Milos; Mortet, Vincent

2015-01-01

Highlights: • B-doped diamond is nanostructured by corrosion-driven modifications occurring at carbonaceous impurity sites (sp 2 -carbons). • The electrochemical oxidation partly transforms a hydrogen-terminated diamond surface to O-terminated one, but the electrocatalytic activity of plasmatically O-terminated diamond is not achieved. • In contrast to all usual sp 2 carbons, the Raman spectra of B-doped diamond electrodes do not change upon electrochemical charging/discharging. - Abstract: Comparative studies of boron-doped diamonds electrodes (polycrystalline, single-crystalline, H-/O-terminated, and with different sp 3 /sp 2 ratios) indicate morphological modifications of diamond which are initiated by corrosion at nanoscale. In-situ electrochemical AFM imaging evidences that the textural changes start at non-diamond carbonaceous impurity sites treated at high positive potentials (>2.2 V vs. Ag/AgCl). The primary perturbations subsequently develop into sub-micron-sized craters. Raman spectroscopy shows that the primary erosion site is graphite-like (sp 2 -carbon), which is preferentially removed by anodic oxidation. Other non-diamond impurity, viz. tetrahedral amorphous carbon (t-aC), is less sensitive to oxidative decomposition. The diamond-related Raman features, including the B-doping-assigned modes, are intact during reversible electrochemical charging/discharging, which is a salient difference from all usual sp 2 -carbons. The electrochemical oxidation partly transforms a hydrogen-terminated diamond surface to O-terminated one, but the electrocatalytic activity of plasmatically O-terminated diamond is not achieved for a model redox couple, Fe 3+/2+ . Electrochemical impedance spectra were fitted to six different equivalent circuits. The determination of acceptor concentrations is feasible even for highly-doped diamond electrodes.

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

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).

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

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

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.

Water-mediated electrochemical nano-writing on thin ceria films

International Nuclear Information System (INIS)

Yang, Nan; Doria, Sandra; Tebano, Antonello; Licoccia, Silvia; Balestrino, Giuseppe; Kumar, Amit; Arruda, Thomas M; Jesse, Stephen; Ivanov, Ilia N; Baddorf, Arthur P; Strelcov, Evgheni; Kalinin, Sergei V; Jang, Jae Hyuck; Borisevich, Albina Y

2014-01-01

Bias dependent mechanisms of irreversible cathodic and anodic processes on a pure CeO 2 film are studied using modified atomic force microscopy (AFM). For a moderate positive bias applied to the AFM tip an irreversible electrochemical reduction reaction is found, associated with significant local volume expansion. By changing the experimental conditions we are able to deduce the possible role of water in this process. Simultaneous detection of tip height and current allows the onset of conductivity and the electrochemical charge transfer process to be separated, further elucidating the reaction mechanism. The standard anodic/cathodic behavior is recovered in the high bias regime, where a sizable transport current flows between the tip and the film. These studies give insight into the mechanisms of the tip-induced electrochemical reactions as mediated by electronic currents, and into the role of water in these processes, as well as providing a different approach for electrochemical nano-writing. (paper)

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.

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.

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

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.

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

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 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.

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.%.

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.

The study of optimal conditions of electrochemical etching of tunnel electron microscopy tungsten tips; Estudio de las condiciones optimas para la preparacion electroquimica de puntas de tungsteno para el Microscopio de Efecto Tunel

Energy Technology Data Exchange (ETDEWEB)

Anguiano, E; Aguilar, M [Instituto de Ciencia de Materiales del SCIC, Madrid (Spain); Olivar, A I [Centro de Investigacion y de Estudios Avanzados del IPN Unidad Merida. Departamento de fisica Aplicada, Yucatan, Mexico (Mexico)

1997-12-31

We present the experimental results obtained during the study made in the electrochemical etching of tunneling electron microscopy tungsten tips. The experiments was made using DC and two usual electrolytes: KOH and NaOH. For the tip preparation we used a electrochemical cell with stainless steel cathode and the tungsten wire as anode. the electrodes was introduced in a glass recipient containing the electrolytic solution. We study the effects of applied voltage, polish time, tip length and electrolyte concentration as process relevant parameters. The best condition for tip preparation was obtained with a metallurgical microscope and with a SEM.EDX and Auger analysis was made. The results shown the better tips was made with KOH as electrolyte with a limited concentration range (2-4 normal) and applied voltage (2-6 volts) (Author) 20 refs.

Electrochemical attosyringe.

Science.gov (United States)

Laforge, François O; Carpino, James; Rotenberg, Susan A; Mirkin, Michael V

2007-07-17

The ability to manipulate ultrasmall volumes of liquids is essential in such diverse fields as cell biology, microfluidics, capillary chromatography, and nanolithography. In cell biology, it is often necessary to inject material of high molecular weight (e.g., DNA, proteins) into living cells because their membranes are impermeable to such molecules. All techniques currently used for microinjection are plagued by two common problems: the relatively large injector size and volume of injected fluid, and poor control of the amount of injected material. Here we demonstrate the possibility of electrochemical control of the fluid motion that allows one to sample and dispense attoliter-to-picoliter (10(-18) to 10(-12) liter) volumes of either aqueous or nonaqueous solutions. By changing the voltage applied across the liquid/liquid interface, one can produce a sufficient force to draw solution inside a nanopipette and then inject it into an immobilized biological cell. A high success rate was achieved in injections of fluorescent dyes into cultured human breast cells. The injection of femtoliter-range volumes can be monitored by video microscopy, and current/resistance-based approaches can be used to control injections from very small pipettes. Other potential applications of the electrochemical syringe include fluid dispensing in nanolithography and pumping in microfluidic systems.

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.

A reusable device for electrochemical applications of hydrogel supported black lipid membranes

DEFF Research Database (Denmark)

Mech-Dorosz, Agnieszka; Heiskanen, Arto; Bäckström, Sania

2015-01-01

the ETFE substrate and a gold electrode microchip, thus allowing direct electrochemical studies with the integrated working electrodes. Using electrochemical impedance spectroscopy (EIS), X-ray photoelectron spectroscopy and contact angle measurements, we demonstrate the optimized chemical modifications...... of the gold electrode microchips and plasma modification of the ETFE aperture arrays facilitating covalent "sandwiching" of the hydrogel. Both fluorescence microscopy and EIS were used to demonstrate the induced spontaneous thinning of a deposited lipid solution, leading to formation of stabilized hs...

Surface modification and electrochemical behaviour of undoped nanodiamonds

International Nuclear Information System (INIS)

Zang Jianbing; Wang Yanhui; Bian Linyan; Zhang Jinhui; Meng Fanwei; Zhao Yuling; Ren Shubin; Qu Xuanhui

2012-01-01

Surface modifications of undoped nanodiamond (ND) particles were carried out through different annealing treatments. The methods of Fourier transform infrared spectroscopy, Raman spectroscopy, and transmission electron microscopy were used to characterize the ND surface before and after the annealing process. The electrochemical properties of the modified ND powders in aqueous solution were investigated with Fe(CN) 6 3−/4− as a redox probe. When the annealing temperature was below 850 °C, vacuum annealing removed parts of the oxygen-containing surface functionalities from the ND surface and produced more sp 2 carbon atoms in the shell. The charge transfer of the Fe(CN) 6 3−/4− redox couple decreased with increasing annealing temperature. Re-annealing in air restored the original surface conditions: few sp 2 -bonded carbon atoms and similar surface functionalities, and thus the electrochemical activity. When ND was annealed in vacuum at 900–1100 °C, more serious graphitization produced a continuous fullerenic shell wrapped around a diamond core, which had a high conductivity and electrochemical activity. This provides a novel nanoparticle with high conductivity and high stability for electrochemical applications.

Ultra-nanocrystalline diamond nanowires with enhanced electrochemical properties

International Nuclear Information System (INIS)

Shalini, Jayakumar; Lin, Yi-Chieh; Chang, Ting-Hsun; Sankaran, Kamatchi Jothiramalingam; Chen, Huang-Chin; Lin, I.-Nan; Lee, Chi-Young; Tai, Nyan-Hwa

2013-01-01

The effects of N 2 incorporation in Ar/CH 4 plasma on the electrochemical properties and microstructure of ultra-nanocrystalline diamond (UNCD) films are reported. While the electrical conductivity of the films increased monotonously with increasing N 2 content (up to 25%) in the plasma, the electrochemical behavior was optimized for UNCD films grown in (Ar–10% N 2 )/CH 4 plasma. Transmission electron microscopy showed that the main factor resulting in high conductivity in the films was the formation of needle-like nanodiamond grains and the induction graphite layer encapsulating these grains. The electrochemical process for N 2 -incorporated UNCD films can readily be activated due to the presence of nanographite along the grain boundaries of the films. The formation of needle-like diamond grains was presumably due to the presence of CN species that adhered to the existing nanodiamond clusters, which suppressed radial growth of the nanodiamond crystals, promoting anisotropic growth and the formation of needle-like nanodiamond. The N 2 -incorporated UNCD films outperformed other electrochemical electrode materials, such as boron-doped diamond and glassy carbon, in that the UNCD electrodes could sense dopamine, urea, and ascorbic acid simultaneously in the same mixture with clear resolution

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.

Capsid protein oxidation in feline calicivirus using an electrochemical inactivation treatment

Energy Technology Data Exchange (ETDEWEB)

Shionoiri, Nozomi; Nogariya, Osamu; Tanaka, Masayoshi; Matsunaga, Tadashi; Tanaka, Tsuyoshi, E-mail: tsuyo@cc.tuat.ac.jp

2015-02-11

Highlights: • Feline calicivirus was inactivated electrochemically by a factor of >5 log. • The electrochemical treatment was performed at 0.9 V (vs. Ag/AgCl) for 15 min. • Electrochemical treatment caused oxidation of viral proteins. • Oxidation of viral proteins can lead to loss of viral structural integrity. - Abstract: Pathogenic viral infections are an international public health concern, and viral disinfection has received increasing attention. Electrochemical treatment has been used for treatment of water contaminated by bacteria for several decades, and although in recent years several reports have investigated viral inactivation kinetics, the mode of action of viral inactivation by electrochemical treatment remains unclear. Here, we demonstrated the inactivation of feline calicivirus (FCV), a surrogate for human noroviruses, by electrochemical treatment in a developed flow-cell equipped with a screen-printed electrode. The viral infectivity titer was reduced by over 5 orders of magnitude after 15 min of treatment at 0.9 V vs. Ag/AgCl. Proteomic study of electrochemically inactivated virus revealed oxidation of peptides located in the viral particles; oxidation was not observed in the non-treated sample. Furthermore, transmission electron microscopy revealed that viral particles in the treated sample had irregular structures. These results suggest that electrochemical treatment inactivates FCV via oxidation of peptides in the structural region, causing structural deformation of virus particles. This first report of viral protein damage through electrochemical treatment will contribute to broadening the understanding of viral inactivation mechanisms.

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.

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)

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

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.

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.

Fabrication a new modified electrochemical sensor based on Au–Pd bimetallic nanoparticle decorated graphene for citalopram determination

Energy Technology Data Exchange (ETDEWEB)

Daneshvar, Leili [Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, Mashhad (Iran, Islamic Republic of); Rounaghi, Gholam Hossein, E-mail: ghrounaghi@yahoo.com [Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, Mashhad (Iran, Islamic Republic of); Es' haghi, Zarrin [Department of Chemistry, Faculty of Sciences, Payame Noor University, Mashhad (Iran, Islamic Republic of); Chamsaz, Mahmoud; Tarahomi, Somayeh [Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, Mashhad (Iran, Islamic Republic of)

2016-12-01

This paper proposes a simple approach for sensing of citalopram (CTL) using gold–palladium bimetallic nanoparticles (Au–PdNPs) decorated graphene modified gold electrode. Au–PdNPs were deposited at the surface of a graphene modified gold electrode with simple electrodeposition method. The morphology and the electrochemical properties of the modified electrode were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), energy dispersion spectroscopy (EDS), electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV) and square wave voltammetry (SWV). The novel sensor exhibited an excellent catalytic activity towards the oxidation of CTL. The oxidation peak current of CTL, was linear in the range of 0.5–50 μM with a detection limit 0.049 μM with respect to concentration of citalopram. The proposed sensor was successfully applied for determination of CTL tablet and human plasma samples with satisfactory results. - Highlights: • A novel sensor based on Au-PdNPs deposited graphene modified gold electrode was fabricated. • The morphology and the electrochemical properties of the sensor were characterized by several methods. • The fabricated sensor was employed for the detection of antidepressant drug CTL with satisfactory results.

In situ electrochemical etching and examination by SPM of titanate ceramics

International Nuclear Information System (INIS)

Thorogood, G.J.; Short, K.T; Zhang, Y.

2002-01-01

Full text: The aqueous durability of titanate related ceramics is of great importance for the immobilisation of high level radioactive waste-in order to observe the reaction progress at the solid-liquid interface of these durable ceramics, we have attempted to accelerate the dissolution process via electrochemical means by using a SPM cell with electrochemical capability. The experiment involves placing a titanate ceramic disk (with flat polished surfaces) in the electrochemical cell. The cell is then set up with the ceramic acting as one electrode and another electrode being placed in the solution. In a flow through cell it is possible to select the pH and observe the change, not only in surface morphology as dissolution occurs, but also the frictional characteristics of the surface. The SPM tip plays no role in the electrochemical reaction. We will be presenting results from our work and discussing possible mechanisms for dissolution and future directions of the work. Copyright (2002) Australian Society for Electron Microscopy Inc

Platinum nanoparticles functionalized nitrogen doped graphene platform for sensitive electrochemical glucose biosensing

International Nuclear Information System (INIS)

Yang, Zhanjun; Cao, Yue; Li, Juan; Jian, Zhiqin; Zhang, Yongcai; Hu, Xiaoya

2015-01-01

Highlights: • An efficient PtNPs@NG nanocomposite was prepared for the immobilization of enzyme. • A novel electrochemical glucose biosensor was constructed based on this PtNPs@NG. • The proposed glucose biosensor showed high sensitivity and low detection limit. • The PtNPs@NG composite provided a promising platform for biosensing applications. - Abstract: In this work, we reported an efficient platinum nanoparticles functionalized nitrogen doped graphene (PtNPs@NG) nanocomposite for devising novel electrochemical glucose biosensor for the first time. The fabricated PtNPs@NG and biosensor were characterized using transmission electron microscopy, high-resolution transmission electron microscopy, X-ray photoelectron spectroscopy, static water contact angle, UV–vis spectroscopy, electrochemical impedance spectra and cyclic voltammetry, respectively. PtNPs@NG showed large surface area and excellent biocompatibility, and enhanced the direct electron transfer between enzyme molecules and electrode surface. The glucose oxidase (GOx) immobilized on PtNPs@NG nanocomposite retained its bioactivity, and exhibited a surface controlled, quasi-reversible and fast electron transfer process. The constructed glucose biosensor showed wide linear range from 0.005 to 1.1 mM with high sensitivity of 20.31 mA M −1 cm −2 . The detection limit was calculated to be 0.002 mM at signal-to-noise of 3, which showed 20-fold decrease in comparison with single NG-based electrochemical biosensor for glucose. The proposed glucose biosensor also demonstrated excellent selectivity, good reproducibility, acceptable stability, and could be successfully applied in the detection of glucose in serum samples at the applied potential of −0.33 V. This research provided a promising biosensing platform for the development of excellent electrochemical biosensors

Platinum nanoparticles functionalized nitrogen doped graphene platform for sensitive electrochemical glucose biosensing

Energy Technology Data Exchange (ETDEWEB)

Yang, Zhanjun, E-mail: zjyang@yzu.edu.cn; Cao, Yue; Li, Juan; Jian, Zhiqin; Zhang, Yongcai; Hu, Xiaoya

2015-04-29

Highlights: • An efficient PtNPs@NG nanocomposite was prepared for the immobilization of enzyme. • A novel electrochemical glucose biosensor was constructed based on this PtNPs@NG. • The proposed glucose biosensor showed high sensitivity and low detection limit. • The PtNPs@NG composite provided a promising platform for biosensing applications. - Abstract: In this work, we reported an efficient platinum nanoparticles functionalized nitrogen doped graphene (PtNPs@NG) nanocomposite for devising novel electrochemical glucose biosensor for the first time. The fabricated PtNPs@NG and biosensor were characterized using transmission electron microscopy, high-resolution transmission electron microscopy, X-ray photoelectron spectroscopy, static water contact angle, UV–vis spectroscopy, electrochemical impedance spectra and cyclic voltammetry, respectively. PtNPs@NG showed large surface area and excellent biocompatibility, and enhanced the direct electron transfer between enzyme molecules and electrode surface. The glucose oxidase (GOx) immobilized on PtNPs@NG nanocomposite retained its bioactivity, and exhibited a surface controlled, quasi-reversible and fast electron transfer process. The constructed glucose biosensor showed wide linear range from 0.005 to 1.1 mM with high sensitivity of 20.31 mA M{sup −1} cm{sup −2}. The detection limit was calculated to be 0.002 mM at signal-to-noise of 3, which showed 20-fold decrease in comparison with single NG-based electrochemical biosensor for glucose. The proposed glucose biosensor also demonstrated excellent selectivity, good reproducibility, acceptable stability, and could be successfully applied in the detection of glucose in serum samples at the applied potential of −0.33 V. This research provided a promising biosensing platform for the development of excellent electrochemical biosensors.

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)

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 behaviour of monolayer and bilayer graphene

OpenAIRE

Valota, Anna T.; Kinloch, Ian A.; Novoselov, Kostya S.; Casiraghi, Cinzia; Eckmann, Axel; Hill, Ernie W.; Dryfe, Robert A. W.

2011-01-01

Results of a study on the electrochemical properties of exfoliated single and multilayer graphene flakes are presented. Graphene flakes were deposited on silicon/silicon oxide wafers to enable fast and accurate characterization by optical microscopy and Raman spectroscopy. Conductive silver paint and silver wires were used to fabricate contacts; epoxy resin was employed as masking coating in order to expose a stable, well defined area of graphene. Both multilayer and monolayer graphene microe...

Graphene Nanosheets/Poly(3,4-ethylenedioxythiophene) Nanotubes Composite Materials for Electrochemical Biosensing Applications

International Nuclear Information System (INIS)

Huang, Tzu-Yen; Kung, Chung-Wei; Wang, Jen-Yuan; Lee, Min-Han; Chen, Lin-Chi; Chu, Chih-Wei; Ho, Kuo-Chuan

2015-01-01

Highlights: • Novel composite materials contain 2D rGO nanosheets and 1D PEDOT nanotubes. • 3D nanocomposite film effectively improved the sensitivity for analyte detection. • The rGO/PEDOT NTs film shows good catalytic activities toward hydrazine and H 2 O 2 . • The rGO/PEDOT NTs film also exhibits high selectivity from the interference test. -- Graphical abstract: Display Omitted -- Abstract: In this study, we developed the novel composite materials containing reduced graphene oxide (rGO) nanosheets and poly(3,4-ethylenedioxythiophene) nanotubes (PEDOT NTs) for electrochemical biosensing applications. Transmission electron microscopy, scanning electron microscopy and atomic force microscopy suggested that the rGO nanosheets cover the substrate uniformly, and the PEDOT NTs act as a conducting bridge to connect the rGO sheets. By combining the two materials, it's expected to enhance the conductivity of the film and improve the surface coverage. We applied the rGO/PEDOT NTs composite for electrochemical detection of hydrazine and hydrogen peroxide; noticeable improvements in electrochemical activity and reactivity were observed compared to those of the pristine rGO and PEDOT NTs electrodes. This may be attributed to the better surface coverage of the rGO/PEDOT NTs modified electrode with superior conductivity. Furthermore, interference tests indicate that the rGO/PEDOT NTs composite film exhibits high selectivity toward the analyte. The rGO/PEDOT NTs composite thus provides a potential platform for biosensing applications

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.

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.

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

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.

Investigation of selective corrosion resistance of aged lean duplex stainless steel 2101 by non-destructive electrochemical techniques

International Nuclear Information System (INIS)

Gao Juan; Jiang Yiming; Deng Bo; Zhang Wei; Zhong Cheng; Li Jin

2009-01-01

Lean duplex stainless steel 2101 (LDX2101) shows wide application potential due to its better corrosion performance and lower cost than traditional 304 austenite steel. This paper investigates the effects of thermal aging treatments at 700 deg. C for various aging times up to 100 h on the selective corrosion resistance of LDX2101 by two non-destructive electrochemical measurements: double-loop electrochemical potentiokinetic reactivation (DL-EPR) and electrochemical impedance spectroscopy (EIS). The evolution of microstructure was examined by optical microscopy, SEM microscopy and X-ray diffraction techniques (XRD). The results showed that the two applied electrochemical measurements agreed very well. Both methods were able to reveal the relationship between microstructure and selective corrosion resistance, which was related to the formation of chromium- and molybdenum-depleted zones around the precipitates, especially the σ phase, during aging. Nevertheless, more information could be obtained using EIS methods, including the interfacial charge transfer reaction and the corrosion product adsorption process. The results suggest that the susceptibility of the aged alloy to selective corrosion is presumably codetermined by the formation of chromium- and molybdenum-depleted areas, as well as by the replenishment of them, in these areas from the bulk during aging.

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.

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.

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.

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

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.

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.

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.

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

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

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.

Investigation of the cleanliness of transferred graphene. The first step toward its application as a window material for electron microscopy and spectroscopy

International Nuclear Information System (INIS)

Ma, Tao; Miyazaki, Kotaro; Ariga, Hiroko; Takakusagi, Satoru; Asakura, Kiyotaka

2015-01-01

The cleanliness of transferred graphene is of significant importance for its application as the window material in environmental cells used for electron microscopy and spectroscopy. We investigated the dependence of the cleanliness of graphene on transfer routes, including FeCl 3 etching, (NH 4 ) 2 S 2 O 8 etching, electrochemical delamination, and O 2 -bubbling, by means of transmission electron microscopy and X-ray photoelectron spectroscopy. It was found that electrochemical delamination provided the cleanest graphene with only a small amount of poly(methyl methacrylate) (PMMA) residue existing on the surface. (author)

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.

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

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.

Spectroscopic and electrochemical characterization of nanostructured optically transparent carbon electrodes.

Science.gov (United States)

Benavidez, Tomás E; Garcia, Carlos D

2013-07-01

The present paper describes the results related to the optical and electrochemical characterization of thin carbon films fabricated by spin coating and pyrolysis of AZ P4330-RS photoresist. The goal of this paper is to provide comprehensive information allowing for the rational selection of the conditions to fabricate optically transparent carbon electrodes (OTCE) with specific electrooptical properties. According to our results, these electrodes could be appropriate choices as electrochemical transducers to monitor electrophoretic separations. At the core of this manuscript is the development and critical evaluation of a new optical model to calculate the thickness of the OTCE by variable angle spectroscopic ellipsometry. Such data were complemented with topography and roughness (obtained by atomic force microscopy), electrochemical properties (obtained by cyclic voltammetry), electrical properties (obtained by electrochemical impedance spectroscopy), and structural composition (obtained by Raman spectroscopy). Although the described OTCE were used as substrates to investigate the effect of electrode potential on the real-time adsorption of proteins by ellipsometry, these results could enable the development of other biosensors that can be then integrated into various CE platforms. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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...

Surface monitoring for pitting evolution into uniform corrosion on Cu-Ni-Zn ternary alloy in alkaline chloride solution: ex-situ LCM and in-situ SECM

Science.gov (United States)

Kong, Decheng; Dong, Chaofang; Zheng, Zhaoran; Mao, Feixiong; Xu, Aoni; Ni, Xiaoqing; Man, Cheng; Yao, Jizheng; Xiao, Kui; Li, Xiaogang

2018-05-01

The evolution of the corrosion process on Cu-Ni-Zn alloy in alkaline chloride solution was investigated by in-situ scanning electrochemical microscopy, X-ray photoelectron spectroscopy, and ex-situ laser confocal microscopy, and the effects of ambient temperature and polarization time were also discussed. The results demonstrated a higher pitting nucleation rate and lower pit growth rate at low temperature. The ratio of pit depth to mouth diameter decreased with increasing pit volume and temperature, indicating that pits preferentially propagate in the horizontal direction rather than the vertical direction owing to the presence of corrosion products and deposited copper. The surface current was uniform and stabilized at approximately 2.2 nA during the passive stage, whereas the current increased after the pits were formed with the maximum approaching 3 nA. Increasing the temperature led to an increase in porous corrosion products (CuO, Zn(OH)2, and Ni(OH)2) and significantly increased the rate of transition from pitting to uniform corrosion. Dezincification corrosion was detected by energy dispersive spectrometry, and a mechanism for pitting transition into uniform corrosion induced by dezincification at the grain boundaries is proposed.

Oxidative stabilization of polyacrylonitrile nanofibers and carbon nanofibers containing graphene oxide (GO: a spectroscopic and electrochemical study

Directory of Open Access Journals (Sweden)

İlknur Gergin

2017-08-01

Full Text Available In this study, a precursor for carbon nanofibers (CNF was fabricated via electrospinning and carbonized through a thermal process. Before carbonization, oxidative stabilization should be applied, and the oxidation mechanism also plays an important role during carbonization. Thus, the understanding of the oxidation mechanism is an essential part of the production of CNF. The oxidation process of polyacrylonitrile was studied and nanofiber webs containing graphene oxide (GO are obtained to improve the electrochemical properties of CNF. Structural and morphological characterizations of the webs are carried out by using attenuated total reflectance Fourier transform infrared spectroscopy and Raman spectroscopy, scanning electron microscopy, atomic force microscopy and transmission electron microscopy. Mechanical tests are performed with a dynamic mechanical analyzer, and thermal studies are conducted by using thermogravimetric analysis. Electrochemical impedance spectroscopy, and cyclic voltammetry are used to investigate capacitive behavior of the products. The proposed equivalent circuit model was consistent with charge-transfer processes taking place at interior pores filled with electrolyte.

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)

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.

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.

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.

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

Sensitive Electrochemical Detection of Native and Aggregated x-Synuclein Protein Involved in Parkinson's Disease

NARCIS (Netherlands)

Masarik, Michal; Stobiecka, Agata; Kizek, René; Jelen, Frantisek; Pechan, Zdenk; Hoyer, Wolfgang; Subramaniam, Vinod; Palecek, Emil

2004-01-01

The aggregation of α-synuclein, a 14 kDa protein, is involved in several human neurodegenerative disorders, including Parkinson's disease. We studied native and in vitro aggregated α-synuclein by circular dichroism (CD), atomic force microscopy (AFM) and electrochemical methods. We used constant

Shadow corrosion phenomenon. An out-of-pile study on electrochemical effects

Energy Technology Data Exchange (ETDEWEB)

Weber, Nadine

2017-04-28

galvanic current could be decreased by a CrN coating layer on Inconel 718. Objectives including a deeper knowledge about the corrosion mechanism with its influencing parameters and driving forces by studying Shadow Corrosion with out-of-pile autoclave experiments are listed in chapter 4. A further aim was to test the effectiveness of a possible spacer coating to reduce the corrosion or even to prevent the reactor plant components against Shadow Corrosion. Chapter 5 gives an overview of the experimental part with a description of the materials and chemicals, like Zircaloy and Inconel 718, as well as the specimen preparation techniques, such as etching, pre-oxidation or coating with CrN. Moreover, the three experimental test set-ups used to simulate the different conditions as a function of temperature and water chemistry parameters are depicted. The electrochemical measuring methods including electrochemical corrosion potential (ECP), galvanic corrosion (GC), electrochemical impe-dance spectroscopy (EIS) and conductometry are described. Further methods for surface analyses comprising microscopy, scanning electron microscopy (SEM), focused ion beam (FIB), transmission electron microscopy (TEM), ellipsometry, ion coupled plasma optical emission spectroscopy (ICP-OES) and spectrophotometry are presented. Results and corresponding discussions are summarized in chapter 6, which is divided into three subchapters. Chapter 6.1 deals with electrochemical parameters, like electrochemical corrosion potential, galvanic potential, and galvanic current as well as parameters obtained from electrochemical impedance spectroscopy as a function of different water chemistry parameters. The focus was on the concentration of hydrogen peroxide, the presence of impurities in the form of nitrate, and the exposure to UV-light. Furthermore, surface analyses via the focused ion beam technique and the transmission electron microscopy were gathered to visualize the oxide layer structure, composition

Shadow corrosion phenomenon. An out-of-pile study on electrochemical effects

International Nuclear Information System (INIS)

Weber, Nadine

2017-01-01

N coating layer on Inconel 718. Objectives including a deeper knowledge about the corrosion mechanism with its influencing parameters and driving forces by studying Shadow Corrosion with out-of-pile autoclave experiments are listed in chapter 4. A further aim was to test the effectiveness of a possible spacer coating to reduce the corrosion or even to prevent the reactor plant components against Shadow Corrosion. Chapter 5 gives an overview of the experimental part with a description of the materials and chemicals, like Zircaloy and Inconel 718, as well as the specimen preparation techniques, such as etching, pre-oxidation or coating with CrN. Moreover, the three experimental test set-ups used to simulate the different conditions as a function of temperature and water chemistry parameters are depicted. The electrochemical measuring methods including electrochemical corrosion potential (ECP), galvanic corrosion (GC), electrochemical impe-dance spectroscopy (EIS) and conductometry are described. Further methods for surface analyses comprising microscopy, scanning electron microscopy (SEM), focused ion beam (FIB), transmission electron microscopy (TEM), ellipsometry, ion coupled plasma optical emission spectroscopy (ICP-OES) and spectrophotometry are presented. Results and corresponding discussions are summarized in chapter 6, which is divided into three subchapters. Chapter 6.1 deals with electrochemical parameters, like electrochemical corrosion potential, galvanic potential, and galvanic current as well as parameters obtained from electrochemical impedance spectroscopy as a function of different water chemistry parameters. The focus was on the concentration of hydrogen peroxide, the presence of impurities in the form of nitrate, and the exposure to UV-light. Furthermore, surface analyses via the focused ion beam technique and the transmission electron microscopy were gathered to visualize the oxide layer structure, composition, and thickness after exposure to oxygenated

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.

Effect of preparation methods on dispersion stability and electrochemical performance of graphene sheets

International Nuclear Information System (INIS)

Chen, Li; Li, Na; Zhang, Mingxia; Li, Pinnan; Lin, Zhengping

2017-01-01

Chemical exfoliation is one of the most important strategies for preparing graphene. The aggregation of graphene sheets severely prevents graphene from exhibiting excellent properties. However, there are no attempts to investigate the effect of preparation methods on the dispersity of graphene sheets. In this study, three chemical exfoliation methods, including Hummers method, modified Hummers method, and improved method, were used to prepare graphene sheets. The influence of preparation methods on the structure, dispersion stability in organic solvents, and electrochemical properties of graphene sheets were investigated. Fourier transform infrared microscopy, Raman spectra, transmission electron microscopy, and UV–vis spectrophotometry were employed to analyze the structure of the as-prepared graphene sheets. The results showed that graphene prepared by improved method exhibits excellent dispersity and stability in organic solvents without any additional stabilizer or modifier, which is attributed to the completely exfoliation and regular structure. Moreover, cyclic voltammetric and electrochemical impedance spectroscopy measurements showed that graphene prepared by improved method exhibits superior electrochemical properties than that prepared by the other two methods. - Graphical abstract: Graphene oxides with different oxidation degree were obtained via three methods, and then graphene with different crystal structures were created by chemical reduction of exfoliated graphene oxides. - Highlights: • Graphene oxides with different oxidation degree were obtained via three oxidation methods. • The influence of oxidation methods on microstructure of graphene was investigated. • The effect of oxidation methods on dispersion stability of graphene was investigated. • The effect of oxidation methods on electrochemical properties of graphene was discussed.

Effect of preparation methods on dispersion stability and electrochemical performance of graphene sheets

Energy Technology Data Exchange (ETDEWEB)

Chen, Li, E-mail: chenli1981@lut.cn; Li, Na; Zhang, Mingxia; Li, Pinnan; Lin, Zhengping

2017-05-15

Chemical exfoliation is one of the most important strategies for preparing graphene. The aggregation of graphene sheets severely prevents graphene from exhibiting excellent properties. However, there are no attempts to investigate the effect of preparation methods on the dispersity of graphene sheets. In this study, three chemical exfoliation methods, including Hummers method, modified Hummers method, and improved method, were used to prepare graphene sheets. The influence of preparation methods on the structure, dispersion stability in organic solvents, and electrochemical properties of graphene sheets were investigated. Fourier transform infrared microscopy, Raman spectra, transmission electron microscopy, and UV–vis spectrophotometry were employed to analyze the structure of the as-prepared graphene sheets. The results showed that graphene prepared by improved method exhibits excellent dispersity and stability in organic solvents without any additional stabilizer or modifier, which is attributed to the completely exfoliation and regular structure. Moreover, cyclic voltammetric and electrochemical impedance spectroscopy measurements showed that graphene prepared by improved method exhibits superior electrochemical properties than that prepared by the other two methods. - Graphical abstract: Graphene oxides with different oxidation degree were obtained via three methods, and then graphene with different crystal structures were created by chemical reduction of exfoliated graphene oxides. - Highlights: • Graphene oxides with different oxidation degree were obtained via three oxidation methods. • The influence of oxidation methods on microstructure of graphene was investigated. • The effect of oxidation methods on dispersion stability of graphene was investigated. • The effect of oxidation methods on electrochemical properties of graphene was discussed.

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 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

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

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.

Electrochemical performance studies of MnO2 nanoflowers recovered from spent battery

International Nuclear Information System (INIS)

Ali, Gomaa A.M.; Tan, Ling Ling; Jose, Rajan; Yusoff, Mashitah M.; Chong, Kwok Feng

2014-01-01

Highlights: • MnO 2 is recovered from spent zinc–carbon batteries as nanoflowers structure. • Recovered MnO 2 nanoflowers show high specific capacitance. • Recovered MnO 2 nanoflowers show stable electrochemical cycling up to 900 cycles. • Recovered MnO 2 nanoflowers show low resistance in EIS data. - Abstract: The electrochemical performance of MnO 2 nanoflowers recovered from spent household zinc–carbon battery is studied by cyclic voltammetry, galvanostatic charge/discharge cycling and electrochemical impedance spectroscopy. MnO 2 nanoflowers are recovered from spent zinc–carbon battery by combination of solution leaching and electrowinning techniques. In an effort to utilize recovered MnO 2 nanoflowers as energy storage supercapacitor, it is crucial to understand their structure and electrochemical performance. X-ray diffraction analysis confirms the recovery of MnO 2 in birnessite phase, while electron microscopy analysis shows the MnO 2 is recovered as 3D nanostructure with nanoflower morphology. The recovered MnO 2 nanoflowers exhibit high specific capacitance (294 F g −1 at 10 mV s −1 ; 208.5 F g −1 at 0.1 A g −1 ) in 1 M Na 2 SO 4 electrolyte, with stable electrochemical cycling. Electrochemical data analysis reveal the great potential of MnO 2 nanoflowers recovered from spent zinc–carbon battery in the development of high performance energy storage supercapacitor system

GOX-functionalized nanodiamond films for electrochemical biosensor

Energy Technology Data Exchange (ETDEWEB)

Villalba, Pedro [Department of Chemical and Biomedical Engineering, University of South Florida (United States); Departamento de Medicina, Universidad del Norte, Barranquilla (Colombia); Ram, Manoj K., E-mail: mkram@usf.edu [Department of Mechanical Engineering, University of South Florida, 4202 E Fowler Avenue, Tampa, FL, 33620-5350 (United States); Nanotechnology Research and Education Center, University of South Florida (United States); Gomez, Humberto [Department of Mechanical Engineering, University of South Florida, 4202 E Fowler Avenue, Tampa, FL, 33620-5350 (United States); Departamento de Medicina, Universidad del Norte, Barranquilla (Colombia); Kumar, Amrita [Department of Physiology, Emory University. Atlanta GA (United States); Bhethanabotla, Venkat [Department of Chemical and Biomedical Engineering, University of South Florida (United States); Kumar, Ashok [Department of Mechanical Engineering, University of South Florida, 4202 E Fowler Avenue, Tampa, FL, 33620-5350 (United States); Nanotechnology Research and Education Center, University of South Florida (United States)

2011-07-20

The importance of nanodiamond in biological and technological applications has been recognized recently, and applied in drug delivery, biochip, sensors and biosensors. Under this investigation, nanodiamond (ND) and nitrogen doped nanodiamond (NND) were deposited on n-type silicon films, and later functionalized with enzyme Glucose oxidase (GOX). The GOX functionalized doped and undoped ND films were characterized using combination of several techniques; i.e. FTIR spectroscopy, Raman spectroscopy, atomic force microscopy (AFM) and electrochemical techniques. ND/GOX and NND/GOX thin films on n-type silicon have been found to provide sensitive glucose sensor. GOX has been chosen as a model enzyme system to functionalize with ND at molecular level to understand the glucose biosensor. - Research highlights: {yields} Nanodiamond (ND) films were used as an enzyme electrode for glucose quantification. {yields} Electrochemical behavior of doped and intrinsic films was analyzed. {yields} Electrode demonstrates sensitivity to glucose concentration in dynamic condition. {yields} Linear behavior was observed upto 8mM before saturation condition.

GOX-functionalized nanodiamond films for electrochemical biosensor

International Nuclear Information System (INIS)

Villalba, Pedro; Ram, Manoj K.; Gomez, Humberto; Kumar, Amrita; Bhethanabotla, Venkat; Kumar, Ashok

2011-01-01

The importance of nanodiamond in biological and technological applications has been recognized recently, and applied in drug delivery, biochip, sensors and biosensors. Under this investigation, nanodiamond (ND) and nitrogen doped nanodiamond (NND) were deposited on n-type silicon films, and later functionalized with enzyme Glucose oxidase (GOX). The GOX functionalized doped and undoped ND films were characterized using combination of several techniques; i.e. FTIR spectroscopy, Raman spectroscopy, atomic force microscopy (AFM) and electrochemical techniques. ND/GOX and NND/GOX thin films on n-type silicon have been found to provide sensitive glucose sensor. GOX has been chosen as a model enzyme system to functionalize with ND at molecular level to understand the glucose biosensor. - Research highlights: → Nanodiamond (ND) films were used as an enzyme electrode for glucose quantification. → Electrochemical behavior of doped and intrinsic films was analyzed. → Electrode demonstrates sensitivity to glucose concentration in dynamic condition. → Linear behavior was observed upto 8mM before saturation condition.

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.

Dual harmonic Kelvin probe force microscopy at the graphene–liquid interface

International Nuclear Information System (INIS)

Collins, Liam; Rodriguez, Brian J.; Kilpatrick, Jason I.; Weber, Stefan A. L.; Vlassiouk, Ivan V.; Tselev, Alexander; Jesse, Stephen; Kalinin, Sergei V.

2014-01-01

Kelvin probe force microscopy (KPFM) is a powerful technique for the determination of the contact potential difference (CPD) between an atomic force microscope tip and a sample under ambient and vacuum conditions. However, for many energy storage and conversion systems, including graphene-based electrochemical capacitors, understanding electrochemical phenomena at the solid–liquid interface is paramount. Despite the vast potential to provide fundamental insight for energy storage materials at the nanoscale, KPFM has found limited applicability in liquid environments to date. Here, using dual harmonic (DH)-KPFM, we demonstrate CPD imaging of graphene in liquid. We find good agreement with measurements performed in air, highlighting the potential of DH-KPFM to probe electrochemistry at the graphene–liquid interface

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)

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.

Electrochemical Behavior of Pure Copper in Phosphate Buffer Solutions: A Comparison Between Micro- and Nano-Grained Copper

Science.gov (United States)

Imantalab, O.; Fattah-alhosseini, A.; Keshavarz, M. K.; Mazaheri, Y.

2016-02-01

In this work, electrochemical behavior of annealed (micro-) and nano-grained pure copper (fabricated by accumulative roll bonding process) in phosphate buffer solutions of various pH values ranging from 10.69 to 12.59 has been studied. Before any electrochemical measurements, evaluation of microstructure was obtained by optical microscope and transmission electron microscopy. To investigate the electrochemical behavior of the samples, the potentiodynamic polarization, Mott-Schottky analysis, and electrochemical impedance spectroscopy (EIS) were carried out. Potentiodynamic polarization plots and EIS measurements revealed that as a result of grain refinement, the passive behavior of the nano-grained sample was improved compared to that of annealed pure copper. Also, Mott-Schottky analysis indicated that the passive films behaved as p-type semiconductors and grain refinement did not change the semiconductor type of passive films.

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

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.

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

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

Effect of Ce addition on the mechanical and electrochemical properties of a lithium battery shell alloy

Energy Technology Data Exchange (ETDEWEB)

Zhang, Junchao [School of Materials Science and Engineering, Shanghai Jiao Tong University, Shanghai 200240 (China); Ding, Dongyan, E-mail: dyding@sjtu.edu.cn [School of Materials Science and Engineering, Shanghai Jiao Tong University, Shanghai 200240 (China); Xu, Xinglong [School of Materials Science and Engineering, Shanghai Jiao Tong University, Shanghai 200240 (China); Gao, Yongjin; Chen, Guozhen; Chen, Weigao; You, Xiaohua [Huafon NLM Al Co., Ltd, Shanghai 201506 (China); Huang, Yuanwei; Tang, Jinsong [Shanghai Huafon Materials Technology Institute, Shanghai 201203 (China)

2014-12-25

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{sub 8}Cu{sub 4}Ce phase and many Al{sub 20}Cu{sub 2}Mn{sub 3} particles could be found. In addition, the precipitation of conventionally dominant phase of Al{sub 2}Cu could be suppressed in alloy. The Ce addition was found to result in enhanced tensile strength and improved corrosion resistance.

The investigation on electrochemical reaction mechanism of CuF2 thin film with lithium

International Nuclear Information System (INIS)

Cui Yanhua; Xue Mingzhe; Zhou Yongning; Peng Shuming; Wang Xiaolin; Fu Zhengwen

2011-01-01

Crystalline CuF 2 thin films were prepared by pulsed laser deposition under room temperature. The physical and electrochemical properties of the as-deposited thin films have been investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), galvanostatic cycling and cyclic voltammetry (CV). Reversible capacity of 544 mAh g -1 was achieved in the potential range of 1.0-4.0 V. A reversible couple of redox peaks at 3.0 V and 3.7 V was firstly observed. By using ex situ XRD and TEM techniques, an insertion process followed by a fully conversion reaction to Cu and LiF was revealed in the lithium electrochemical reaction of CuF 2 thin film electrode. The reversible insertion reaction above 2.8 V could provide a capacity of about 125 mAh g -1 , which makes CuF 2 a potential cathode material for rechargeable lithium batteries.

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.

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

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

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

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.

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.

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 Polishing Applications and EIS of a Vitamin B4-Based Ionic Liquid

International Nuclear Information System (INIS)

Wixtrom, Alex I.; Buhler, Jessica E.; Reece, Charles E.; Abdel-Fattah, Tarek M.

2013-01-01

Modern particle accelerators require minimal interior surface roughness for Niobium superconducting radio frequency (SRF) cavities. Polishing of the Nb is currently achieved via electrochemical polishing with concentrated mixtures of sulfuric and hydrofluoric acids. This acid-based approach is effective at reducing the surface roughness to acceptable levels for SRF use, but due to acid-related hazards and extra costs (including safe disposal of used polishing solutions), an acid-free method would be preferable. This study focuses on an alternative electrochemical polishing method for Nb, using a novel ionic liquid solution containing choline chloride, also known as Vitamin B 4 (VB 4 ). Potentiostatic electrochemical impedance spectroscopy (EIS) was also performed on the VB4-based system. Nb polished using the VB4-based method was found to have a final surface roughness comparable to that achieved via the acid-based method, as assessed by atomic force microscopy (AFM). These findings indicate that acid-free VB 4 -based electrochemical polishing of Nb represents a promising replacement for acid-based methods of SRF cavity preparation

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

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)

Facile route to covalently-jointed graphene/polyaniline composite and it's enhanced electrochemical performances for supercapacitors

Science.gov (United States)

Qiu, Hanxun; Han, Xuebin; Qiu, Feilong; Yang, Junhe

2016-07-01

A polyaniline/graphene composite with covalently-bond is synthesized by a novel approach. In this way, graphene oxide is functionalized firstly by introducing amine groups onto the surface with the reduction of graphene oxide in the process and then served as the anchor sites for the growth of polyaniline (PANI) via in-situ polymerization. The composite material is characterized by electron microscopy, the resonant Raman spectra, X-ray diffraction, transform infrared spectroscopy and X-ray photoelectron spectroscopy. The electrochemical properties of the composite are measured by cyclic voltammetry, electrochemical impedance spectroscopy and galvanostatic charging/discharging. With the functionalization process, the graphene/polyaniline composite electrode exhibits remarkably enhanced electrochemical performance with specific capacitance of 489 F g-1 at 0.5 A g-1, which is superior to those of its individual components. The outstanding electrochemical performance of the hybrid can be attributed to its covalently synergistic effect between graphene and polyaniline, suggesting promising potentials for supercapacitors.

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

The preparation and electrochemical performances of LiFePO4-multiwalled nanotubes composite cathode materials for lithium ion batteries

International Nuclear Information System (INIS)

Feng Yan

2010-01-01

LiFePO 4 -MWCNTs (multi-walled carbon nanotubes) composite cathode materials were prepared by mixing LiFePO 4 and MWCNTs in ethanol followed by heat-treatment at 500 deg. C for 5 h. The structural, morphology and electrochemical performances of LiFePO 4 -MWCNTs composite materials were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), galvanostatic charge-discharge cycle tests, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The results indicated that MWCNTs adding improved the electronic conductivity, the discharge capacity, cycle stability and lithium ion diffusion kinetics of LiFePO 4 , but MWCNTs adding did not charge the orthorhombic olivine-type structure of LiFePO 4 . In all these prepared LiFePO 4 with x wt.% MWCNTs (x = 4, 7, 10) composites, 7 wt.% MWCNTs adding composite cathode shows the best electrochemical performance, which gets an initial discharge capacity of 152.7 mAh g -1 at 0.18 C discharge rates with capacity retention ratio of 97.77% after 100 cycles.

One step electrochemical synthesis of bimetallic PdAu supported on nafion–graphene ribbon film for ethanol electrooxidation

Energy Technology Data Exchange (ETDEWEB)

Shendage, Suresh S., E-mail: sureshsshendage@gmail.com; Singh, Abilash S.; Nagarkar, Jayashree M., E-mail: jm.nagarkar@ictmumbai.edu.in

2015-10-15

Highlights: • Electrochemical deposition of bimetallic PdAu NPs. • Highly loaded PdAu NPs are obtained. • Nafion–graphene supported PdAu NPs shows good activity for ethanol electrooxidation. - Abstract: A nafion–graphene ribbon (Nf–GR) supported bimetallic PdAu nanoparticles (PdAu/Nf–GR) catalyst was prepared by electrochemical codeposition of Pd and Au at constant potential. The prepared catalyst was characterized by scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), transmission electron microscopy (TEM) and X-ray diffraction analysis (XRD). The average particle size of PdAu nanoparticles (NPs) determined from XRD was 3.5 nm. The electrocatalytic activity of the PdAu/Nf–GR catalyst was examined by cyclic voltametry. It was observed that the as prepared catalyst showed efficient activity and good stability for ethanol electrooxidation in alkaline medium.

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.

Electrochemical reactivity of Co-Li2S nanocomposite for lithium-ion batteries

International Nuclear Information System (INIS)

Zhou, Yongning; Wu, Changliang; Zhang, Hua; Wu, Xiaojing; Fu, Zhengwen

2007-01-01

The fabrication of Co-Li 2 S nanocomposite thin film is reported by pulsed laser deposition (PLD) for the first time. Li 2 S-Co nanocomposite thin film is used as storing Li electrodes that have led to promising electrochemical activity and good electrochemical performance. The releasing Li process from the as-deposited Li 2 S-Co nanocomposite thin films is confirmed by the ex situ high resolution transmission electron microscopy (HR-TEM) and selected area electron diffraction (SAED) measurements and may come from the decomposition of Li 2 S with and without the interaction of metal Co into CoS 2 and S. The electrochemical reaction mechanism of Co-Li 2 S nanocomposite film electrode involving both the formation and decomposition of Li 2 S and the lithium extraction/insertion of CoS 2 after the initial charging process is proposed. Our results demonstrate the advantages of using Co-Li 2 S nanocomposite in storage lithium materials

Real-time studies of battery electrochemical reactions inside a transmission electron microscope.

Energy Technology Data Exchange (ETDEWEB)

Leung, Kevin; Hudak, Nicholas S.; Liu, Yang; Liu, Xiaohua H.; Fan, Hongyou; Subramanian, Arunkumar; Shaw, Michael J.; Sullivan, John Patrick; Huang, Jian Yu

2012-01-01

We report the development of new experimental capabilities and ab initio modeling for real-time studies of Li-ion battery electrochemical reactions. We developed three capabilities for in-situ transmission electron microscopy (TEM) studies: a capability that uses a nanomanipulator inside the TEM to assemble electrochemical cells with ionic liquid or solid state electrolytes, a capability that uses on-chip assembly of battery components on to TEM-compatible multi-electrode arrays, and a capability that uses a TEM-compatible sealed electrochemical cell that we developed for performing in-situ TEM using volatile battery electrolytes. These capabilities were used to understand lithiation mechanisms in nanoscale battery materials, including SnO{sub 2}, Si, Ge, Al, ZnO, and MnO{sub 2}. The modeling approaches used ab initio molecular dynamics to understand early stages of ethylene carbonate reduction on lithiated-graphite and lithium surfaces and constrained density functional theory to understand ethylene carbonate reduction on passivated electrode surfaces.

Non-aqueous electrochemical deposition of lead zirconate titanate films for flexible sensor applications

Science.gov (United States)

Joseph, Sherin; Kumar, A. V. Ramesh; John, Reji

2017-11-01

Lead zirconate titanate (PZT) is one of the most important piezoelectric materials widely used for underwater sensors. However, PZTs are hard and non-compliant and hence there is an overwhelming attention devoted toward making it flexible by preparing films on flexible substrates by different routes. In this work, the electrochemical deposition of composition controlled PZT films over flexible stainless steel (SS) foil substrates using non-aqueous electrolyte dimethyl sulphoxide (DMSO) was carried out. Effects of various key parameters involved in electrochemical deposition process such as current density and time of deposition were studied. It was found that a current density of 25 mA/cm2 for 5 min gave a good film. The morphology and topography evaluation of the films was carried out by scanning electron microscopy (SEM) and atomic force microscopy (AFM), respectively, which showed a uniform morphology with a surface roughness of 2 nm. The PZT phase formation was studied using X-ray diffraction (XRD) and corroborated with Raman spectroscopic studies. The dielectric constant, dielectric loss, hysteresis and I-V characteristics of the film was evaluated.

Atomic force microscopy study of anion intercalation into highly oriented pyrolytic graphite

Energy Technology Data Exchange (ETDEWEB)

Alliata, D; Haering, P; Haas, O; Koetz, R [Paul Scherrer Inst. (PSI), Villigen (Switzerland); Siegenthaler, H [University of Berne (Switzerland)

1999-08-01

In the context of ion transfer batteries, we studied highly oriented pyrolytic graphite (HOPG) in perchloric acid, as a model to elucidate the mechanism of electrochemical intercalation in graphite. Aim of the work is the local and time dependent investigation of dimensional changes of the host material during electrochemical intercalation processes on the nanometer scale. We used atomic force microscopy (AFM), combined with cyclic voltammetry, as in-situ tool of analysis during intercalation and expulsion of perchloric anions into the HOPG electrodes. According to the AFM measurements, the HOPG interlayer spacing increases by 32% when perchloric anions intercalate, in agreement with the formation of stage IV of graphite intercalation compounds. (author) 3 figs., 3 refs.

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 detection of uric acid using ruthenium-dioxide-coated carbon nanotube directly grown onto Si wafer

Science.gov (United States)

Shih, Yi-Ting; Lee, Kuei-Yi; Lin, Chung-Kuang

2015-12-01

Carbon nanotubes (CNTs) directly grown onto a Si substrate by thermal chemical vapor deposition were used in uric acid (UA) detection. The process is simple and formation is easy without the need for additional chemical treatments. However, CNTs lack selectivity and sensitivity to UA. To enhance the electrochemical analysis, ruthenium oxide was used as a catalytic mediator in the modification of electrodes. The electrochemical results show that RuO2 nanostructures coated onto CNTs can strengthen the UA signal. The peak currents of RuO2 nanostructures coated onto CNTs linearly increase with increasing UA concentration, meaning that they can work as electrodes for UA detection. The lowest detection limit and highest sensitivity were 55 nM and 4.36 µA/µM, respectively. Moreover, the characteristics of RuO2 nanostructures coated onto CNTs were examined by scanning electron microscopy, transmission electron microscopy, and Raman spectroscopy.

Electrochemical Oxidation of Cyanide Using Platinized Ti Electrodes

Directory of Open Access Journals (Sweden)

Aušra VALIŪNIENĖ

2013-12-01

Full Text Available The cyanide-containing effluents are dangerous ecological hazards and must be treated before discharging into the environment. Anodic oxidation is one of the best ways to degrade cyanides. Pt anodes as the most efficient material for the cyanide electrochemical degradation are widely used. However, these electrodes are too expensive for industrial purposes. In this work Ti electrodes covered with nano-sized Pt particle layer were prepared and used for the anodic oxidation of cyanide ions. Surface images of Ti electrodes and Ti electrodes covered with different thickness layer of Pt were compared and characterized by the atomic force microscopy (AFM. The products formed in the solution during the CN- ions electrooxidation were examined by the Raman spectroscopy. An electrochemical Fast Fourier transformation (FFT impedance spectroscopy was used to estimate the parameters that reflect real surface roughness of Pt-modified Ti electrodes.DOI: http://dx.doi.org/10.5755/j01.ms.19.4.2514

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

Synthesis of bismuth sulfide/reduced graphene oxide composites and their electrochemical properties for lithium ion batteries

International Nuclear Information System (INIS)

Zhang, Zhian; Zhou, Chengkun; Huang, Lei; Wang, Xiwen; Qu, Yaohui; Lai, Yanqing; Li, Jie

2013-01-01

Graphical abstract: The Bi 2 S 3 /reduced graphene oxide composites were synthesized by a one-pot hydrothermal route and exhibited an extraordinary capacity of 1073.1 mAh g −1 with excellent cycling stability and high rate capability as anode material of lithium ion battery. The enhancement in the electrochemical performance could be attributed to the introduction of RGO sheets that not only buffer the large volume changes during the alloy/dealloy reaction of Li and Bi, but also provide a highly conductive network for rapid electron transport in electrode during electrochemical reaction. -- Highlights: •Bi 2 S 3 /RGO composites were in situ prepared by one-pot hydrothermal route. •The Bi 2 S 3 nanoparticles are homogeneous dispersion on the RGO sheets. •Bi 2 S 3 /RGO exhibits excellent cycling stability and high rate capability. •This work will also of interest for supercapacitor and solar cells. -- Abstract: A simple one-pot hydrothermal route was developed to synthesize bismuth sulfide/reduced graphene oxide composites (Bi 2 S 3 /RGO composites) in this work. The morphology and crystalline structure of the obtained products were investigated by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and high resolution transmission electron microscopy (HRTEM). The results of Raman spectra and Fourier transform infrared (FTIR) spectra demonstrated that graphite oxide (GO) sheets were in situ reduced to a certain extent. Transmission electron microscopy (TEM) observation indicated that the Bi 2 S 3 nanoparticles, with a size of 80–100 nm in length, are anchored on RGO sheets. Electrochemical tests show the Bi 2 S 3 /RGO composite exhibits an extraordinary capacity of 1073.1 mAh g −1 with excellent cycling stability and high rate capability compared to pure Bi 2 S 3 particles prepared by a similar route in the absence of GO. The enhancement in the electrochemical performance could be attributed to the introduction of RGO sheets

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

Towards the use of protein A-tagged gold nanoparticles for signal amplification of electrochemical immunosensors in virus detection

International Nuclear Information System (INIS)

Huy Tran, Quang; Thuy Nguyen, Thanh; Chung Pham, Van; Hong Hanh Nguyen, Thi; Tuan Mai, Anh

2012-01-01

In this paper we represent a study on the potential use of protein A-tagged gold nanoparticles applied for signal amplification of electrochemical immunosensors. Gold nanoparticles (GNPs) were synthesized by the chemical reduction of tetrachloroauric (III) acid trihydrate using sodium ascorbate, and then tagged with protein A (PrA) via ultracentrifugation. UV-Vis spectroscopy and transmission electron microscopy were used to verify the characteristics of formed GNPs/PrA complex. The analyzed results indicate that GNPs were found spherically, homogeneously, and with an average diameter of about 10 nm. Immunoelectron microscopy was then used to investigate the bioactivity of the GNPs/PrA complex in solution by the effective binding of GNPs to viral particles. Scanning electron and fluorescence microscopies were also used to investigate the distribution and the bioactivity of the GNPs/PrA complex on the surface of the interdigitated sensor. Consequently, this study provided some assumptions of the potential application of protein A-tagged gold nanoparticles for signal amplification of electrochemical immunosensors in virus detection from clinical samples

Controlled amino-functionalization by electrochemical reduction of bromo and nitro azobenzene layers bound to Si(111) surfaces

NARCIS (Netherlands)

Ullien, D.; Thüne, P.C.; Jager, W.F.; Sudhölter, E.J.R.; De Smet, L.C.P.M.

2014-01-01

4-Nitrobenzenediazonium (4-NBD) and 4-bromobenzenediazonium (4-BBD) salts were grafted electrochemically onto H-terminated, p-doped silicon (Si) surfaces. Atomic force microscopy (AFM) and ellipsometry experiments clearly showed layer thicknesses of 2–7 nm, which indicate multilayer formation.

Fabrication of a novel PbO2 electrode with a graphene nanosheet interlayer for electrochemical oxidation of 2-chlorophenol

International Nuclear Information System (INIS)

Duan, Xiaoyue; Zhao, Cuimei; Liu, Wei; Zhao, Xuesong; Chang, Limin

2017-01-01

Highlights: • A novel PbO 2 electrode with a GNS interlayer (GSN-PbO 2 ) was prepared. • The GNS interlayer reduced grain size of β-PbO 2 crystals. • The GNS interlayer enhanced electrochemical activity of PbO 2 electrode. • The lifetime of GSN-PbO 2 electrode was 1.93 times that of PbO 2 electrode. • An electrochemical mineralization mechanism of 2-chlorophenol was proposed. - Abstract: A novel PbO 2 electrode with a graphene nanosheet interlayer (marked as GNS-PbO 2 ) was prepared combining electrophoretic deposition and electro-deposition technologies. The micro morphology, crystal structure and surface chemical states of GNS-PbO 2 electrodes were characterized using scanning electronic microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). Their electrochemical properties and stability were determined using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), ·OH radicals test and accelerated life test, and compared with traditional PbO 2 electrodes. Besides, their potential application in the electrochemical degradation of 2-chlorophenol (2-CP) was investigated. The GNS-PbO 2 electrode possessed perfect octahedral β-PbO 2 microcrystals, and its grain size was much smaller than that of traditional PbO 2 electrode. It exhibited higher electrochemical activity than traditional PbO 2 electrode due to its larger electrochemical active surface area and stronger ·OH radicals generation ability. The service lifetime of GNS-PbO 2 electrode (107.9 h) was 1.93 times longer than that of traditional PbO 2 electrode (55.9 h). The electrochemical degradation rate constant of 2-CP on GNS-PbO 2 electrode (k app = 2.75 × 10 −2 min −1 ) is much higher than for PbO 2 electrode (k app = 1.76 × 10 −2 min −1 ). 2-CP oxidation yielded intermediates including aromatic compounds (catechol, phenol and ortho-benzoquinone) and organic acids (oxalic acid, maleic acid and

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.

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.

Electrochemical and surface characterisation of carbon-film-coated piezoelectric quartz crystals

International Nuclear Information System (INIS)

Pinto, Edilson M.; Gouveia-Caridade, Carla; Soares, David M.; Brett, Christopher M.A.

2009-01-01

The electrochemical properties of carbon films, of thickness between 200 and 500 nm, sputter-coated on gold- and platinum-coated 6 MHz piezoelectric quartz crystal oscillators, as new electrode materials have been investigated. Comparative studies under the same experimental conditions were performed on bulk electrodes. Cyclic voltammetry was carried out in 0.1 M KCl electrolyte solution, and kinetic parameters of the model redox systems Fe(CN) 6 3-/4- and [Ru(NH 3 ) 6 ] 3+/2+ as well as the electroactive area of the electrodes were obtained. Atomic force microscopy was used in order to examine the surface morphology of the films, and the properties of the carbon films and the electrode-solution interface were studied by electrochemical impedance spectroscopy. The results obtained demonstrate the feasibility of the preparation and development of nanometer thick carbon film modified quartz crystals. Such modified crystals should open up new opportunities for the investigation of electrode processes at carbon electrodes and for the application of electrochemical sensing associated with the EQCM.

A highly sensitive electrochemical sensor for the determination of methanol based on PdNPs@SBA-15-PrEn modified electrode.

Science.gov (United States)

Karimi, Ziba; Shamsipur, Mojtaba; Tabrizi, Mahmoud Amouzadeh; Rostamnia, Sadegh

2018-05-01

In this study, a novel electrochemical sensor for the determination of methanol based on palladium nanoparticles supported on Santa barbara amorphous-15- PrNHEtNH 2 (PdNPs@SBA-15-PrEn) as nanocatalysis platform is presented. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and electrochemical methods are employed to characterize the PdNPs@SBA-15-PrEn nanocomposite. The Nafion-Pd@SBA-15-PrEn modified glassy carbon electrode (Nafion-PdNPs@SBA-15-PrEn/GCE) displayed the high electrochemical activity and excellent catalytic characteristic for electro-oxidation of methanol in an alkaline solution. The electro-oxidation performance of the proposed sensor was investigated using cyclic voltammetry (CV) and amperometry. The sensor exhibits a good sensitivity of 0.0905 Amol -1 Lcm -2 , linear range of 20-1000 μM and the corresponding detection limit of 12 μM (3σ). The results demonstrate that the Nafion-PdNPs@SBA-15-PrEn/GCE has potential as an efficient and integrated sensor for methanol detection. Copyright © 2018 Elsevier Inc. All rights reserved.

Fabrication and electrochemical behavior of single-walled carbon nanotube/graphite-based electrode

International Nuclear Information System (INIS)

Moghaddam, Abdolmajid Bayandori; Ganjali, Mohammad Reza; Dinarvand, Rassoul; Razavi, Taherehsadat; Riahi, Siavash; Rezaei-Zarchi, Saeed; Norouzi, Parviz

2009-01-01

An electrochemical method for determining the dihydroxybenzene derivatives on glassy carbon (GC) has been developed. In this method, the performance of a single-walled carbon nanotube (SWCNT)/graphite-based electrode, prepared by mixing SWCNTs and graphite powder, was described. The resulting electrode shows an excellent behavior for redox of 3,4-dihydroxybenzoic acid (DBA). SWCNT/graphite-based electrode presents a significant decrease in the overvoltage for DBA oxidation as well as a dramatic improvement in the reversibility of DBA redox behavior in comparison with graphite-based and glassy carbon (GC) electrodes. In addition, scanning electron microscopy (SEM) and atomic force microscopy (AFM) procedures performed for used SWCNTs

In situ electrochemical atomic force microscope study on graphite electrodes

Energy Technology Data Exchange (ETDEWEB)

Hirasawa, K.A.; Sato, Tomohiro; Asahina, Hitoshi; Yamaguchi, Shoji; Mori, Shoichiro [Mitsubishi Chemical Corp., Inashiki, Ibaraki (Japan). Tsukuba Research Center

1997-04-01

Interest in the formation of the solid electrolyte interphase (SEI) film on graphite electrodes has increased recently in the quest to improve the performance of lithium-ion batteries. Topographic and frictional changes on the surface of a highly oriented pyrolytic graphite electrode in 1 M LiCiO{sub 4} ethylene carbonate/ethylmethyl carbonate (1:1) electrolyte were examined during charge and discharge by in situ electrochemical atomic force microscopy and friction force microscopy simultaneously in real-time. Solid electrolyte interphase film formation commenced at approximately 2 V vs. Li/Li{sup +} and stable film formation with an island-like morphology was observed below approximately 0.9 V vs. Li/Li{sup +}. Further experiments on a KS-44 graphite/polyvinylidene difluoride binder composite electrode showed similar phenomena.

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

Detection of nicotine based on molecularly imprinted TiO{sub 2}-modified electrodes

Energy Technology Data Exchange (ETDEWEB)

Wu, C.-T.; Chen, P.-Y.; Chen, J.-G.; Suryanarayanan, Vembu [Department of Chemical Engineering, National Taiwan University, Taipei 10617, Taiwan (China); Ho, K.-C. [Department of Chemical Engineering, National Taiwan University, Taipei 10617, Taiwan (China); Institute of Polymer Science and Engineering, National Taiwan University, Taipei 10617, Taiwan (China)], E-mail: kcho@ntu.edu.tw

2009-02-02

Amperometric detection of nicotine (NIC) was carried out on a titanium dioxide (TiO{sub 2})/poly(3,4-ethylenedioxythiophene) (PEDOT)-modified electrode by a molecular imprinting technique. In order to improve the conductivity of the substrate, PEDOT was coated onto the sintered electrode by in situ electrochemical polymerization of the monomer. The sensing potential of the NIC-imprinted TiO{sub 2} electrode (ITO/TiO{sub 2}[NIC]/PEDOT) in a phosphate-buffered saline (PBS) solution (pH 7.4) containing 0.1 M KCl was determined to be 0.88 V (vs. Ag/AgCl/saturated KCl). The linear detection range for NIC oxidation on the so-called ITO/TiO{sub 2}[NIC]/PEDOT electrode was 0-5 mM, with a sensitivity and limit of detection of 31.35 {mu}A mM{sup -1} cm{sup -2} and 4.9 {mu}M, respectively. When comparing with the performance of the non-imprinted one, the sensitivity ratio was about 1.24. The sensitivity enhancement was attributed to the increase in the electroactive area of the imprinted electrode. The at-rest stability of the ITO/TiO{sub 2}[NIC]/PEDOT electrode was tested over a period of 3 days. The current response remained about 85% of its initial value at the end of 2 days. The ITO/TiO{sub 2}[NIC]/PEDOT electrode showed reasonably good selectivity in distinguishing NIC from its major interferent, (-)-cotinine (COT). Moreover, scanning electrochemical microscopy (SECM) was employed to elucidate the surface morphology of the imprinted and non-imprinted electrodes using Fe(CN){sub 6}{sup 3-}/Fe(CN){sub 6}{sup 4-} as a redox probe on a platinum tip. The imprinted electrode was further characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR)

Direct electrochemistry and electrocatalysis of lobetyolin via magnetic functionalized reduced graphene oxide film fabricated electrochemical sensor

International Nuclear Information System (INIS)

Sun, Bolu; Gou, Xiaodan; Bai, Ruibin; Abdelmoaty, Ahmed Attia Ahmed; Ma, Yuling; Zheng, Xiaoping; Hu, Fangdi

2017-01-01

A novel lobetyolin electrochemical sensor based on a magnetic functionalized reduced graphene oxide/Nafion nanohybrid film has been introduced in this work. The magnetic functionalized reduced graphene oxide was characterized by fourier transform infrared spectroscopy, atomic force microscope, X-ray diffraction, transmission electron microscopy and thermogravimetric analysis. The scanning electron microscopy characterized the morphology and microstructure of the prepared sensors, and the electrochemical effective surface areas of the prepared sensors were also calculated by chronocoulometry method. The electrochemical behavior of lobetyolin on the magnetic functionalized reduced graphene oxide/Nafion nanohybrid modified glassy carbon electrode was investigated by cyclic voltammetry and differential pulse voltammetry in a phosphate buffer solution of pH 6.0. The electron-transfer coefficient (α), electron transfer number (n), and electrode reaction rate constant (Κs) were calculated as 0.78, 0.73, and 4.63 s −1 , respectively. Under the optimized conditions, the sensor based on magnetic functionalized reduced graphene oxide/Nafion showed a linear voltammetric response to the lobetyolin concentration at 1.0 × 10 −7 to 1.0 × 10 −4 mol/L with detection limit (S/N = 3)of 4.3 × 10 −8 mol/L. The proposed sensor also displayed acceptable reproducibility, long-term stability, and high selectivity, and performs well for analysis of lobetyolin in real samples. The voltammetric sensor was successfully applied to detect lobetyolin in Codonopsis pilosula with recovery values in the range of 96.12% –102.66%. - Graphical abstract: Schematic diagram of the synthesis of MrGO hybrid and the fabrication process of the MrGO/Nafion/GCE for determination of lobetyolin. Display Omitted - Highlights: • The MrGO/Nafion@GCE electrochemical sensor was successfully fabricated. • The prepared MrGO was characterized by AFM, XRD, FTIR, VSM, TEM and SEM. • The proposed

Direct electrochemistry and electrocatalysis of lobetyolin via magnetic functionalized reduced graphene oxide film fabricated electrochemical sensor

Energy Technology Data Exchange (ETDEWEB)

Sun, Bolu [School of Pharmacy, Lanzhou University, Lanzhou 730000 (China); Gou, Xiaodan [School of Chemistry and Chemical Engineering, Nanjing University, 210046 (China); Bai, Ruibin; Abdelmoaty, Ahmed Attia Ahmed; Ma, Yuling; Zheng, Xiaoping [School of Pharmacy, Lanzhou University, Lanzhou 730000 (China); Hu, Fangdi, E-mail: hufd@lzu.edu.cn [School of Pharmacy, Lanzhou University, Lanzhou 730000 (China)

2017-05-01

A novel lobetyolin electrochemical sensor based on a magnetic functionalized reduced graphene oxide/Nafion nanohybrid film has been introduced in this work. The magnetic functionalized reduced graphene oxide was characterized by fourier transform infrared spectroscopy, atomic force microscope, X-ray diffraction, transmission electron microscopy and thermogravimetric analysis. The scanning electron microscopy characterized the morphology and microstructure of the prepared sensors, and the electrochemical effective surface areas of the prepared sensors were also calculated by chronocoulometry method. The electrochemical behavior of lobetyolin on the magnetic functionalized reduced graphene oxide/Nafion nanohybrid modified glassy carbon electrode was investigated by cyclic voltammetry and differential pulse voltammetry in a phosphate buffer solution of pH 6.0. The electron-transfer coefficient (α), electron transfer number (n), and electrode reaction rate constant (Κs) were calculated as 0.78, 0.73, and 4.63 s{sup −1}, respectively. Under the optimized conditions, the sensor based on magnetic functionalized reduced graphene oxide/Nafion showed a linear voltammetric response to the lobetyolin concentration at 1.0 × 10{sup −7} to 1.0 × 10{sup −4} mol/L with detection limit (S/N = 3)of 4.3 × 10{sup −8} mol/L. The proposed sensor also displayed acceptable reproducibility, long-term stability, and high selectivity, and performs well for analysis of lobetyolin in real samples. The voltammetric sensor was successfully applied to detect lobetyolin in Codonopsis pilosula with recovery values in the range of 96.12% –102.66%. - Graphical abstract: Schematic diagram of the synthesis of MrGO hybrid and the fabrication process of the MrGO/Nafion/GCE for determination of lobetyolin. Display Omitted - Highlights: • The MrGO/Nafion@GCE electrochemical sensor was successfully fabricated. • The prepared MrGO was characterized by AFM, XRD, FTIR, VSM, TEM and SEM. �

Electrochemical polymerization of pyrrole over AZ31 Mg alloy for biomedical applications

International Nuclear Information System (INIS)

Srinivasan, A.; Ranjani, P.; Rajendran, N.

2013-01-01

Highlights: ► Polymerization of pyrrole over AZ31 Mg was carried out using cyclic voltammetry. ► Pyrrole concentration was optimized to accomplish the adherent and uniform coating. ► Effect of monomer concentration on the surface morphology was discussed. ► Corrosion resistance of AZ31 Mg in SBF was studied as a function of Py concentration. ► PPy coated AZ31 Mg alloy exhibited enhanced corrosion resistance at 0.25 M of Py. -- Abstract: Electrochemical polymerization of pyrrole (Py) from aqueous salicylate solution over AZ31 Mg alloy was carried out using cyclic voltammetry (CV). The effect of monomer concentration on the surface and electrochemical corrosion in simulated body fluid (SBF) were analysed. Attenuated total reflection-infrared (ATR-IR) spectra showed the characteristic ring stretching peaks for polypyrrole (PPy). Scanning electron microscopy (SEM) and atomic force microscopy (AFM) studies exhibited typical cauliflower morphology with rough surface for PPy coated AZ31 Mg alloy. Open circuit potential measurement and potentiodynamic polarization studies revealed that the coating prepared using 0.25 M of Py had positive shift of about 120 mV in corrosion potential and lower corrosion current density (0.03 mA/cm 2 ) compared to other concentrations and uncoated AZ31 Mg alloy (0.25 mA/cm 2 ). Electrochemical impedance spectroscopic (EIS) studies of uncoated and PPy coated Mg alloy in SBF revealed three-time constants behaviour with about one order of increment in impedance value for 0.25 M of Py

One-pot synthesis and electrochemical reactivity of carbon coated LiFePO4 spindles

International Nuclear Information System (INIS)

Yu Juanjuan; Hu Juncheng; Li Jinlin

2012-01-01

Highlights: ► Carbon coated LiFePO 4 spindles have been successfully synthesized via a novel supercritical method. ► The concentrations of lithium have an effect on the morphology of carbon coated LiFePO 4 . ► Amorphous carbon layer formed on the surface of LiFePO 4 by adding glucose. ► The carbon coating is responsible for the enhanced electrochemical performance. - Abstract: Spindle-like carbon coated LiFePO 4 (LiFePO 4 /C) composites have been successfully synthesized via a novel one-pot supercritical methanol method. The products were characterized by X-ray power diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS) and thermogravimetric analysis (TGA). The particle size, morphology and electrochemical reactivity changed with the concentration of lithium and carbon source. A possible morphology evolution process was also proposed. The glucose not only facilitates the formation of single crystalline LiFePO 4 , but also gives an amorphous carbon layer on the surface LiFePO 4 spindles.

Modified glassy carbon electrodes based on carbon nanostructures for ultrasensitive electrochemical determination of furazolidone.

Science.gov (United States)

Shahrokhian, Saeed; Naderi, Leila; Ghalkhani, Masoumeh

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. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

Electrochemical determination of bisphenol A at ordered mesoporous carbon modified nano-carbon ionic liquid paste electrode.

Science.gov (United States)

Li, Yonghong; Zhai, Xiurong; Liu, Xinsheng; Wang, Ling; Liu, Herong; Wang, Haibo

2016-02-01

A simple bisphenol A (BPA) sensor was successfully fabricated based on ordered mesoporous carbon CMK-3 modified nano-carbon ionic liquid paste electrode (CMK-3/nano-CILPE). The nanostructure of CMK-3 and the surface morphologies of modified electrodes were characterized by transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Electrochemical properties of the fabricated electrodes were investigated by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The fabricated sensor displayed excellent electroactivity towards bisphenol A using linear sweep voltammetry (LSV). Experimental conditions influencing the analytical performance of the modified electrode were optimized. Under optimal conditions, the oxidation peak current was proportional to BPA concentration in the range from 0.2 μM to 150 μM with a detection limit of 0.05 μM (S/N=3). This method was successfully used for determination of BPA leached from drinking bottle and plastic bag with good recoveries. Copyright © 2015 Elsevier B.V. All rights reserved.

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

Electrochemical deposition of Prussian blue on hydrogen terminated silicon(111)

International Nuclear Information System (INIS)

Zhao Jianwei; Zhang Yan; Shi Chuanguo; Chen, Hongyuan; Tong Lianming; Zhu Tao; Liu Zhongfan

2006-01-01

Electrochemical deposition of Prussian blue (PB) was performed by cyclic voltammetry on hydrogen terminated n-type Si(111) surface. The characterization of the samples based on atomic force microscopy and X-ray diffraction spectroscopy showed a nanocrystal form of the PB films on the silicon surface. The thickness of PB films as a function of the potential cycling number was monitored simultaneously by Raman spectroscopy, proving that the growth of the films is in a good controllable manner

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.

Facile synthesis of reduced graphene oxide/CoWO4 nanocomposites with enhanced electrochemical performances for supercapacitors

International Nuclear Information System (INIS)

Xu, Xiaowei; Shen, Jianfeng; Li, Na; Ye, Mingxin

2014-01-01

Highlights: • RGO/CoWO 4 composites were successfully prepared through a facile hydrothermal method. • RGO/CoWO 4 composites show much higher specific capacitances than pure CoWO 4 . • Enhanced electrical conductivity leads to superior electrochemical performance. - Abstract: A facile one-pot hydrothermal method was provided for synthesis of the reduced graphene oxide-cobalt tungstate (RGO/CoWO 4 ) nanocomposites with the enhanced electrochemical performances for supercapacitors for the first time. The resulting nanocomposites are comprised of CoWO 4 nanospheres that are well-anchored on graphene sheets by in situ reducing. The prepared RGO/CoWO 4 nanocomposites have been thoroughly characterized by Fourier–transform infrared spectroscopy, X-ray diffraction, Raman spectroscopy, Thermogravimetric analysis, Scanning electron microscopy, Transmission electron microscopy, X-ray photoelectron spectroscopy, and N 2 adsorption–desorption. Importantly, the prepared nanocomposites exhibit superior electrochemical performance to CoWO 4 as electrodes for supercapacitors. As a result, RGO/CoWO 4 nanocomposites with 91.6 wt% CoWO 4 content achieved a specific capacitance about 159.9 F g −1 calculated from the CV curves at 5 mV s −1 , which was higher than that of CoWO 4 (60.6 F g −1 ). The good electrochemical performance can be attributed to the increased electrical conductivity and the creation of new active sites due to the synergetic effect of RGO and CoWO 4 nanospheres. The cyclic stability tests demonstrated capacitance retention of about 94.7% after 1000 cycles, suggesting the potential application of RGO/CoWO 4 nanocomposites in energy-storage devices

Graphene prepared by one-pot solvent exfoliation as a highly sensitive platform for electrochemical sensing

Energy Technology Data Exchange (ETDEWEB)

Wu, Can; Cheng, Qin [Key Laboratory for Large-Format Battery Materials and System, Ministry of Education, School of Chemistry and Chemical Engineering, Huazhong University of Science and Technology, Wuhan 430074 (China); Wu, Kangbing, E-mail: kbwu@hust.edu.cn [Key Laboratory for Large-Format Battery Materials and System, Ministry of Education, School of Chemistry and Chemical Engineering, Huazhong University of Science and Technology, Wuhan 430074 (China); Wu, Gang [Materials Physics and Applications Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Li, Qing, E-mail: qing_li_2@brown.edu [Materials Physics and Applications Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)

2014-05-01

Highlights: • Graphene was prepared by one-step solvent exfoliation as superior electrode material. • Compared with RGO, prepared graphene exhibited stronger signal enhancement. • A widespread and highly-sensitive electrochemical sensing platform was constructed. - Abstract: Graphene was easily obtained via one-step ultrasonic exfoliation of graphite powder in N-methyl-2-pyrrolidone. Scanning electron microscopy, transmission electron microscopy, Raman and particle size measurements indicated that the exfoliation efficiency and the amount of produced graphene increased with ultrasonic time. The electrochemical properties and analytical applications of the resulting graphene were systematically studied. Compared with the predominantly-used reduced graphene oxides, the obtained graphene by one-step solvent exfoliation greatly enhanced the oxidation signals of various analytes, such as ascorbic acid (AA), dopamine (DA), uric acid (UA), xanthine (XA), hypoxanthine (HXA), bisphenol A (BPA), ponceau 4R, and sunset yellow. The detection limits of AA, DA, UA, XA, HXA, BPA, ponceau 4R, and sunset yellow were evaluated to be 0.8 μM, 7.5 nM, 2.5 nM, 4 nM, 10 nM, 20 nM, 2 nM, and 1 nM, which are much lower than the reported values. Thus, the prepared graphene via solvent exfoliation strategy displays strong signal amplification ability and holds great promise in constructing a universal and sensitive electrochemical sensing platform.

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.

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 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.

Molybdenum disulfide nanoflower-chitosan-Au nanoparticles composites based electrochemical sensing platform for bisphenol A determination

International Nuclear Information System (INIS)

Huang, Ke-Jing; Liu, Yu-Jie; Liu, Yan-Ming; Wang, Ling-Ling

2014-01-01

Highlights: • This work constructs a novel electrochemical biosensor for bisphenol A detection. • Flower-like MoS 2 are prepared by a simple hydrothermal procedure. • AuNPs are assembled on MoS 2 nanoflowers modified electrode for signal amplification. • The developed sensor exhibits low detection limit and wide linear range. - Abstract: Two-dimensional transition metal dichalcogenide are attracting increasing attention in electrochemical sensing due to their unique electronic properties. In this work, flower-like molybdenum disulfide (MoS 2 ) was prepared by a simple hydrothermal method. The scanning electron microscopy and transmission electron microscopy images showed the MoS 2 nanoflower had sizes with diameter of about 200 nm and was constructed with many irregular sheets as a petal-like structure with thickness of several nanometers. A novel electrochemical sensor was constructed for the determination of bisphenol A (BPA) based on MoS 2 and chitosan-gold nanoparticles composites modified electrode. The sensor showed an efficient electrocatalytic role for the oxidation of BPA, and the oxidation overpotentials of BPA decreased significantly and the peak current increased greatly compared with bare GCE and other modified electrode. A good linear relationship between the oxidation peak current and BPA concentration was obtained in the range from 0.05 to 100 μM with a detection limit of 5.0 × 10 −9 M (S/N = 3). The developed sensor exhibited high sensitivity and long-term stability, and it was successfully applied for the determination of BPA in different samples. This work indicated MoS 2 nanoflowers were promising in electrochemical sensing and catalytic applications

Facile synthesis of core–shell structured PANI-Co_3O_4 nanocomposites with superior electrochemical performance in supercapacitors

International Nuclear Information System (INIS)

Hai, Zhenyin; Gao, Libo; Zhang, Qiang; Xu, Hongyan; Cui, Danfeng; Zhang, Zengxing; Tsoukalas, Dimitris; Tang, Jun; Yan, Shubin; Xue, Chenyang

2016-01-01

Graphical abstract: - Highlights: • PANI-Co_3O_4 is synthesized by carbon-assisted and in situ polymerization methods. • PANI coating improves the properties of Co_3O_4 affecting electrochemical performance. • The nanocomposites exhibit a high specific capacitance of 1184 F g"−"1 at 1.25 A g"−"1. - Abstract: Core–shell structured PANI-Co_3O_4 nanocomposites for supercapacitor applications were synthesized by combination of carbon-assisted method and in situ polymerization method. The crystalline structure, optical band gap, morphology, and hydrophilic property, as the major factors affecting the performances of supercapacitors, were investigated by X-ray diffraction (XRD), UV–vis spectrophotometry (UV–vis), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and water contact angle (WCA). The core–shell structured PANI-Co_3O_4 nanocomposites are characterized by amorphous PANI, small bandgaps, large surface area and favorable hydrophilicity, which indicates the superior electrochemical performances of the nanocomposites as electrode material for supercapacitors. Cyclic voltammetry (CV), galvanostatic charge/discharge and electrochemical impedance spectroscopy (EIS) measurements were conducted in 6 M KOH aqueous solution to evaluate the electrochemical performances. The results shows that core–shell structured PANI-Co_3O_4 nanocomposites exhibit a high specific capacitance of 1184 F g"−"1 at 1.25 A g"−"1, excellent cycling stability of a capacitance retention of 84.9% after 1000 galvanostatic charge/discharge cycles, good electrical conductivity and ion diffusion behavior.

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.

Effects of microplasma arc AISI 316L welds on the corrosion behaviour of pipelines in LiBr cooling systems

International Nuclear Information System (INIS)

Sánchez-Tovar, R.; Montañés, M.T.; García-Antón, J.

2013-01-01

Highlights: •SECM tests reveal differences in electrochemical activity of base and welded alloys. •The highest electrochemical activity is obtained for the welded alloy. •Microplasma arc welding process hinders passivation in lithium bromide. •Microplasma arc welding increases corrosion rate and susceptibility to pitting. •The galvanic pair between base and welded alloys in LiBr is weak. -- Abstract: The effect of microplasma arc welding (MPAW) on the electrochemical and corrosion behaviour of AISI 316L stainless steel tubes has been studied. Scanning electrochemical measurements were performed in sodium chloride to evaluate the difference in the electrochemical activity of base (non-welded) and welded samples. Oxygen reduction rates increase in AISI 316L due to the heat treatment effect induced by welding, indicating a higher electrochemical activity in the welded samples. Additionally, the use of MPA weldments in lithium bromide (LiBr) absorption machines was also analysed at typical operating temperatures and Reynolds numbers. The welding process increases corrosion rates, hinders passivation and increases the susceptibility to pitting attack in LiBr. However, zero-resistance ammeter and localization index measurements show that the galvanic pair generated between the base and welded alloys is weak, both electrodes being in their passive state. Temperature greatly affects the corrosion process

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.

Facile route to covalently-jointed graphene/polyaniline composite and it’s enhanced electrochemical performances for supercapacitors

Energy Technology Data Exchange (ETDEWEB)

Qiu, Hanxun [School of Materials Science and Engineering, University of Shanghai for Science and Technology, Shanghai 200093 (China); Han, Xuebin; Qiu, Feilong [School of Materials Science and Engineering, University of Shanghai for Science and Technology, Shanghai 200093 (China); School of Environment and Architecture, University of Shanghai for Science and Technology, Shanghai 200093 (China); Yang, Junhe, E-mail: hxqiu@usst.edu.cn [School of Materials Science and Engineering, University of Shanghai for Science and Technology, Shanghai 200093 (China)

2016-07-15

Highlights: • A novel synthetic approach to graphene/polyaniline composite is developed. • Covalently bonds are introduced between graphene and polyaniline. • The composite exhibits great electrochemical property with capacitance of 489 F g{sup −1}. - Abstract: A polyaniline/graphene composite with covalently-bond is synthesized by a novel approach. In this way, graphene oxide is functionalized firstly by introducing amine groups onto the surface with the reduction of graphene oxide in the process and then served as the anchor sites for the growth of polyaniline (PANI) via in-situ polymerization. The composite material is characterized by electron microscopy, the resonant Raman spectra, X-ray diffraction, transform infrared spectroscopy and X-ray photoelectron spectroscopy. The electrochemical properties of the composite are measured by cyclic voltammetry, electrochemical impedance spectroscopy and galvanostatic charging/discharging. With the functionalization process, the graphene/polyaniline composite electrode exhibits remarkably enhanced electrochemical performance with specific capacitance of 489 F g{sup −1} at 0.5 A g{sup −1}, which is superior to those of its individual components. The outstanding electrochemical performance of the hybrid can be attributed to its covalently synergistic effect between graphene and polyaniline, suggesting promising potentials for supercapacitors.

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...

Ultraporous poly(3,4-ethylenedioxythiophene) for nanometric electrochemical supercapacitor

Energy Technology Data Exchange (ETDEWEB)

Aradilla, David [Departament d' Enginyeria Quimica, ETSEIB, Universitat Politecnica de Catalunya, Avda. Diagonal 647, Barcelona E-08028 (Spain); Center for Research in Nano-Engineering, Universitat Politecnica de Catalunya, Campus Sud, Edifici C' , C/Pasqual i Vila s/n, Barcelona E-08028 (Spain); Estrany, Francesc [Center for Research in Nano-Engineering, Universitat Politecnica de Catalunya, Campus Sud, Edifici C' , C/Pasqual i Vila s/n, Barcelona E-08028 (Spain); Departament d' Enginyeria Quimica, EUETIB, Universitat Politecnica de Catalunya, Comte d' Urgell 187, Barcelona E-08036 (Spain); Armelin, Elaine [Departament d' Enginyeria Quimica, ETSEIB, Universitat Politecnica de Catalunya, Avda. Diagonal 647, Barcelona E-08028 (Spain); Center for Research in Nano-Engineering, Universitat Politecnica de Catalunya, Campus Sud, Edifici C' , C/Pasqual i Vila s/n, Barcelona E-08028 (Spain); Aleman, Carlos, E-mail: carlos.aleman@upc.edu [Departament d' Enginyeria Quimica, ETSEIB, Universitat Politecnica de Catalunya, Avda. Diagonal 647, Barcelona E-08028 (Spain); Center for Research in Nano-Engineering, Universitat Politecnica de Catalunya, Campus Sud, Edifici C' , C/Pasqual i Vila s/n, Barcelona E-08028 (Spain)

2012-04-30

Ultrathin films of poly(3,4-ethylenedioxythiophene) (PEDOT) have been prepared by electropolymerization on steel and indium-tin oxide (ITO) substrates under identical experimental conditions. Scanning electron microscopy and atomic force microscopy indicate that the substrate affects dramatically both the morphology and topography of films when the polymerization times are very short. An ultraporous three-dimensional network involving ultrathin sticks with a fiber-like morphology was formed on ITO. Asymmetric and symmetric supercapacitors have been fabricated by assembling electrodes of PEDOT deposited on ITO and steel. The specific capacitance, electrochemical stability, supercapacitor behavior and Coulombic efficiency measured for devices with an ITO/steel configuration were similar to those reported for advanced PEDOT-inorganic hybrid composites. Furthermore, the performance of the ITO/steel assembly is higher than those determined for symmetric supercapacitors derived from two identical electrodes of PEDOT deposited on steel or on ITO. The unique properties of the asymmetric supercapacitors have been attributed to the ultraporous structure of the ultrathin films deposited on ITO, which is not significantly perturbed when the device is submitted to a very high number of consecutive oxidation-reduction processes, and the different electroactivities of the two electrodes. - Highlights: Black-Right-Pointing-Pointer Ultrathin poly(3,4-ethylenedioxythiophene) (PEDOT) films show fiber-like morphology. Black-Right-Pointing-Pointer The porosity of ultrathin PEDOT films induces a very high electrochemical stability. Black-Right-Pointing-Pointer Asymmetric supercapacitors made of ultrathin PEDOT behave like hybrid nanocomposites.

Ultraporous poly(3,4-ethylenedioxythiophene) for nanometric electrochemical supercapacitor

International Nuclear Information System (INIS)

Aradilla, David; Estrany, Francesc; Armelin, Elaine; Alemán, Carlos

2012-01-01

Ultrathin films of poly(3,4-ethylenedioxythiophene) (PEDOT) have been prepared by electropolymerization on steel and indium-tin oxide (ITO) substrates under identical experimental conditions. Scanning electron microscopy and atomic force microscopy indicate that the substrate affects dramatically both the morphology and topography of films when the polymerization times are very short. An ultraporous three-dimensional network involving ultrathin sticks with a fiber-like morphology was formed on ITO. Asymmetric and symmetric supercapacitors have been fabricated by assembling electrodes of PEDOT deposited on ITO and steel. The specific capacitance, electrochemical stability, supercapacitor behavior and Coulombic efficiency measured for devices with an ITO/steel configuration were similar to those reported for advanced PEDOT-inorganic hybrid composites. Furthermore, the performance of the ITO/steel assembly is higher than those determined for symmetric supercapacitors derived from two identical electrodes of PEDOT deposited on steel or on ITO. The unique properties of the asymmetric supercapacitors have been attributed to the ultraporous structure of the ultrathin films deposited on ITO, which is not significantly perturbed when the device is submitted to a very high number of consecutive oxidation–reduction processes, and the different electroactivities of the two electrodes. - Highlights: ► Ultrathin poly(3,4-ethylenedioxythiophene) (PEDOT) films show fiber-like morphology. ► The porosity of ultrathin PEDOT films induces a very high electrochemical stability. ► Asymmetric supercapacitors made of ultrathin PEDOT behave like hybrid nanocomposites.

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.

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.

Electrochemical behavior of monolayer and bilayer graphene.

Science.gov (United States)

Valota, Anna T; Kinloch, Ian A; Novoselov, Kostya S; Casiraghi, Cinzia; Eckmann, Axel; Hill, Ernie W; Dryfe, Robert A W

2011-11-22

Results of a study on the electrochemical properties of exfoliated single and multilayer graphene flakes are presented. Graphene flakes were deposited on silicon/silicon oxide wafers to enable fast and accurate characterization by optical microscopy and Raman spectroscopy. Conductive silver paint and silver wires were used to fabricate contacts; epoxy resin was employed as a masking coating in order to expose a stable, well-defined area of graphene. Both multilayer and monolayer graphene microelectrodes showed quasi-reversible behavior during voltammetric measurements in potassium ferricyanide. However, the standard heterogeneous charge transfer rate constant, k°, was estimated to be higher for monolayer graphene flakes. © 2011 American Chemical Society

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.

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.

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...

Synthesis and electrochemical properties of {alpha}-MnO{sub 2} microspheres

Energy Technology Data Exchange (ETDEWEB)

Wang Hongen [College of Chemistry and Chemical Engineering, Central South University, Changsha 410083 (China); Zhengzhou Research Institute of CHALCO, Zhengzhou Research Institute of Light Metals, Zhengzhou 450041 (China); Qian Dong [College of Chemistry and Chemical Engineering, Central South University, Changsha 410083 (China)], E-mail: qiandong6@yahoo.com.cn

2008-06-15

We report the synthesis of {alpha}-MnO{sub 2} microspheres by a low-temperature hydrothermal method involving no templates or catalysts. The products were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), Energy-dispersive X-ray spectrum (EDX), transmission electron microscopy (TEM), Fourier transform infrared spectrum (FT-IR), and Brunauer-Emmett-Teller (BET). The results show that the as-synthesized products are mainly composed of large quantities of {alpha}-MnO{sub 2} microspheres having a sea-urchin shape and a few microspheres constructed of small nanorods. Electrochemical characterization indicates that the resulting {alpha}-MnO{sub 2} microspheres display promising discharge properties than the commercial electrolytic manganese dioxides (EMD) when used as cathodes in alkaline Zn-MnO{sub 2} batteries.

Combined spectroscopy and microscopy of supported MoS2 nanoparticles

DEFF Research Database (Denmark)

Nielsen, Jane Hvolbæk; Bech, Lone; Nielsen, Kenneth

2009-01-01

Supported molybdenum-sulfide nanoparticles are known catalysts for petroleum hydrodesulfurization as well as for electrochemical hydrogen evolution. In this study, we investigate molybdenum-sulfide nanoparticles supported on Au(111) using X-ray photoelectron spectroscopy (XPS) and scanning...... tunneling microscopy (STM), aiming to correlate spectroscopically determined chemical states with atomically resolved nanostructure. The results of this study allow us to conclude the following: (1) the XPS results from our model system are in good agreement with previously published results on supported Mo...

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

Kinetics of electrochemical boriding of low carbon steel

International Nuclear Information System (INIS)

Kartal, G.; Eryilmaz, O.L.; Krumdick, G.; Erdemir, A.; Timur, S.

2011-01-01

In this study, the growth kinetics of the boride layers forming on low carbon steel substrates was investigated during electrochemical boriding which was performed at a constant current density of 200 mA/cm 2 in a borax based electrolyte at temperatures ranging from 1123 K to 1273 K for periods of 5-120 min. After boriding, the presence of both FeB and Fe 2 B phases were confirmed by the X-ray diffraction method. Cross-sectional microscopy revealed a very dense and thick morphology for both boride phases. Micro hardness testing of the borided steel samples showed a significant increase in the hardness of the borided surfaces (i.e., up to (1700 ± 200) HV), while the hardness of un-borided steel samples was approximately (200 ± 20) HV. Systematic studies over a wide range of boriding time and temperature confirmed that the rate of the boride layer formation is strongly dependent on boriding duration and has a parabolic character. The activation energy of boride layer growth for electrochemical boriding was determined as (172.75 ± 8.6) kJ/mol.

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

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

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).

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)

Graphene-supported SnO2 nanoparticles prepared by a solvothermal approach for an enhanced electrochemical performance in lithium-ion batteries.

Science.gov (United States)

Wang, Bei; Su, Dawei; Park, Jinsoo; Ahn, Hyojun; Wang, Guoxiu

2012-04-13

SnO2 nanoparticles were dispersed on graphene nanosheets through a solvothermal approach using ethylene glycol as the solvent. The uniform distribution of SnO2 nanoparticles on graphene nanosheets has been confirmed by scanning electron microscopy and transmission electron microscopy. The particle size of SnO2 was determined to be around 5 nm. The as-synthesized SnO2/graphene nanocomposite exhibited an enhanced electrochemical performance in lithium-ion batteries, compared with bare graphene nanosheets and bare SnO2 nanoparticles. The SnO2/graphene nanocomposite electrode delivered a reversible lithium storage capacity of 830 mAh g-1 and a stable cyclability up to 100 cycles. The excellent electrochemical properties of this graphene-supported nanocomposite could be attributed to the insertion of nanoparticles between graphene nanolayers and the optimized nanoparticles distribution on graphene nanosheets.

The influence of current collector corrosion on the performance of electrochemical capacitors

Science.gov (United States)

Wojciechowski, Jarosław; Kolanowski, Łukasz; Bund, Andreas; Lota, Grzegorz

2017-11-01

This paper discusses the effect of current collector (stainless steel 316L) corrosion on the performance of electrochemical capacitors operated in aqueous electrolytes. This topic seems to be often neglected in scientific research. The studied electrolytes were 1 M H2SO4, 1 M KI, 1 M Na2SO4, 1 M KOH and 6 M KOH. The corrosion process was investigated by means of selected direct and alternating current techniques. The surface of the current collectors as well as the corrosion products were characterised using scanning electron microscopy, energy-dispersive X-ray spectroscopy, Raman spectroscopy and atomic force microscopy. Stainless steel 316L in alkaline solutions is characterised by the lowest values of corrosion potentials whereas the potentials in acidic media become the most noble. Our studies show that corrosion potentials increase with decreasing pH value. This phenomenon can be explained with the formation of passive oxide films on the stainless steel current collectors. The passive oxide films are usually thicker and more porous in alkaline solutions than that in the other electrolytes. The processes occurring at the electrode/electrolyte interfaces strongly influence the working parameters of electrochemical capacitors such as voltage, working potentials of single electrodes, self-discharge as well as the internal resistance and cycling stability.

Impact of incorporation of chromium on electrochemical properties of LiFePO4/C for Li-ion batteries

Directory of Open Access Journals (Sweden)

Naik Amol

2015-12-01

Full Text Available LiFe0.95Cr0.05PO4/C was successfully synthesized by one-step solid-state reaction using a single mode microwave reactor. The effect of incorporation of chromium on LiFePO4 lattice parameters was systematically investigated by X-ray diffraction. Surface analysis was done by scanning electron microscopy and transmission electron microscopy. The ratio of amorphous to graphitic carbon was determined from Raman spectroscopic data. The influence of chromium incorporation on electrochemical properties was studied by recording charge/discharge cycles combined with electrochemical impedance spectroscopy (EIS and cyclic voltammetry. It was found that Cr incorporation significantly enhanced the electrochemical performance of LiFePO4 at all current densities up to 10 C. LiFe0.95Cr0.05PO4/C prepared exhibited the best performance with an initial specific discharge capacity of 157.7, 144.8, 138.3, 131.0, 124.1 and 111.1 mAh·g−1 at 0.1 C, 0.5 C, 1.0 C, 2.0 C, 5 C and 10 C, respectively. The doped sample displayed excellent capacity retention, which was substantially superior than that of pristine LiFePO4/C at a higher current rate.

Novel Ag@TiO2 nanocomposite synthesized by electrochemically active biofilm for nonenzymatic hydrogen peroxide sensor.

Science.gov (United States)

Khan, Mohammad Mansoob; Ansari, Sajid Ali; Lee, Jintae; Cho, Moo Hwan

2013-12-01

A novel nonenzymatic sensor for H2O2 was developed based on an Ag@TiO2 nanocomposite synthesized using a simple and cost effective approach with an electrochemically active biofilm. The optical, structural, morphological and electrochemical properties of the as-prepared Ag@TiO2 nanocomposite were examined by UV-vis spectroscopy, X-ray diffraction, transmission electron microscopy and cyclic voltammetry (CV). The Ag@TiO2 nanocomposite was fabricated on a glassy carbon electrode (GCE) and their electrochemical performance was analyzed by CV, differential pulse voltammetry and electrochemical impedance spectroscopy. The Ag@TiO2 nanocomposite modified GCE (Ag@TiO2/GCE) displayed excellent performance towards H2O2 sensing at -0.73 V in the linear response range from 0.83 μM to 43.3 μM, within a detection limit and sensitivity of 0.83 μM and ~65.2328±0.01 μA μM(-1) cm(-2), respectively. In addition, Ag@TiO2/GCE exhibited good operational reproducibility and long term stability. © 2013.

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.

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.

Synthesis of palladium nanoparticle modified reduced graphene oxide and multi-walled carbon nanotube hybrid structures for electrochemical applications

Energy Technology Data Exchange (ETDEWEB)

Hu, Jie, E-mail: hujie@tyut.edu.cn [Micro and Nano System Research Center, Key Lab of Advanced Transducers and Intelligent Control System (Ministry of Education) & College of Information Engineering, Taiyuan University of Technology, Taiyuan, 030024, Shanxi (China); Zhao, Zhenting; Zhang, Jun; Li, Gang; Li, Pengwei; Zhang, Wendong [Micro and Nano System Research Center, Key Lab of Advanced Transducers and Intelligent Control System (Ministry of Education) & College of Information Engineering, Taiyuan University of Technology, Taiyuan, 030024, Shanxi (China); Lian, Kun, E-mail: liankun@tyut.edu.cn [Micro and Nano System Research Center, Key Lab of Advanced Transducers and Intelligent Control System (Ministry of Education) & College of Information Engineering, Taiyuan University of Technology, Taiyuan, 030024, Shanxi (China); School of Nano-Science and Nano-Engineering, Suzhou & Collaborative Innovation Center of Suzhou Nano Science and Technology, Xi' an Jiaotong University, Xi' an, 710049 (China); Center for Advanced Microstructures and Devices, Louisiana State University, LA, 70806 (United States)

2017-02-28

Graphical abstract: A sensitive hydrazine electrochemical sensor was fabricated by using palladium (Pd) nanoparticle functionalized reduced graphene oxide (rGO) and multi-walled carbon nanotube (MWCNTs) hybrid structures (Pd/rGO-MWCNTs). - Highlights: • rGO-MWCNTs hybrid structures and Pd nanoparticles are prepared using electrochemical methods. • rGO-MWCNTs hybrid films are used as supports and co-catalysts for Pd nanoparticles. • The Pd/rGO-MWCNTs hybrid structure based sensor shows an ultra-high sensitivity of 7.09 μA μM{sup −1} cm{sup −2} and a low detection limit of 0.15 μM. • The proposed electrochemical sensor exhibits excellent selectivity. - Abstract: In this work, palladium (Pd) nanoparticles functionalized reduced graphene oxide (rGO) and multi-walled carbon nanotubes (MWCNTs) hybrid structures (Pd/rGO-MWCNTs) were successfully prepared by a combination of electrochemical reduction with electrodeposition method. The morphology, structure, and composition of the Pd/rGO-MWCNTs hybrid were characterized by scanning electron microscopy, transmission electron microscopy and energy dispersive spectroscopy. The as-synthesized hybrid structures were modified on the glassy carbon electrode (GCE) and further utilized for hydrazine sensing. Electrochemical impedance spectroscopic, cyclic voltammetry and single-potential amperometry experiments were carried out on Pd/rGO-MWCNTs hybrid structures to investigate the interface properties and sensing performance. The measured results demonstrate that the fabricated Pd/rGO-MWCNTs/GCE sensor show a high sensitivity of 7.09 μA μM{sup −1} cm{sup −2} in a large concentration range of 1.0 to 1100 μM and a low detection limit of 0.15 μM. Moreover, the as-prepared sensor exhibits good selectivity and stability for the determination of hydrazine under interference conditions.

Synthesis of palladium nanoparticle modified reduced graphene oxide and multi-walled carbon nanotube hybrid structures for electrochemical applications

International Nuclear Information System (INIS)

Hu, Jie; Zhao, Zhenting; Zhang, Jun; Li, Gang; Li, Pengwei; Zhang, Wendong; Lian, Kun

2017-01-01

Graphical abstract: A sensitive hydrazine electrochemical sensor was fabricated by using palladium (Pd) nanoparticle functionalized reduced graphene oxide (rGO) and multi-walled carbon nanotube (MWCNTs) hybrid structures (Pd/rGO-MWCNTs). - Highlights: • rGO-MWCNTs hybrid structures and Pd nanoparticles are prepared using electrochemical methods. • rGO-MWCNTs hybrid films are used as supports and co-catalysts for Pd nanoparticles. • The Pd/rGO-MWCNTs hybrid structure based sensor shows an ultra-high sensitivity of 7.09 μA μM"−"1 cm"−"2 and a low detection limit of 0.15 μM. • The proposed electrochemical sensor exhibits excellent selectivity. - Abstract: In this work, palladium (Pd) nanoparticles functionalized reduced graphene oxide (rGO) and multi-walled carbon nanotubes (MWCNTs) hybrid structures (Pd/rGO-MWCNTs) were successfully prepared by a combination of electrochemical reduction with electrodeposition method. The morphology, structure, and composition of the Pd/rGO-MWCNTs hybrid were characterized by scanning electron microscopy, transmission electron microscopy and energy dispersive spectroscopy. The as-synthesized hybrid structures were modified on the glassy carbon electrode (GCE) and further utilized for hydrazine sensing. Electrochemical impedance spectroscopic, cyclic voltammetry and single-potential amperometry experiments were carried out on Pd/rGO-MWCNTs hybrid structures to investigate the interface properties and sensing performance. The measured results demonstrate that the fabricated Pd/rGO-MWCNTs/GCE sensor show a high sensitivity of 7.09 μA μM"−"1 cm"−"2 in a large concentration range of 1.0 to 1100 μM and a low detection limit of 0.15 μM. Moreover, the as-prepared sensor exhibits good selectivity and stability for the determination of hydrazine under interference conditions.

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

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 catalytic activities of nanoporous palladium rods for methanol electro-oxidation

Energy Technology Data Exchange (ETDEWEB)

Wang, Xiaoguang; Wang, Weimin; Qi, Zhen; Zhao, Changchun; Ji, Hong; Zhang, Zhonghua [Key Laboratory for Liquid-Solid Structural Evolution and Processing of Materials (MOE), School of Materials Science and Engineering, Shandong University, Jingshi Road 73, Jinan 250061 (China)

2010-10-01

A novel electrocatalyst, nanoporous palladium (npPd) rods can be facilely fabricated by dealloying a binary Al{sub 80}Pd{sub 20} alloy in a 5 wt.% HCl aqueous solution under free corrosion conditions. The microstructure of these nanoporous palladium rods has been characterized using scanning electron microscopy and transmission electron microscopy. The results show that each Pd rod is several microns in length and several hundred nanometers in diameter. Moreover, all the rods exhibit a typical three-dimensional bicontinuous interpenetrating ligament-channel structure with length scale of 15-20 nm. The electrochemical experiments demonstrate that these peculiar nanoporous palladium rods (mixed with Vulcan XC-72 carbon powders to form a npPd/C catalyst) reveal a superior electrocatalytic performance toward methanol oxidation in the alkaline media. In addition, the electrocatalytic activity obviously depends on the metal loading on the electrode and will reach to the highest level (223.52 mA mg{sup -1}) when applying 0.4 mg cm{sup -2} metal loading on the electrode. Moreover, a competing adsorption mechanism should exist when performing methanol oxidation on the surface of npPd rods, and the electro-oxidation reaction is a diffusion-controlled electrochemical process. Due to the advantages of simplicity and high efficiency in the mass production, the npPd rods can act as a promising candidate for the anode catalyst for direct methanol fuel cells (DMFCs). (author)

Low hydrogen containing amorphous carbon films - Growth and electrochemical properties as lithium battery anodes

Energy Technology Data Exchange (ETDEWEB)

Subramanian, V.; Masarapu, Charan; Wei, Bingqing [Department of Mechanical Engineering, University of Delaware, 130 Academy Street, Newark, DE 19716 (United States); Karabacak, Tansel [Department of Applied Science, University of Arkansas at Little Rock, 2801 South University Avenue, Little Rock, AR 72204 (United States); Teki, Ranganath [Department of Chemical and Biological Engineering, Rensselaer Polytechnic Institute, Troy, NY 12180 (United States); Lu, Toh-Ming [Department of Physics, Applied Physics, and Astronomy, Rensselaer Polytechnic Institute, Troy, NY 12180 (United States)

2010-04-02

Amorphous carbon films were deposited successfully on Cu foils by DC magnetron sputtering technique. Electrochemical performance of the film as lithium battery anode was evaluated across Li metal at 0.2 C rate in a non-aqueous electrolyte. The discharge curves showed unusually low irreversible capacity in the first cycle with a reversible capacity of {proportional_to}810 mAh g{sup -1}, which is at least 2 times higher than that of graphitic carbon. For the first time we report here an amorphous carbon showing such a high reversibility in the first cycle, which is very much limited to the graphitic carbon. The deposited films were extensively characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and step profilometer for the structural and surface properties. The hydrogen content of the synthesized films was studied using residual gas analysis (RGA). The low hydrogen content and the low specific surface area of the synthesized amorphous carbon film are considered responsible for such a high first cycle columbic efficiency. The growth mechanism and the reasons for enhanced electrochemical performance of the carbon films are discussed. (author)

Low hydrogen containing amorphous carbon films-Growth and electrochemical properties as lithium battery anodes

Science.gov (United States)

Subramanian, V.; Karabacak, Tansel; Masarapu, Charan; Teki, Ranganath; Lu, Toh-Ming; Wei, Bingqing

Amorphous carbon films were deposited successfully on Cu foils by DC magnetron sputtering technique. Electrochemical performance of the film as lithium battery anode was evaluated across Li metal at 0.2 C rate in a non-aqueous electrolyte. The discharge curves showed unusually low irreversible capacity in the first cycle with a reversible capacity of ∼810 mAh g -1, which is at least 2 times higher than that of graphitic carbon. For the first time we report here an amorphous carbon showing such a high reversibility in the first cycle, which is very much limited to the graphitic carbon. The deposited films were extensively characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and step profilometer for the structural and surface properties. The hydrogen content of the synthesized films was studied using residual gas analysis (RGA). The low hydrogen content and the low specific surface area of the synthesized amorphous carbon film are considered responsible for such a high first cycle columbic efficiency. The growth mechanism and the reasons for enhanced electrochemical performance of the carbon films are discussed.

Electrochemical stability and postmortem studies of Pt/SiC catalysts for polymer electrolyte membrane fuel cells

DEFF Research Database (Denmark)

Stamatin, Serban Nicolae; Spéder, József; Dhiman, Rajnish

2015-01-01

In the presented work, the electrochemical stability of platinized silicon carbide is studied. Postmortem transmission electron microscopy and X-ray photoelectron spectroscopy were used to document the change in the morphology and structure upon potential cycling of Pt/SiC catalysts. Two differen......, silicon carbide undergoes at least mild oxidation if not even silicon leaching....

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)

Amplified electrochemical determination of maltol in food based on graphene oxide-wrapped tin oxide@carbon nanospheres.

Science.gov (United States)

Gan, Tian; Sun, Junyong; Yu, Miaomiao; Wang, Kaili; Lv, Zhen; Liu, Yanming

2017-01-01

The study presents a new approach for rapid and ultrasensitive detection of maltol using a glassy carbon electrode (GCE) modified with graphene oxide-wrapped tin oxide@carbon nanospheres (SnO2@C@GO). The morphological and components properties of SnO2@C@GO nanocomposites were investigated by means of X-ray diffraction spectroscopy, Raman spectroscopy, field emission scanning electron microscopy, high resolution transmission electron microscopy, and electrochemical impedance spectroscopy. SnO2@C@GO nanocomposite on a GCE had a synergetic effect on the electrochemical oxidation of maltol by means of square wave voltammetry. Under the optimum conditions, anodic peak current response of maltol was linear with its concentration in the range of 80nM-10μM, and a detection limit of 12nM was achieved for maltol. The experiment results presented that the method showed good selectivity, sensitivity, reproducibility, and long-term stability, as well as excellent potential for use as an ideal inexpensive voltammetric method applicable for complex food matrices. Copyright © 2016 Elsevier Ltd. All rights reserved.

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.

Electrochemical detection of ultratrace nitroaromatic explosives using ordered mesoporous carbon

Energy Technology Data Exchange (ETDEWEB)

Zang Jianfeng; Guo Chunxian; Hu Fengping [School of Chemical and Biomedical Engineering and Center for Advanced Bionanosystems, Nanyang Technological University, 70 Nanyang Drive, Singapore 637457 (Singapore); Yu Lei [Department of Chemical, Materials and Biomolecular Engineering, University of Connecticut, Storrs, CT 06269 (United States); Li Changming, E-mail: ecmli@ntu.edu.sg [School of Chemical and Biomedical Engineering and Center for Advanced Bionanosystems, Nanyang Technological University, 70 Nanyang Drive, Singapore 637457 (Singapore)

2011-01-10

A sensitive electrochemical sensor has been fabricated to detect ultratrace nitroaromatic explosives using ordered mesoporus carbon (OMC). OMC was synthesized and characterized by scanning electron microscopy, transmission electron microscopy and nitrogen adsorption/desorption measurements. Glassy carbon electrodes functionalized with OMC show high sensitivity of 62.7 {mu}A cm{sup -2} per ppb towards 2,4,6-trinitrotoluene (TNT). By comparison with other materials such as carbon nanotubes and ordered mesoporous silica, it is found that the high performance of OMC toward sensing TNT is attributed to its large specific surface area and fast electron transfer capability. As low as 0.2 ppb TNT, 1 ppb 2,4-dinitrotoluene and 1 ppb 1,3-dinitrobenzene can be detected on OMC based electrodes. This work renders new opportunities to detect ultratrace explosives for applications of environment protections and home securities against chemical warfare agents.

An ultrasensitive electrochemical DNA biosensor based on a copper oxide nanowires/single-walled carbon nanotubes nanocomposite

International Nuclear Information System (INIS)

Chen, Mei; Hou, Changjun; Huo, Danqun; Yang, Mei; Fa, Huanbao

2016-01-01

Graphical abstract: A novel and sensitive electrochemical biosensor based on hybrid nanocomposite consisting of copper oxide nanowires (CuO NWs) and carboxyl-functionalized single-walled carbon nanotubes (SWCNTs-COOH) was first developed for the detection of the specific-sequence target DNA. This schematic represents the fabrication procedure of our DNA biosensor. - Highlights: • An ultrasensitive DNA electrochemical biosensor was developed. • CuO NWs entangled with the SWCNTs formed a mesh structure with good conductivity. • It is the first time use of CuONWs-SWCNTs hybrid nanocomposite for DNA detection. • The biosensor is simple, selective, stable, and sensitive. • The biosensor has great potential for use in analysis of real samples. - Abstract: Here, we developed a novel and sensitive electrochemical biosensor to detect specific-sequence target DNA. The biosensor was based on a hybrid nanocomposite consisting of copper oxide nanowires (CuO NWs) and carboxyl-functionalized single-walled carbon nanotubes (SWCNTs-COOH). The resulting CuO NWs/SWCNTs layers exhibited a good differential pulse voltammetry (DPV) current response for the target DNA sequences, which we attributed to the properties of CuO NWs and SWCNTs. CuO NWs and SWCNTs hybrid composites with highly conductive and biocompatible nanostructure were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), and cyclic voltammetry (CV). Immobilization of the probe DNA on the electrode surface was largely improved due to the unique synergetic effect of CuO NWs and SWCNTs. DPV was applied to monitor the DNA hybridization event, using adriamycin as an electrochemical indicator. Under optimal conditions, the peak currents of adriamycin were linear with the logarithm of target DNA concentrations (ranging from 1.0 × 10"−"1"4 to 1.0 × 10"−"8 M), with a detection limit of 3.5 × 10"−"1"5 M (signal/noise ratio of 3). The biosensor also showed high selectivity to

An ultrasensitive electrochemical DNA biosensor based on a copper oxide nanowires/single-walled carbon nanotubes nanocomposite

Energy Technology Data Exchange (ETDEWEB)

Chen, Mei [Key Laboratory of Biorheology Science and Technology, Ministry of Education, College of Bioengineering, Chongqing University, Chongqing 400044 (China); Hou, Changjun, E-mail: houcj@cqu.edu.cn [Key Laboratory of Biorheology Science and Technology, Ministry of Education, College of Bioengineering, Chongqing University, Chongqing 400044 (China); National Key Laboratory of Fundamental Science of Micro/Nano-Device and System Technology, Chongqing University, Chongqing 400044 (China); Huo, Danqun [Key Laboratory of Biorheology Science and Technology, Ministry of Education, College of Bioengineering, Chongqing University, Chongqing 400044 (China); National Key Laboratory of Fundamental Science of Micro/Nano-Device and System Technology, Chongqing University, Chongqing 400044 (China); Yang, Mei [Key Laboratory of Biorheology Science and Technology, Ministry of Education, College of Bioengineering, Chongqing University, Chongqing 400044 (China); Fa, Huanbao [College of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400044 (China)

2016-02-28

Graphical abstract: A novel and sensitive electrochemical biosensor based on hybrid nanocomposite consisting of copper oxide nanowires (CuO NWs) and carboxyl-functionalized single-walled carbon nanotubes (SWCNTs-COOH) was first developed for the detection of the specific-sequence target DNA. This schematic represents the fabrication procedure of our DNA biosensor. - Highlights: • An ultrasensitive DNA electrochemical biosensor was developed. • CuO NWs entangled with the SWCNTs formed a mesh structure with good conductivity. • It is the first time use of CuONWs-SWCNTs hybrid nanocomposite for DNA detection. • The biosensor is simple, selective, stable, and sensitive. • The biosensor has great potential for use in analysis of real samples. - Abstract: Here, we developed a novel and sensitive electrochemical biosensor to detect specific-sequence target DNA. The biosensor was based on a hybrid nanocomposite consisting of copper oxide nanowires (CuO NWs) and carboxyl-functionalized single-walled carbon nanotubes (SWCNTs-COOH). The resulting CuO NWs/SWCNTs layers exhibited a good differential pulse voltammetry (DPV) current response for the target DNA sequences, which we attributed to the properties of CuO NWs and SWCNTs. CuO NWs and SWCNTs hybrid composites with highly conductive and biocompatible nanostructure were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), and cyclic voltammetry (CV). Immobilization of the probe DNA on the electrode surface was largely improved due to the unique synergetic effect of CuO NWs and SWCNTs. DPV was applied to monitor the DNA hybridization event, using adriamycin as an electrochemical indicator. Under optimal conditions, the peak currents of adriamycin were linear with the logarithm of target DNA concentrations (ranging from 1.0 × 10{sup −14} to 1.0 × 10{sup −8} M), with a detection limit of 3.5 × 10{sup −15} M (signal/noise ratio of 3). The biosensor also showed high

Highly-sensitive electrochemical sensing platforms for food colourants based on the property-tuning of porous carbon

Energy Technology Data Exchange (ETDEWEB)

Cheng, Qin [Key Laboratory for Large-Format Battery Materials and System, Ministry of Education, School of Chemistry and Chemical Engineering, Huazhong University of Science and Technology, Wuhan, 430074 (China); Xia, Shanhong; Tong, Jianhua [State Key Laboratory of Transducer Technology, Institute of Electronics, Chinese Academy of Science, Beijing, 100190 (China); Wu, Kangbing, E-mail: kbwu@hust.edu.cn [Key Laboratory for Large-Format Battery Materials and System, Ministry of Education, School of Chemistry and Chemical Engineering, Huazhong University of Science and Technology, Wuhan, 430074 (China)

2015-08-05

It is very challenging to develop highly-sensitive analytical platforms for toxic synthetic colourants that widely added in food samples. Herein, a series of porous carbon (PC) was prepared using CaCO{sub 3} nanoparticles (nano-CaCO{sub 3}) as the hard template and starch as the carbon precursor. Characterizations of scanning electron microscopy and transmission electron microscopy indicated that the morphology and porous structure were controlled by the weight ratio of starch and nano-CaCO{sub 3}. The electrochemical behaviours of four kinds of widely-used food colourants, Sunset yellow, Tartrazine, Ponceau 4R and Allura red, were studied. On the surface of PC samples, the oxidation signals of colourants enhanced obviously, and more importantly, the signal enhancement abilities of PC were also dependent on the starch/nano-CaCO{sub 3} weight ratio. The greatly-increased electron transfer ability and accumulation efficiency were the main reason for the enhanced signals of colourants, as confirmed by electrochemical impedance spectroscopy and chronocoulometry. The prepared PC-2 sample by 1:1 starch/nano-CaCO{sub 3} weight ratio was more active for the oxidation of food colourtants, and increased the signals by 89.4-fold, 79.3-fold, 47.3-fold and 50.7-fold for Sunset yellow, Tartrazine, Ponceau 4R and Allura red. As a result, a highly-sensitive electrochemical sensing platform was developed, and the detection limits were 1.4, 3.5, 2.1 and 1.7 μg L{sup −1} for Sunset yellow, Tartrazine, Ponceau 4R and Allura red. The practical application of this new sensing platform was demonstrated using drink samples, and the detected results consisted with the values that obtained by high-performance liquid chromatography. - Highlights: • PC samples with different morphology and electrochemical activities were prepared. • Highly sensitive electrochemical sensing platform was developed for food colourants. • The accuracy and practicability was testified to be good by HPLC.

Highly-sensitive electrochemical sensing platforms for food colourants based on the property-tuning of porous carbon

International Nuclear Information System (INIS)

Cheng, Qin; Xia, Shanhong; Tong, Jianhua; Wu, Kangbing

2015-01-01

It is very challenging to develop highly-sensitive analytical platforms for toxic synthetic colourants that widely added in food samples. Herein, a series of porous carbon (PC) was prepared using CaCO 3 nanoparticles (nano-CaCO 3 ) as the hard template and starch as the carbon precursor. Characterizations of scanning electron microscopy and transmission electron microscopy indicated that the morphology and porous structure were controlled by the weight ratio of starch and nano-CaCO 3 . The electrochemical behaviours of four kinds of widely-used food colourants, Sunset yellow, Tartrazine, Ponceau 4R and Allura red, were studied. On the surface of PC samples, the oxidation signals of colourants enhanced obviously, and more importantly, the signal enhancement abilities of PC were also dependent on the starch/nano-CaCO 3 weight ratio. The greatly-increased electron transfer ability and accumulation efficiency were the main reason for the enhanced signals of colourants, as confirmed by electrochemical impedance spectroscopy and chronocoulometry. The prepared PC-2 sample by 1:1 starch/nano-CaCO 3 weight ratio was more active for the oxidation of food colourtants, and increased the signals by 89.4-fold, 79.3-fold, 47.3-fold and 50.7-fold for Sunset yellow, Tartrazine, Ponceau 4R and Allura red. As a result, a highly-sensitive electrochemical sensing platform was developed, and the detection limits were 1.4, 3.5, 2.1 and 1.7 μg L −1 for Sunset yellow, Tartrazine, Ponceau 4R and Allura red. The practical application of this new sensing platform was demonstrated using drink samples, and the detected results consisted with the values that obtained by high-performance liquid chromatography. - Highlights: • PC samples with different morphology and electrochemical activities were prepared. • Highly sensitive electrochemical sensing platform was developed for food colourants. • The accuracy and practicability was testified to be good by HPLC

Electrochemical functionalization of glassy carbon electrode by reduction of diazonium cations in protic ionic liquid

International Nuclear Information System (INIS)

Shul, Galyna; Ruiz, Carlos Alberto Castro; Rochefort, Dominic; Brooksby, Paula A.; Bélanger, Daniel

2013-01-01

Protic ionic liquid based on 2-methoxypyridine and trifluoroacetic acid was used as electrolyte for the functionalization of a glassy carbon electrode surface by electrochemical reduction of in situ generated 4-chlorobenzene diazonium and 4-nitrobenzene diazonium cations. The diazonium cations were synthesized in an electrochemical cell by reaction of the corresponding amines with NaNO 2 dissolved in protic ionic liquid. The resulting electrografted organic layers exhibit similar properties to those layers obtained by the derivatization from isolated diazonium salts dissolved in protic ionic liquid. Functionalized glassy carbon electrode surfaces were characterized by cyclic voltammetry, Fourier transform infrared and X-ray photoelectron spectroscopies. Atomic force microscopy thickness measurements revealed that, in our experimental conditions, the use of protic ionic liquid led to the formation of film with a thickness of about 1.5 nm. It is also demonstrated that the nitrobenzene chemisorbed on glassy carbon electrode or dissolved in protic ionic liquid undergoes electrochemical conversion to hydroxyaminobenzene

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.

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.

Characterization of the silicon/hydrofluoric acid interface: electrochemical processes under weak potential disturbance

International Nuclear Information System (INIS)

Bertagna, Valerie

1996-01-01

Within the frame of the increase of the density of integrated circuits, of simplification of cleaning processes and of improvement of control of surface reactions (for a better control of the elimination of defects and contamination risks), this research thesis first gives a large overview of previous works in the fields of silicon electrochemistry in hydrofluoric environment, of silicon chemical condition after treatment by a diluted hydrofluoric acid, of metallic contamination of silicon during cleaning with a diluted hydrofluoric acid, and of theoretical models of interpretation. Then, the author reports the development of a new electrochemical cell, and the detailed study of mono-crystalline silicon in a diluted hydrofluoric environment (electrochemical investigation, modelling of charge transfer at the interface, studies by atomic force microscopy, contamination of silicon by copper)

Electrochemical Single‐Molecule AFM of the Redox Metalloenzyme Copper Nitrite Reductase in Action

DEFF Research Database (Denmark)

Hao, Xian; Zhang, Jingdong; Christensen, Hans Erik Mølager

2012-01-01

We studied the electrochemical behavior of the redox metalloenzyme copper nitrite reductase (CNiR, Achromobacter xylosoxidans) immobilized on a Au(111)‐electrode surface modified by a self‐assembled cysteamine molecular monolayer (SAM) using a combination of cyclic voltammetry and electrochemically......‐controlled atomic force microscopy (in situ AFM). The enzyme showed no voltammetric signals in the absence of nitrite substrate, whereas a strong reductive electrocatalytic signal appeared in the presence of nitrite. Such a pattern is common in protein film and monolayer voltammetry and points to conformational...... in the presence of nitrite. No change in size was observed in the absence of nitrite over the same potential range. The enzyme size variation is suggested to offer clues to the broadly observed substrate triggering in metalloenzyme monolayer voltammetry....

Surface-treated commercially pure titanium for biomedical applications: Electrochemical, structural, mechanical and chemical characterizations

International Nuclear Information System (INIS)

Ogawa, Erika S.; Matos, Adaias O.; Beline, Thamara; Marques, Isabella S.V.; Sukotjo, Cortino; Mathew, Mathew T.; Rangel, Elidiane C.; Cruz, Nilson C.; Mesquita, Marcelo F.; Consani, Rafael X.

2016-01-01

Modified surfaces have improved the biological performance and biomechanical fixation of dental implants compared to machined (polished) surfaces. However, there is a lack of knowledge about the surface properties of titanium (Ti) as a function of different surface treatment. This study investigated the role of surface treatments on the electrochemical, structural, mechanical and chemical properties of commercial pure titanium (cp-Ti) under different electrolytes. Cp-Ti discs were divided into 6 groups (n = 5): machined (M—control); etched with HCl + H_2O_2 (Cl), H_2SO_4 + H_2O_2 (S); sandblasted with Al_2O_3 (Sb), Al_2O_3 followed by HCl + H_2O_2 (SbCl), and Al_2O_3 followed by H_2SO_4 + H_2O_2 (SbS). Electrochemical tests were conducted in artificial saliva (pHs 3; 6.5 and 9) and simulated body fluid (SBF—pH 7.4). All surfaces were characterized before and after corrosion tests using atomic force microscopy, scanning electron microscopy, energy dispersive microscopy, X-ray diffraction, surface roughness, Vickers microhardness and surface free energy. The results indicated that Cl group exhibited the highest polarization resistance (R_p) and the lowest capacitance (Q) and corrosion current density (I_c_o_r_r) values. Reduced corrosion stability was noted for the sandblasted groups. Acidic artificial saliva decreased the R_p values of cp-Ti surfaces and produced the highest I_c_o_r_r values. Also, the surface treatment and corrosion process influenced the surface roughness, Vickers microhardness and surface free energy. Based on these results, it can be concluded that acid-etching treatment improved the electrochemical stability of cp-Ti and all treated surfaces behaved negatively in acidic artificial saliva. - Highlights: • Characterization of surface treatment for biomedical implants was investigated. • Sandblasting reduced the corrosion stability of cp-Ti. • Acid etching is a promising dental implants surface treatment.

Surface-treated commercially pure titanium for biomedical applications: Electrochemical, structural, mechanical and chemical characterizations

Energy Technology Data Exchange (ETDEWEB)

Ogawa, Erika S.; Matos, Adaias O.; 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); 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); Sukotjo, Cortino [Department of Restorative Dentistry, University of Illinois at Chicago, College of Dentistry, 801 S Paulina, Chicago, IL, USA, 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 Biomedical Sciences, University of Illinois, College of Medicine at Rockford, 1601 Parkview Avenue, Rockford, IL, USA, 61107 (United States); Rangel, Elidiane C.; Cruz, Nilson C. [IBTN/Br—Institute of Biomaterials, Tribocorrosion and Nanomedicine—Brazilian Branch (Brazil); Laboratory of Technological Plasmas, Engineering College, Univ Estadual Paulista (UNESP), Av Três de Março, 511, Sorocaba, São Paulo 18087-180 (Brazil); Mesquita, Marcelo F.; Consani, Rafael X. [Department of Prosthodontics and Periodontology, Piracicaba Dental School, University of Campinas (UNICAMP), Av Limeira, 901, Piracicaba, São Paulo 13414-903 (Brazil); and others

2016-08-01

Modified surfaces have improved the biological performance and biomechanical fixation of dental implants compared to machined (polished) surfaces. However, there is a lack of knowledge about the surface properties of titanium (Ti) as a function of different surface treatment. This study investigated the role of surface treatments on the electrochemical, structural, mechanical and chemical properties of commercial pure titanium (cp-Ti) under different electrolytes. Cp-Ti discs were divided into 6 groups (n = 5): machined (M—control); etched with HCl + H{sub 2}O{sub 2} (Cl), H{sub 2}SO{sub 4} + H{sub 2}O{sub 2} (S); sandblasted with Al{sub 2}O{sub 3} (Sb), Al{sub 2}O{sub 3} followed by HCl + H{sub 2}O{sub 2} (SbCl), and Al{sub 2}O{sub 3} followed by H{sub 2}SO{sub 4} + H{sub 2}O{sub 2} (SbS). Electrochemical tests were conducted in artificial saliva (pHs 3; 6.5 and 9) and simulated body fluid (SBF—pH 7.4). All surfaces were characterized before and after corrosion tests using atomic force microscopy, scanning electron microscopy, energy dispersive microscopy, X-ray diffraction, surface roughness, Vickers microhardness and surface free energy. The results indicated that Cl group exhibited the highest polarization resistance (R{sub p}) and the lowest capacitance (Q) and corrosion current density (I{sub corr}) values. Reduced corrosion stability was noted for the sandblasted groups. Acidic artificial saliva decreased the R{sub p} values of cp-Ti surfaces and produced the highest I{sub corr} values. Also, the surface treatment and corrosion process influenced the surface roughness, Vickers microhardness and surface free energy. Based on these results, it can be concluded that acid-etching treatment improved the electrochemical stability of cp-Ti and all treated surfaces behaved negatively in acidic artificial saliva. - Highlights: • Characterization of surface treatment for biomedical implants was investigated. • Sandblasting reduced the corrosion stability of cp

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

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.

Graphene-supported SnO2 nanoparticles prepared by a solvothermal approach for an enhanced electrochemical performance in lithium-ion batteries

OpenAIRE

Wang, Bei; Su, Dawei; Park, Jinsoo; Ahn, Hyojun; Wang, Guoxiu

2012-01-01

SnO2 nanoparticles were dispersed on graphene nanosheets through a solvothermal approach using ethylene glycol as the solvent. The uniform distribution of SnO2 nanoparticles on graphene nanosheets has been confirmed by scanning electron microscopy and transmission electron microscopy. The particle size of SnO2 was determined to be around 5 nm. The as-synthesized SnO2/graphene nanocomposite exhibited an enhanced electrochemical performance in lithium-ion batteries, compared with bare graphene ...

Electrochemical and morphological investigation of silver and zinc modified calcium phosphate bioceramic coatings on metallic implant materials

International Nuclear Information System (INIS)

Furko, M.; Jiang, Y.; Wilkins, T.A.; Balázsi, C.

2016-01-01

In our research nanostructured silver and zinc doped calcium-phosphate (CaP) bioceramic coatings were prepared on commonly used orthopaedic implant materials (Ti6Al4V). The deposition process was carried out by the pulse current technique at 70 °C from electrolyte containing the appropriate amount of Ca(NO_3)_2 and NH_4H_2PO_4 components. During the electrochemical deposition Ag"+ and Zn"2"+ ions were introduced into the solution. The electrochemical behaviour and corrosion rate of the bioceramic coatings were investigated by potentiodynamic polarization and Electrochemical Impedance Spectroscopy (EIS) measurements in conventional Ringer's solution in a three electrode open cell. The coating came into contact with the electrolyte and corrosion occurred during immersion. In order to achieve antimicrobial properties, it is important to maintain a continuous release of silver ions into physiological media, while the bioactive CaP layer enhances the biocompatibility properties of the layer by fostering the bone cell growth. The role of Zn"2"+ is to shorten wound healing time. Morphology and composition of coatings were studied by Scanning Electron Microscopy, Transmission Electron Microscopy and Energy-dispersive X-ray spectroscopy. Differential thermal analyses (DTA) were performed to determine the thermal stability of the pure and modified CaP bioceramic coatings while the structure and phases of the layers were characterized by X-ray diffraction (XRD) measurements. - Highlights: • Ag and Zn doped calcium phosphate (CaP) layers were electrochemically deposited. • Layer degradation was studied by EIS and potentiodynamic measurements. • The bioceramic coatings became passive after a period of immersion time. • Ag and Zn modified layer shows higher degradation rate compared to pure CaP coating.

Effects of Electrodeposition Mode and Deposition Cycle on the Electrochemical Performance of MnO2-NiO Composite Electrodes for High-Energy-Density Supercapacitors.

Science.gov (United States)

Rusi; Majid, S R

2016-01-01

Nanostructured network-like MnO2-NiO composite electrodes were electrodeposited onto stainless steel substrates via different electrodeposition modes, such as chronopotentiometry, chronoamperometry, and cyclic voltammetry, and then subjected to heat treatment at 300°C for metal oxide conversion. X-ray diffraction, field emission scanning electron microscopy, and transmission electron microscopy were used to study the crystalline natures and morphologies of the deposited films. The electrochemical properties were investigated using cyclic voltammetry and charge/discharge tests. The results revealed that the electrochemical performance of the as-obtained composite electrodes depended on the electrodeposition mode. The electrochemical properties of MnO2-NiO composite electrodes prepared using cyclic voltammetry exhibited the highest capacitance values and were most influenced by the deposition cycle number. The optimum specific capacitance was 3509 Fg-1 with energy and power densities of 1322 Wh kg-1 and 110.5 kW kg-1, respectively, at a current density of 20 Ag-1 in a mixed KOH/K3Fe(CN)6 electrolyte.

Effects of Electrodeposition Mode and Deposition Cycle on the Electrochemical Performance of MnO2-NiO Composite Electrodes for High-Energy-Density Supercapacitors.

Directory of Open Access Journals (Sweden)

Rusi

Full Text Available Nanostructured network-like MnO2-NiO composite electrodes were electrodeposited onto stainless steel substrates via different electrodeposition modes, such as chronopotentiometry, chronoamperometry, and cyclic voltammetry, and then subjected to heat treatment at 300°C for metal oxide conversion. X-ray diffraction, field emission scanning electron microscopy, and transmission electron microscopy were used to study the crystalline natures and morphologies of the deposited films. The electrochemical properties were investigated using cyclic voltammetry and charge/discharge tests. The results revealed that the electrochemical performance of the as-obtained composite electrodes depended on the electrodeposition mode. The electrochemical properties of MnO2-NiO composite electrodes prepared using cyclic voltammetry exhibited the highest capacitance values and were most influenced by the deposition cycle number. The optimum specific capacitance was 3509 Fg-1 with energy and power densities of 1322 Wh kg-1 and 110.5 kW kg-1, respectively, at a current density of 20 Ag-1 in a mixed KOH/K3Fe(CN6 electrolyte.

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)

Synthesis and electrochemical properties of nanosized LiFeO2 particles with a layered rocksalt structure for lithium batteries

International Nuclear Information System (INIS)

Hirayama, Masaaki; Tomita, Hiroki; Kubota, Kei; Ido, Hidekazu; Kanno, Ryoji

2012-01-01

Highlights: ► 40-nm-sized O3-LiFeO 2 exhibits higher discharge capacities and rate characteristics than 400-nm-sized O3-LiFeO 2 . ► The cation disorder of Li and Fe ions might have affected the electrochemical activity of the O3-LiFeO 2 nanoparticles. ► A phase change from a layered structure to a cubic structure during electrochemical cycling. ► The new cubic phase allowed a stable electrochemical reaction between 4.5 and 1.0 V. -- Abstract: Layered rocksalt-type LiFeO 2 particles (O3-LiFeO 2 ) with average particle sizes of ca. 40 and 400 nm were synthesized by an ion exchange reaction from α-NaFeO 2 precursors. X-ray diffraction (XRD) patterns and scanning electron microscopy (SEM) images confirmed the formation of nanosized O3-LiFeO 2 . 40-nm LiFeO 2 exhibited a higher discharge capacity (115 mAh g −1 ) than 400-nm LiFeO 2 (80 mAh g −1 ), and also had better rate characteristics. The downsizing effect and cation disorder between the lithium and iron layers may have improved the electrochemical activity of the LiFeO 2 particles. Transmission electron microscopy (TEM) observation indicated a phase transition from O3-LiFeO 2 to a cubic lattice system during the electrochemical process. The cubic lithium iron oxide exhibited stable electrochemical reactions based on the Fe 2+ /Fe 3+ and Fe 2+ /Fe 0 redox couples at voltages between 4.5 and 1.0 V. The discharge capacities of 40-nm LiFeO 2 were ca. 115, 210, and 390 mAh g −1 under cutoff voltages of 4.5–2.0 V, 4.5–1.5 V, and 4.5–1.0 V, respectively.

Tunable atomic force microscopy bias lithography on electron beam induced carbonaceous platforms

Directory of Open Access Journals (Sweden)

Narendra Kurra

2013-09-01

Full Text Available Tunable local electrochemical and physical modifications on the carbonaceous platforms are achieved using Atomic force microscope (AFM bias lithography. These carbonaceous platforms are produced on Si substrate by the technique called electron beam induced carbonaceous deposition (EBICD. EBICD is composed of functionalized carbon species, confirmed through X-ray photoelectron spectroscopy (XPS analysis. AFM bias lithography in tapping mode with a positive tip bias resulted in the nucleation of attoliter water on the EBICD surface under moderate humidity conditions (45%. While the lithography in the contact mode with a negative tip bias caused the electrochemical modifications such as anodic oxidation and etching of the EBICD under moderate (45% and higher (60% humidity conditions respectively. Finally, reversible charge patterns are created on these EBICD surfaces under low (30% humidity conditions and investigated by means of electrostatic force microscopy (EFM.

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.

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)

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

CuO nanoparticle sensor for the electrochemical determination of dopamine

International Nuclear Information System (INIS)

Reddy, Sathish; Kumara Swamy, B.E.; Jayadevappa, H.

2012-01-01

Highlights: ► The MCPE prepared from flake-shaped CuO nanoparticles exhibits good electrocatalytic activity for DA compared with MCPE prepared from rod-shaped CuO nanoparticles. ► The MCPE prepared from SDS/polyglycine/flake-shaped CuO nanoparticles strong electrocatalytic enhancement of redox peak currents for DA and large peak potential separation between E AA − E DA . ► Analysis of DA shows linearly increase in anodic peak current in presence of excess ascorbic acid. ► Ease of preparation and good analytical response supports its claim for use as a potential dopamine sensor. - Abstract: In the present work, different shaped CuO nanoparticles were synthesized using cetyl trimethyl ammonium bromide (CTAB) and sodium dodecyl sulfate (SDS) in a co-precipitation method. The CuO nanoparticles were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), infrared absorption spectroscopy (IR) and UV–visible absorption spectroscopy (UV–vis). The prepared CuO nanoparticles were used for the preparation of modified carbon-paste electrodes (MCPE) for the electrochemical detection of dopamine (DA) at pH 6.0. The MCPE prepared from flake-shaped CuO nanoparticles exhibited an enhanced current response for DA. Electrochemical parameters, such as the surface area of the electrode, the heterogeneous rate constant (k s ) and the lower detection limit (5.5 × 10 −8 M), were calculated and compared with those of the MCPE prepared from rod-shaped CuO nanoparticles. The MCPE prepared from SDS/polyglycine/flake-shaped CuO nanoparticles exhibited a further improved current response for DA and a high selectivity (E AA − E DA = 0.28 V) for the simultaneous investigation of DA and ascorbic acid (AA) at pH 6.0. The modified carbon-paste electrochemical sensors were compared, and the MCPE prepared from SDS/polyglycine/flake-shaped CuO nanoparticles exhibited better performance than the MCPE prepared from CTAB

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.

Lipid Bilayer Membrane in a Silicon Based Micron Sized Cavity Accessed by Atomic Force Microscopy and Electrochemical Impedance Spectroscopy.

Science.gov (United States)

Khan, Muhammad Shuja; Dosoky, Noura Sayed; Patel, Darayas; Weimer, Jeffrey; Williams, John Dalton

2017-07-05

Supported lipid bilayers (SLBs) are widely used in biophysical research to probe the functionality of biological membranes and to provide diagnoses in high throughput drug screening. Formation of SLBs at below phase transition temperature ( Tm ) has applications in nano-medicine research where low temperature profiles are required. Herein, we report the successful production of SLBs at above-as well as below-the Tm of the lipids in an anisotropically etched, silicon-based micro-cavity. The Si-based cavity walls exhibit controlled temperature which assist in the quick and stable formation of lipid bilayer membranes. Fusion of large unilamellar vesicles was monitored in real time in an aqueous environment inside the Si cavity using atomic force microscopy (AFM), and the lateral organization of the lipid molecules was characterized until the formation of the SLBs. The stability of SLBs produced was also characterized by recording the electrical resistance and the capacitance using electrochemical impedance spectroscopy (EIS). Analysis was done in the frequency regime of 10 -2 -10⁵ Hz at a signal voltage of 100 mV and giga-ohm sealed impedance was obtained continuously over four days. Finally, the cantilever tip in AFM was utilized to estimate the bilayer thickness and to calculate the rupture force at the interface of the tip and the SLB. We anticipate that a silicon-based, micron-sized cavity has the potential to produce highly-stable SLBs below their Tm . The membranes inside the Si cavity could last for several days and allow robust characterization using AFM or EIS. This could be an excellent platform for nanomedicine experiments that require low operating temperatures.

Electrochemical detection of acetaminophen on the functionalized MWCNTs modified electrode using layer-by-layer technique

International Nuclear Information System (INIS)

Manjunatha, Revanasiddappa; Nagaraju, Dodahalli Hanumantharayudu; Suresh, Gurukar Shivappa; Melo, Jose Savio; D'Souza, Stanislaus F.; Venkatesha, Thimmappa Venkatarangaiah

2011-01-01

A selective electrochemical method is fabricated via layer-by-layer (LBL) method using both positively and negatively charged multi walled carbon nanotubes (MWCNTs) on poly (diallyldimetheylammonium chloride) (PDDA)/poly styrene sulfonate (PSS) modified graphite electrode, for the determination of acetaminophen (ACT) in the presence of dopamine (DA) and high concentration of ascorbic acid (AA). The modified electrode was characterized by cyclic voltammetry (CV) electrochemical impedance spectroscopy (EIS), atomic force microscopy (AFM) and scanning electron microscopy (SEM). Experimental conditions such as pH, accumulation potential and time, effect of potential sweep rates and interferents were studied. In CV well defined peaks for AA, ACT and DA are obtained at 24, 186 and 374 mV, respectively. The separations of peaks were 210, 188 and 398 mV between AA and DA, DA and ACT and AA and ACT, respectively. The diffusion coefficient was calculated by chronocoulometric. Chronoamperometric studies showed the linear relationship between oxidation peak current and concentration of ACT in the range 25-400 μM (R = 0.9991). The detection limit was 5 x 10 -7 mol/L. The proposed method gave satisfactory results in the determination of ACT in pharmaceutical and human serum samples.

Novel Ag@TiO2 nanocomposite synthesized by electrochemically active biofilm for nonenzymatic hydrogen peroxide sensor

International Nuclear Information System (INIS)

Khan, Mohammad Mansoob; Ansari, Sajid Ali; Lee, Jintae; Cho, Moo Hwan

2013-01-01

A novel nonenzymatic sensor for H 2 O 2 was developed based on an Ag@TiO 2 nanocomposite synthesized using a simple and cost effective approach with an electrochemically active biofilm. The optical, structural, morphological and electrochemical properties of the as-prepared Ag@TiO 2 nanocomposite were examined by UV–vis spectroscopy, X-ray diffraction, transmission electron microscopy and cyclic voltammetry (CV). The Ag@TiO 2 nanocomposite was fabricated on a glassy carbon electrode (GCE) and their electrochemical performance was analyzed by CV, differential pulse voltammetry and electrochemical impedance spectroscopy. The Ag@TiO 2 nanocomposite modified GCE (Ag@TiO 2 /GCE) displayed excellent performance towards H 2 O 2 sensing at − 0.73 V in the linear response range from 0.83 μM to 43.3 μM, within a detection limit and sensitivity of 0.83 μM and ∼ 65.2328 ± 0.01 μAμM −1 cm −2 , respectively. In addition, Ag@TiO 2 /GCE exhibited good operational reproducibility and long term stability. - Graphical abstract: Synthesis of Ag@TiO 2 nanocomposite by electrochemically active biofilm for H 2 O 2 sensing. - Highlights: • Electrochemically active biofilm (EAB) • EAB mediated synthesis of Ag@TiO 2 nanocomposite • Ag@TiO 2 nanocomposite modified glassy carbon electrode • Ag@TiO 2 /GCE for H 2 O 2 sensing • Nonenzymatic sensor for H 2 O 2

Passivation of Si(111) surfaces with electrochemically grafted thin organic films

Science.gov (United States)

Roodenko, K.; Yang, F.; Hunger, R.; Esser, N.; Hinrichs, K.; Rappich, J.

2010-09-01

Ultra thin organic films (about 5 nm thick) of nitrobenzene and 4-methoxydiphenylamine were deposited electrochemically on p-Si(111) surfaces from benzene diazonium compounds. Studies based on atomic force microscopy, infrared spectroscopic ellipsometry and x-ray photoelectron spectroscopy showed that upon exposure to atmospheric conditions the oxidation of the silicon interface proceed slower on organically modified surfaces than on unmodified hydrogen passivated p-Si(111) surfaces. Effects of HF treatment on the oxidized organic/Si interface and on the organic layer itself are discussed.

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)

Low temperature thermal ageing embrittlement of austenitic stainless steel welds and its electrochemical assessment

International Nuclear Information System (INIS)

Chandra, K.; Kain, Vivekanand; Raja, V.S.; Tewari, R.; Dey, G.K.

2012-01-01

Highlights: ► Embrittlement study of austenitic stainless steel welds after ageing up to 20,000 h. ► Spinodal decomposition and G-phase precipitation in ferrite at 400 °C. ► Spinodal decomposition of ferrite at 335 and 365 °C. ► Large decrease in corrosion resistance due to G-phase precipitation. ► Good correlation between electrochemical properties and the degree of embrittlement. - Abstract: The low temperature thermal ageing embrittlement of austenitic stainless steel welds is investigated after ageing up to 20,000 h at 335, 365 and 400 °C. Spinodal decomposition and G-phase precipitation after thermal ageing were identified by transmission electron microscopy. Ageing led to increase in hardness of the ferrite phase while there was no change in the hardness of austenite. The degree of embrittlement was evaluated by non-destructive methods, e.g., double-loop and single-loop electrochemical potentiokinetic reactivation tests. A good correlation was obtained between the electrochemical properties and hardening of the ferrite phase of the aged materials.

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.

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.

Characterization of thin CeO{sub 2} films electrochemically deposited on HOPG

Energy Technology Data Exchange (ETDEWEB)

Faisal, Firas [Lehrstuhl für Physikalische Chemie II, Friedrich-Alexander-Universität Erlangen-Nürnberg, Egerlandstrasse 3, 91058 Erlangen (Germany); Toghan, Arafat, E-mail: arafat.toghan@yahoo.com [Lehrstuhl für Physikalische Chemie II, Friedrich-Alexander-Universität Erlangen-Nürnberg, Egerlandstrasse 3, 91058 Erlangen (Germany); Chemistry Department, Faculty of Science, South Valley University, 83523 Qena (Egypt); Khalakhan, Ivan; Vorokhta, Mykhailo; Matolin, Vladimír [Department of Surface and Plasma Science, Charles University in Prague, V Holešovičkách 747/2, 180 00 Prague 8 (Czech Republic); Libuda, Jörg [Lehrstuhl für Physikalische Chemie II, Friedrich-Alexander-Universität Erlangen-Nürnberg, Egerlandstrasse 3, 91058 Erlangen (Germany); Erlangen Catalysis Resource Center, Friedrich-Alexander-Universität Erlangen-Nürnberg, Egerlandstrasse 3, 91058 Erlangen (Germany)

2015-09-30

Graphical abstract: - Highlights: • Preparation of proton exchange membrane fuel cells catalyst using electrochemical thin film deposition. • Electrodeposition thin films of CeO{sub 2} on HOPG substrates. • The samples were characterized by in-situ AFM and ex-situ XPS. • XPS results reveal that the electrochemically deposited cerium oxide films are stoichiometric. • Exposing the films to ambient air, cracking structures are formed. - Abstract: Electrodeposition is widely used for industrial applications to deposit thin films, coatings, and adhesion layers. Herein, CeO{sub 2} thin films were deposited on a highly oriented pyrolytic graphite (HOPG) substrate by cathodic electrodeposition. The influence of the deposition parameters on the yield and on the film morphology is studied and discussed. Morphology and composition of the electrodeposited films were characterized by in-situ atomic force microscopy (AFM), scanning electron microscopy (SEM), Energy Dispersive X-ray spectroscopy (EDX), and X-ray photoelectron spectroscopy (XPS). By AFM we show that the thickness of CeO{sub 2} films can be controlled via the Ce{sup 3+} concentration in solution and the deposition time. After exposing the films to ambient air, cracking structures are formed, which were analyzed by AFM in detail. The chemical composition of the deposits was analyzed by XPS indicating the formation of nearly stoichiometric CeO{sub 2}.

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.

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.

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.

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 lithium insertion in graphite containing dispersed tin-antimony alloys

Energy Technology Data Exchange (ETDEWEB)

Billaud, Denis; Nabais, Catarina; Mercier, Cedric [LCSM, Laboratoire de Chimie du Solide Mineral, Nancy University, BP 239, 54506 Vandoeuvre les Nancy Cedex (France); Schneider, Raphael [LCPME, Laboratoire de Chimie Physique et Microbiologie pour l' Environnement, Nancy University, Faculte de Pharmacie, BP 80 403, 54001 Nancy Cedex (France); Willmann, Patrick [CNES, Centre National d' Etudes Spatiales, 18, Avenue E. Belin, 31055 Toulouse Cedex (France)

2008-09-15

Graphite/SnSb composites were prepared by solution-phase reduction of SnCl{sub 2} and SbCl{sub 5} in the presence of graphite powder using either t-BuONa-activated NaH or t-BuOLi-activated LiH. Crude and washed materials were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and field emission gun-scanning electron microscopy (FEG-SEM). Electrochemical lithium insertion was carried out in both types of composites using voltammetry or galvanostatic charge/discharge techniques. It appeared that graphite-SnSb composites prepared using t-BuOLi-activated LiH as reductant displayed the highest reversible capacity (ca. 500 mA h g{sup -1}). This phenomenon is likely in relation with a better dispersion and grafting of metal particles on graphite, as suggested by FEG-SEM and TEM analyses. However, such dispersion appeared to increase significantly the irreversible capacity. (author)

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...

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.

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.

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.

Recent advances in polymer supporting layered double hydroxides nanocomposite for electrochemical biosensors

Science.gov (United States)

Dhanasekaran, T.; Padmanaban, A.; Gnanamoorthy, G.; Manigandan, R.; Praveen Kumar, S.; Stephen, A.; Narayanan, V.

2018-01-01

In recent years, layered double hydroxides (LDHs) materials having emerging due to their ability of intercalate a variety of anions, either organic or inorganic molecules. The most significance of the LDHs has been found potential applications in catalysis, wastewater treatment, and electrochemical sensors. The Mg-Al LDHs (MAL) and Poly-o-phenylenediamine @ Mg-Al LDHs (P-MAL) was prepared via simple one step hydrothermal method. As prepared material was characterized using many techniques such as, the structural and crystal phase was determined from XRD and Raman analyses. The functional groups were depicted using FT-IR spectroscopy. The optical propertied studied using diffuse reflectance spectroscopy UV-vis spectroscopy and the emission property were analyzed from Photoluminescence spectroscopy. The surface morphology and average particle size was analyzed using FESEM microscopy. The prepared polymer composite material P-MAL was further used for highly sensitive electrochemical detection towards dopamine (DA).

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...

Enhancing the water oxidation activity of Ni2P nanocatalysts by iron-doping and electrochemical activation

International Nuclear Information System (INIS)

Liu, Guang; He, Dongying; Yao, Rui; Zhao, Yong; Li, Jinping

2017-01-01

Highlights: •A sol-gel method for synthesis of Fe-doping Ni 2 P nanocatalysts was present. •Fe-doping Ni 2 P sample exhibited high OER activity after electrochemical activation. •In situ formed Fe-NiOOH layer on activated Fe-Ni 2 P provided more active OER sites. -- Abstract: In this work, we reported a facile and safe route for synthesis of Ni 2 P nanocatalysts by sol-gel method and demonstrated that the oxygen evolution reaction (OER) activity of Ni 2 P nanocatalysts can be dramatically enhanced by iron-doping and electrochemical activation. Compared with the fresh Fe-doped Ni 2 P nanocatalysts, a stable Fe-NiOOH layer was formed on the surface of Fe-doped Ni 2 P nanoparticles by electrochemical activation, thus promoting the charge transfer ability and surface electrochemically active sites generation for the electrochemical activated Fe-doped Ni 2 P nanocatalysts, ultimately accounting for the improvement of water oxidation activity, which was evidenced by cyclic voltammograms (CV), electrochemical impedance spectroscopy (EIS), X-ray photoelectron spectra (XPS) as well as high-resolution transmission electron microscopy (HR-TEM) measurements. For water oxidation reaction in 1 M KOH solution, the electrochemical activated Fe-doped Ni 2 P nanocatalysts can attain 10 mA/cm 2 at an overpotential of 292 mV with Tafel slope of 50 mV/dec, which was also much better than that of individual Ni 2 P, Fe 2 P nanocatalysts as well as commercial RuO 2 electrocatalyst. Moreover, long-term stability performance by chronoamperometric and chronopotentiometric tests for the activated Fe-doped Ni 2 P nanocatalysts exhibited no obvious decline within 56 h. It was demonstrated that modulating the OER catalytic activity for metal phosphide by iron-doping and electrochemical activation may provide new opportunities and avenues to engineer high performance electrocatalysts for water splitting.

Chemical and electrochemical synthesis of nano-sized TiO2 anatase for large-area photon conversion

International Nuclear Information System (INIS)

Babasaheb, Raghunath Sankapal; Shrikrishna, Dattatraya Sartale; Lux-Steiner, M.Ch.; Ennaoui, A.

2006-01-01

We report on the synthesis of nanocrystalline titanium dioxide thin films and powders by chemical and electrochemical deposition methods. Both methods are simple, inexpensive and suitable for large-scale production. Air-annealing of the films and powders at T = 500 C leads to densely packed nanometer sized anatase TiO 2 particles. The obtained layers are characterized by different methods such as: X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). Titanium dioxide TiO 2 (anatase) phase with (101) preferred orientation has been obtained for the films deposited on glass; indium doped tin oxide (ITO) and quartz substrates. The powder obtained as the byproduct consists of TiO 2 with anatase-phase as well. (authors)

Enhanced electrochemical performance of nano-sized LiFePO4/C synthesized by an ultrasonic-assisted co-precipitation method

International Nuclear Information System (INIS)

Liu Youyong; Cao Chuanbao

2010-01-01

A simple and effective method, the ultrasonic-assisted co-precipitation method, was employed to synthesize nano-sized LiFePO 4 /C. A glucose solution was used as the carbon source to produce in situ carbon to improve the conductivity of LiFePO 4 . Ultrasonic irradiation was adopted to control the size and homogenize the LiFePO 4 /C particles. The sample was characterized by X-ray powder diffraction, field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). FE-SEM and TEM show that the as-prepared sample has a reduced particle size with a uniform size distribution, which is around 50 nm. A uniform amorphous carbon layer with a thickness of about 4-6 nm on the particle surface was observed, as shown in the HRTEM image. The electrochemical performance was demonstrated by the charge-discharge test and electrochemical impedance spectra measurements. The results indicate that the nano-sized LiFePO 4 /C presents enhanced discharge capacities (159, 147 and 135 mAh g -1 at 0.1, 0.5 and 2 C-rate, respectively) and stable cycling performance. This study offers a simple method to design and synthesis nano-sized cathode materials for lithium-ion batteries.

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

Facile synthesis of core–shell structured PANI-Co{sub 3}O{sub 4} nanocomposites with superior electrochemical performance in supercapacitors

Energy Technology Data Exchange (ETDEWEB)

Hai, Zhenyin [Key Laboratory of Instrumentation and Dynamic Measurement of Ministry of Education, North University of China, Taiyuan, Shanxi 030051 (China); Gao, Libo [Department of Mechanical and Biomedical Engineering, City University of Hong Kong, Hong Kong SAR, Kowloon 999077 (Hong Kong); Zhang, Qiang [Key Laboratory of Instrumentation and Dynamic Measurement of Ministry of Education, North University of China, Taiyuan, Shanxi 030051 (China); Xu, Hongyan [School of Materials Science and Engineering, North University of China, Taiyuan, Shanxi 030051 (China); Cui, Danfeng; Zhang, Zengxing [Key Laboratory of Instrumentation and Dynamic Measurement of Ministry of Education, North University of China, Taiyuan, Shanxi 030051 (China); Tsoukalas, Dimitris [Department of Applied Physics, National Technical University of Athens, Zografou GR-15780 (Greece); Tang, Jun; Yan, Shubin [Key Laboratory of Instrumentation and Dynamic Measurement of Ministry of Education, North University of China, Taiyuan, Shanxi 030051 (China); Xue, Chenyang, E-mail: xuechenyang@nuc.edu.cn [Key Laboratory of Instrumentation and Dynamic Measurement of Ministry of Education, North University of China, Taiyuan, Shanxi 030051 (China)

2016-01-15

Graphical abstract: - Highlights: • PANI-Co{sub 3}O{sub 4} is synthesized by carbon-assisted and in situ polymerization methods. • PANI coating improves the properties of Co{sub 3}O{sub 4} affecting electrochemical performance. • The nanocomposites exhibit a high specific capacitance of 1184 F g{sup −1} at 1.25 A g{sup −1}. - Abstract: Core–shell structured PANI-Co{sub 3}O{sub 4} nanocomposites for supercapacitor applications were synthesized by combination of carbon-assisted method and in situ polymerization method. The crystalline structure, optical band gap, morphology, and hydrophilic property, as the major factors affecting the performances of supercapacitors, were investigated by X-ray diffraction (XRD), UV–vis spectrophotometry (UV–vis), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and water contact angle (WCA). The core–shell structured PANI-Co{sub 3}O{sub 4} nanocomposites are characterized by amorphous PANI, small bandgaps, large surface area and favorable hydrophilicity, which indicates the superior electrochemical performances of the nanocomposites as electrode material for supercapacitors. Cyclic voltammetry (CV), galvanostatic charge/discharge and electrochemical impedance spectroscopy (EIS) measurements were conducted in 6 M KOH aqueous solution to evaluate the electrochemical performances. The results shows that core–shell structured PANI-Co{sub 3}O{sub 4} nanocomposites exhibit a high specific capacitance of 1184 F g{sup −1} at 1.25 A g{sup −1}, excellent cycling stability of a capacitance retention of 84.9% after 1000 galvanostatic charge/discharge cycles, good electrical conductivity and ion diffusion behavior.

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.

Single- and multi-frequency detection of surface displacements via scanning probe microscopy.

Science.gov (United States)

Romanyuk, Konstantin; Luchkin, Sergey Yu; Ivanov, Maxim; Kalinin, Arseny; Kholkin, Andrei L

2015-02-01

Piezoresponse force microscopy (PFM) provides a novel opportunity to detect picometer-level displacements induced by an electric field applied through a conducting tip of an atomic force microscope (AFM). Recently, it was discovered that superb vertical sensitivity provided by PFM is high enough to monitor electric-field-induced ionic displacements in solids, the technique being referred to as electrochemical strain microscopy (ESM). ESM has been implemented only in multi-frequency detection modes such as dual AC resonance tracking (DART) and band excitation, where the response is recorded within a finite frequency range, typically around the first contact resonance. In this paper, we analyze and compare signal-to-noise ratios of the conventional single-frequency method with multi-frequency regimes of measuring surface displacements. Single-frequency detection ESM is demonstrated using a commercial AFM.

Rapid preparation of α-FeOOH and α-Fe2O3 nanostructures by microwave heating and their application in electrochemical sensors

International Nuclear Information System (INIS)

Marinho, J.Z.; Montes, R.H.O.; Moura, A.P. de; Longo, E.; Varela, J.A.; Munoz, R.A.A.; Lima, R.C.

2014-01-01

Graphical abstract: - Highlights: • Simple microwave method leads to the rapid formation of the goethite and hematite. • Homogenous nucleation and growth of particles are controlled by synthesis time. • Modified electrode with α-FeOOH nanoplates improved the electrochemical response. • The sample is directly heated by microwaves and its crystallization is accelerated. • Fe 3+ nanostructures are promising for development of electrochemical sensors. - Abstract: α-FeOOH (goethite) and α-Fe 2 O 3 (hematite) nanostructures have been successfully synthesized using the microwave-assisted hydrothermal (MAH) method and by the rapid burning in a microwave oven of the as-prepared goethite, respectively. The orthorhombic α-FeOOH to rhombohedralα-Fe 2 O 3 structural transformation was observed by X-ray diffraction (XRD) and Raman spectroscopy results. Plates-like α-FeOOH prepared in 2 min and rounded and quasi-octahedral shaped α-Fe 2 O 3 particles obtained in 10 min were observed using field emission gun scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The use of microwave heating allowed iron oxides to be prepared with shorter reaction times when compared to other synthesis methods. α-FeOOH nanoplates were incorporated into graphite-composite electrodes, which presented electrocatalytic properties towards the electrochemical oxidation of ascorbic acid in comparison with unmodified electrodes. This result demonstrates that such α-FeOOH nanostructures are very promising chemical modifiers for the development of improved electrochemical sensors

Enhanced corrosion resistance and biocompatibility of β-type Ti–25Nb–25Zr alloy by electrochemical anodization

Energy Technology Data Exchange (ETDEWEB)

Huang, Her-Hsiung [Department of Dentistry, National Yang-Ming University, Taipei, 112 Taiwan (China); Graduate Institute of Basic Medical Science, China Medical University, Taichung, 404 Taiwan (China); Department of Biomedical Informatics, Asia University, Taichung, 413 Taiwan (China); Department of Stomatology, Taipei Veterans General Hospital, Taipei, 112 Taiwan (China); Wu, Chia-Ping; Sun, Ying-Sui; Huang, Hsun-Miao [Institute of Oral Biology, National Yang-Ming University, Taipei, 112 Taiwan (China); Lee, Tzu-Hsin, E-mail: biomaterials@hotmail.com [School of Dentistry, Chung Shan Medical University, Taichung, 402 Taiwan (China); Oral Medicine Center, Chung Shan Medical University Hospital, Taichung, 402 Taiwan (China)

2013-12-31

The biocompatibility of implants is largely determined by their surface characteristics. This study presents a novel method for performing electrochemical anodization on β-type Ti–25Nb–25Zr alloy with a low elastic modulus (approximately 70 GPa). This method results in a thin hybrid layer capable of enhancing the surface characteristics of the implants. We investigated the surface topography and microstructure of the resulting Ti–25Nb–25Zr alloy. The corrosion resistance was evaluated using potentiodynamic polarization curve measurements in simulated body fluid. The cytotoxicity was evaluated according to International Organization for Standardization 10993–5 specification. Cell adhesion of human bone marrow mesenchymal stem cells on the test specimens was observed using scanning electron microscopy and fluorescence microscopy. The anodization produced a thin (approximately 40 nm-thick) hybrid oxide layer with a nanoporous outer sublayer (pore size < 15 nm) and a dense inner layer. The thin hybrid oxide layer increased the corrosion resistance of the Ti–25Nb–25Zr alloy by increasing the corrosion potential and decreasing both the corrosion rate and passive current. Ti–25Nb–25Zr alloys with and without anodization treatment were non-toxic. Surface nanotopography on the anodized Ti–25Nb–25Zr alloy enhanced protein adsorption and cell adhesion. Our results demonstrate that electrochemical anodization increases the corrosion resistance and cell adhesion of β-type Ti–25Nb–25Zr alloy while providing a lower elastic modulus suitable for implant applications. - Highlights: • An electrochemical anodization was applied to β-type Ti–25Nb–25Zr alloy surface. • Anodized surface had nanoscale hybrid oxide layer. • Anodized surface increased corrosion resistance due to dense inner sublayer. • Anodized surface enhanced cell adhesion due to nanoporous outer sublayer. • Electrochemical anodization has potential as implant surface treatment.

Enhanced corrosion resistance and biocompatibility of β-type Ti–25Nb–25Zr alloy by electrochemical anodization

International Nuclear Information System (INIS)

Huang, Her-Hsiung; Wu, Chia-Ping; Sun, Ying-Sui; Huang, Hsun-Miao; Lee, Tzu-Hsin

2013-01-01

The biocompatibility of implants is largely determined by their surface characteristics. This study presents a novel method for performing electrochemical anodization on β-type Ti–25Nb–25Zr alloy with a low elastic modulus (approximately 70 GPa). This method results in a thin hybrid layer capable of enhancing the surface characteristics of the implants. We investigated the surface topography and microstructure of the resulting Ti–25Nb–25Zr alloy. The corrosion resistance was evaluated using potentiodynamic polarization curve measurements in simulated body fluid. The cytotoxicity was evaluated according to International Organization for Standardization 10993–5 specification. Cell adhesion of human bone marrow mesenchymal stem cells on the test specimens was observed using scanning electron microscopy and fluorescence microscopy. The anodization produced a thin (approximately 40 nm-thick) hybrid oxide layer with a nanoporous outer sublayer (pore size < 15 nm) and a dense inner layer. The thin hybrid oxide layer increased the corrosion resistance of the Ti–25Nb–25Zr alloy by increasing the corrosion potential and decreasing both the corrosion rate and passive current. Ti–25Nb–25Zr alloys with and without anodization treatment were non-toxic. Surface nanotopography on the anodized Ti–25Nb–25Zr alloy enhanced protein adsorption and cell adhesion. Our results demonstrate that electrochemical anodization increases the corrosion resistance and cell adhesion of β-type Ti–25Nb–25Zr alloy while providing a lower elastic modulus suitable for implant applications. - Highlights: • An electrochemical anodization was applied to β-type Ti–25Nb–25Zr alloy surface. • Anodized surface had nanoscale hybrid oxide layer. • Anodized surface increased corrosion resistance due to dense inner sublayer. • Anodized surface enhanced cell adhesion due to nanoporous outer sublayer. • Electrochemical anodization has potential as implant surface treatment

Electrochemical and morphological investigation of silver and zinc modified calcium phosphate bioceramic coatings on metallic implant materials

Energy Technology Data Exchange (ETDEWEB)

Furko, M., E-mail: monika.furko@bayzoltan.hu [Bay Zoltán Nonprofit Ltd. for Applied Research, H-1116 Budapest, Fehérvári u. 130 (Hungary); Jiang, Y.; Wilkins, T.A. [Institute of Particle Science and Engineering, University of Leeds, LS2 9JT (United Kingdom); Balázsi, C. [Bay Zoltán Nonprofit Ltd. for Applied Research, H-1116 Budapest, Fehérvári u. 130 (Hungary)

2016-05-01

In our research nanostructured silver and zinc doped calcium-phosphate (CaP) bioceramic coatings were prepared on commonly used orthopaedic implant materials (Ti6Al4V). The deposition process was carried out by the pulse current technique at 70 °C from electrolyte containing the appropriate amount of Ca(NO{sub 3}){sub 2} and NH{sub 4}H{sub 2}PO{sub 4} components. During the electrochemical deposition Ag{sup +} and Zn{sup 2+} ions were introduced into the solution. The electrochemical behaviour and corrosion rate of the bioceramic coatings were investigated by potentiodynamic polarization and Electrochemical Impedance Spectroscopy (EIS) measurements in conventional Ringer's solution in a three electrode open cell. The coating came into contact with the electrolyte and corrosion occurred during immersion. In order to achieve antimicrobial properties, it is important to maintain a continuous release of silver ions into physiological media, while the bioactive CaP layer enhances the biocompatibility properties of the layer by fostering the bone cell growth. The role of Zn{sup 2+} is to shorten wound healing time. Morphology and composition of coatings were studied by Scanning Electron Microscopy, Transmission Electron Microscopy and Energy-dispersive X-ray spectroscopy. Differential thermal analyses (DTA) were performed to determine the thermal stability of the pure and modified CaP bioceramic coatings while the structure and phases of the layers were characterized by X-ray diffraction (XRD) measurements. - Highlights: • Ag and Zn doped calcium phosphate (CaP) layers were electrochemically deposited. • Layer degradation was studied by EIS and potentiodynamic measurements. • The bioceramic coatings became passive after a period of immersion time. • Ag and Zn modified layer shows higher degradation rate compared to pure CaP coating.

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....

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.

Characterizing the relationship between hyperstoichiometry, defect structure and local corrosion kinetics of uranium dioxide

International Nuclear Information System (INIS)

He Heming; Qin, Z.; Shoesmith, D.W.

2010-01-01

The ability of the UO 2 fluorite structure to accommodate large amounts of interstitial oxygen in various lattice sites leads to the formation of hyper-stoichiometric phases. The defect structures occurring in hyper-stoichiometric UO 2+x over the range 0.02 ≤ x ≤ 0.1 have been characterized by SEM/EDX and Raman analyses. The results demonstrate that as the nominal stoichiometry increases from 2.002 to 2.1, the diversity of defective structures existing on the UO 2+ surface also increases. Scanning electrochemical microscopy (SECM) measurements combined with a theoretical model were used to determine the rate constant for the reduction of the redox mediator ferrocene methanol, acting as a cathodic oxidant to corrode the four UO 2+x specimens. The rate constant was found to vary with location on the surface. Stoichiometric locations, with a well defined fluorite structure, exhibited very low corrosion rates. Higher rates were observed at more non-stoichiometric locations with the highest rates being obtained on locations exhibiting tetragonal distortions as their composition approached UO 2.33 . The distribution of rates increases with the degree of nominal non-stoichiometry as the diversity of microstructures existing on the UO 2+x surface increases.

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.

Dynamics of electrochemical lithiation/delithiation of graphene-encapsulated silicon nanoparticles studied by in-situ TEM.

Science.gov (United States)

Luo, Langli; Wu, Jinsong; Luo, Jiayan; Huang, Jiaxing; Dravid, Vinayak P

2014-01-24

The incorporation of nanostructured carbon has been recently reported as an effective approach to improve the cycling stability when Si is used as high-capacity anodes for the next generation Li-ion battery. However, the mechanism of such notable improvement remains unclear. Herein, we report in-situ transmission electron microscopy (TEM) studies to directly observe the dynamic electrochemical lithiation/delithiation processes of crumpled graphene-encapsulated Si nanoparticles to understand their physical and chemical transformations. Unexpectedly, in the first lithiation process, crystalline Si nanoparticles undergo an isotropic to anisotropic transition, which is not observed in pure crystalline and amorphous Si nanoparticles. Such a surprising phenomenon arises from the uniformly distributed localized voltage around the Si nanoparticles due to the highly conductive graphene sheets. It is observed that the intimate contact between graphene and Si is maintained during volume expansion/contraction. Electrochemical sintering process where small Si nanoparticles react and merge together to form large agglomerates following spikes in localized electric current is another problem for batteries. In-situ TEM shows that graphene sheets help maintain the capacity even in the course of electrochemical sintering. Such in-situ TEM observations provide valuable phenomenological insights into electrochemical phenomena, which may help optimize the configuration for further improved performance.

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.

Electrochemical behavior of an anticancer drug 5-fluorouracil at methylene blue modified carbon paste electrode

International Nuclear Information System (INIS)

Bukkitgar, Shikandar D.; Shetti, Nagaraj P.

2016-01-01

A novel sensor for the determination of 5-fluorouracil was constructed by electrochemical deposition of methylene blue on surface of carbon paste electrode. The electrode surface morphology was studied using Atomic force microscopy and XRD. The electrochemical activity of modified electrode was characterized using cyclic voltammetry and differential pulse method. The developed sensor shows impressive enlargement in sensitivity of 5-fluorouracil determination. The peak currents obtained from differential pulse voltammetry was linear with concentration of 5-fluorouracil in the range 4 × 10 −5 –1 × 10 −7 M and detection limit and quantification limit were calculated to be 2.04 nM and 6.18 nM respectively. Further, the sensor was successfully applied in pharmaceutical and biological fluid sample analysis. - Highlights: • Electrochemical oxidation of 5-fluorouracil has been investigated for first time at methylene blue modified carbon paste electrode • The electrode process was irreversible and diffusion controlled • Probable electrochemical mechanism was proposed which involved two proton and two electron transfer reaction • The LOD and LOQ values were calculated to be 2.04 nM and 6.18 nM, respectively, with good selectivity and sensitivity. • Proposed method was applied to 5-Fluorouracil determination in pharmaceutical and spiked human urine samples

Morphology-dependent Electrochemical Enhancements of Porous Carbon as Sensitive Determination Platform for Ascorbic Acid, Dopamine and Uric Acid

Science.gov (United States)

Cheng, Qin; Ji, Liudi; Wu, Kangbing; Zhang, Weikang

2016-02-01

Using starch as the carbon precursor and different-sized ZnO naoparticles as the hard template, a series of porous carbon materials for electrochemical sensing were prepared. Experiments of scanning electron microscopy, transmission electron microscopy and Nitrogen adsorption-desorption isotherms reveal that the particle size of ZnO has big impacts on the porous morphology and surface area of the resulting carbon materials. Through ultrasonic dispersion of porous carbon and subsequent solvent evaporation, different sensing interfaces were constructed on the surface of glassy carbon electrode (GCE). The electrochemical behaviors of ascorbic acid (AA), dopamine (DA) and uric acid (UA) were studied. On the surface of porous carbon materials, the accumulation efficiency and electron transfer ability of AA, DA and UA are improved, and consequently their oxidation signals enhance greatly. Moreover, the interface enhancement effects of porous carbon are also controlled by the particle size of hard template. The constructed porous carbon interface displays strong signal amplification ability and holds great promise in constructing a sensitive platform for the simultaneous determination of AA, DA and UA.

Electrochemical synthesis of MoS2 quantum dots embedded nanostructured porous silicon with enhanced electroluminescence property

Science.gov (United States)

Shrivastava, Megha; Kumari, Reeta; Parra, Mohammad Ramzan; Pandey, Padmini; Siddiqui, Hafsa; Haque, Fozia Z.

2017-11-01

In this report we present the successful enhancement in electroluminescence (EL) in nanostructured n-type porous silicon (PS) with an idea of embedding luminophorous Molybdenum disulfide (MoS2) quantum dots (QD's). Electrochemical anodization technique was used for the formation of PS surface and MoS2 QD's were prepared using the electrochemical route. Spin coating technique was employed for the proper incorporation of MoS2 QD's within the PS nanostructures. The crystallographic analysis was performed using X-ray diffraction (XRD), Raman and Fourier transform infrared (FT-IR) spectroscopy techniques. However, surface morphology was determined using Transmission electron microscopy (TEM) and Atomic force microscopy (AFM). The optical measurements were performed on photoluminescence (PL) spectrophotometer; additionally for electroluminescence (EL) study special arrangement of instrumental setup was made at laboratory level which provides novelty to this work. A diode prototype was made comprising Ag/MoS2:PS/Silicon/Ag for EL study. The MoS2:PS shows a remarkable concentration dependent enhancement in PL as well as in EL intensities, which paves a way to better utilize this strategy in optoelectronic device applications.

Nanostructured platform for the detection of Neisseria gonorrhoeae using electrochemical impedance spectroscopy and differential pulse voltammetry

International Nuclear Information System (INIS)

Singh, R.; Matharu, Z.; Srivastava, A.K.; Sood, S.; Gupta, R.K.; Malhotra, B.D.

2012-01-01

We report on a nanocomposite based genosensor for the detection of Neisseria gonorrhoeae, a bacterium causing the sexually transmitted disease gonorrhoea. Amino-labeled probe DNA was covalently immobilized on electrochemically prepared polyaniline and iron oxide (PANI-Fe 3 O 4 ) nanocomposite film on an indium tin oxide (ITO) electrode. Scanning electron microscopy, transmission electron microscopy, electrochemical impedance spectroscopy (EIS) and differential pulse voltammetry (DPV) techniques have been employed to characterize surface of the modified electrode. The genosensor has detection limits of 1 x 10 -15 M and 1 x 10 -17 M, respectively, using the EIS and DPV techniques. This biosensor can discriminate a complementary sequence from a single-base mismatch and from non-complementary DNA, and has been utilized for detection of DNA extracted from N. gonorrhoeae culture, and from patient samples with N. gonorrhoeae. It is found to exhibit good specificity for N. gonorrhoeae species and shows no response towards non-gonorrhoeae type of Neisseria species (NgNs) and other gram-negative bacterias (GNBs). The affinity constant for hybridization calculated using the Langmuir adsorption isotherm model is found to be 3. 39 x 10 8 M -1 . (author)

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 Grafting of Graphene Nano Platelets with Aryl Diazonium Salts.

Science.gov (United States)

Qiu, Zhipeng; Yu, Jun; Yan, Peng; Wang, Zhijie; Wan, Qijin; Yang, Nianjun

2016-10-26

To vary interfacial properties, electrochemical grafting of graphene nano platelets (GNP) with 3,5-dichlorophenyl diazonium tetrafluoroborate (aryl-Cl) and 4-nitrobenzene diazonium tetrafluoroborate (aryl-NO 2 ) was realized in a potentiodynamic mode. The covalently bonded aryl layers on GNP were characterized using atomic force microscopy and X-ray photoelectron spectroscopy. Electrochemical conversion of aryl-NO 2 into aryl-NH 2 was conducted. The voltammetric and impedance behavior of negatively and positively charged redox probes (Fe(CN) 6 3-/4- and Ru(NH 3 ) 6 2+/3+ ) on three kinds of aryl layers grafted on GNP reveal that their interfacial properties are determined by the charge states of redox probes and reactive terminal groups (-Cl, -NO 2 , -NH 2 ) in aryl layers. On aryl-Cl and aryl-NH 2 garted GNP, selective and sensitive monitoring of positively charged lead ions as well as negatively charged nitrite and sulfite ions was achieved, respectively. Such a grafting procedure is thus a perfect way to design and control interfacial properties of graphene.

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

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.

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.

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.

Ferrocenyl-doped silica nanoparticles as an immobilized affinity support for electrochemical immunoassay of cancer antigen 15-3

International Nuclear Information System (INIS)

Hong Chenglin; Yuan Ruo; Chai Yaqin; Zhuo Ying

2009-01-01

The aim of this study is to elaborate a simple and sensitive electrochemical immunoassay using ferrocenecarboxylic (Fc-COOH)-doped silica nanoparticles (SNPs) as an immobilized affinity support for cancer antigen 15-3 (CA 15-3) detection. The Fc-COOH-doped SNPs with redox-active were prepared by using a water-in-oil microemulsion method. The use of colloidal silica could prevent the leakage of Fc-COOH and were easily modified with trialkoxysilane reagents for covalent conjugation of CA 15-3 antibodies (anti-CA 15-3). The Fc-COOH-doped SNPs were characterized by X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). The fabrication process of the electrochemical immunosensor was demonstrated by using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) techniques. Under optimal conditions, the developed immunosensor showed good linearity at the studied concentration range of 2.0-240 U mL -1 with a coefficient 0.9986 and a detection limit of 0.64 U mL -1 at S/N = 3

Ferrocenyl-doped silica nanoparticles as an immobilized affinity support for electrochemical immunoassay of cancer antigen 15-3.

Science.gov (United States)

Hong, Chenglin; Yuan, Ruo; Chai, Yaqin; Zhuo, Ying

2009-02-09

The aim of this study is to elaborate a simple and sensitive electrochemical immunoassay using ferrocenecarboxylic (Fc-COOH)-doped silica nanoparticles (SNPs) as an immobilized affinity support for cancer antigen 15-3 (CA 15-3) detection. The Fc-COOH-doped SNPs with redox-active were prepared by using a water-in-oil microemulsion method. The use of colloidal silica could prevent the leakage of Fc-COOH and were easily modified with trialkoxysilane reagents for covalent conjugation of CA 15-3 antibodies (anti-CA 15-3). The Fc-COOH-doped SNPs were characterized by X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). The fabrication process of the electrochemical immunosensor was demonstrated by using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) techniques. Under optimal conditions, the developed immunosensor showed good linearity at the studied concentration range of 2.0-240 UmL(-1) with a coefficient 0.9986 and a detection limit of 0.64 UmL(-1) at S/N=3.

Improvement on the electrochemical characteristics of graphite anodes by coating of the pyrolytic carbon using tumbling chemical vapor deposition

International Nuclear Information System (INIS)

Han, Young-Soo; Lee, Jai-Young

2003-01-01

The electrochemical characteristics of graphite coated with pyrolytic carbon materials using tumbling chemical vapor deposition (CVD) process have been studied for the active material of anodes in lithium ion secondary batteries. Coating of pyrolytic carbons on the surface of graphite particles, which tumble in a rotating reactor tube, was performed through the pyrolysis of liquid propane gas (LPG). The surface morphology of these graphite particles coated with pyrolytic carbon has been observed with scanning electron microscopy (SEM). The surface of graphite particles can well be covered with pyrolytic carbon by tumbling CVD. High-resolution transmission electron microscopy (HRTEM) image of these carbon particles shows that the core part is highly ordered carbon, while the shell part is disordered carbon. We have found that the new-type carbon obtained from tumbling CVD has a uniform core (graphite)-shell (pyrolytic carbon) structure. The electrochemical property of the new-type carbons has been examined using a charge-discharge cycler. The coating of pyrolytic carbon on the surface of graphite can effectively reduce the initial irreversible capacity by 47.5%. Cyclability and rate-capability of theses carbons with the core-shell structure are much better than those of bare graphite. From electrochemical impedance spectroscopy (EIS) spectra, it is found that the coating of pyrolytic carbon on the surface of graphite causes the decrease of the contact resistance in the carbon electrodes, which means the formation of solid electrolyte interface (SEI) layer is suppressed. We suggest that coating of pyrolytic carbon by the tumbling CVD is an effective method in improving the electrochemical properties of graphite electrodes for lithium ion secondary batteries

Development of an Electrochemical Metal-Ion Biosensor Using Self-Assembled Peptide Nanofibrils

DEFF Research Database (Denmark)

Viguier, Bruno; Zor, Kinga; Kasotakis, Emmanouil

2011-01-01

. These nanofibrils were obtained under aqueous conditions, at room temperature and outside the clean room. The functionalized gold electrode was evaluated by cyclic voltammetry, impedance spectroscopy, energy dispersive X-ray and atomic force microscopy. The obtained results displayed a layer of nanofibrils able......This article describes the combination of self-assembled peptide nanofibrils with metal electrodes for the development of an electrochemical metal-ion biosensor. The biological nanofibrils were immobilized on gold electrodes and used as biorecognition elements for the complexation with copper ions...

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.

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)

New Insights on the Structure of Electrochemically Deposited Lithium Metal and Its Solid Electrolyte Interphases via Cryogenic TEM

Energy Technology Data Exchange (ETDEWEB)

Wang, Xuefeng; Zhang, Minghao; Alvarado, Judith; Wang, Shen; Sina, Mahsa; Lu, Bingyu; Bouwer, James; Xu, Wu [Energy; Xiao, Jie [Energy; Zhang, Ji-Guang [Energy; Liu, Jun [Energy; Meng, Ying Shirley

2017-11-02

Lithium metal has been considered as the “holy grail” anode material for rechargeable batteries though the dendritic growth and low Coulombic efficiency (CE) have crippled its practical use for decades. Its high chemical reactivity and low stability make it difficult to explore the intrinsic chemical and physical properties of the electrochemically deposited lithium (EDLi) and its accompanied solid electrolyte interphase (SEI). To prevent the dendritic growth and enhance the electrochemical reversibility, it is crucial to understand the nano- and meso- structures of EDLi. However, Li metal is very sensitive to beam damage and has low contrast for commonly used characterization techniques such as electron microscopy. Inspired by biological imaging techniques, this work demonstrates the power of cryogenic (cryo)- electron microscopy to reveal the detailed structure of EDLi and the SEI composition at the nano scale while minimizing beam damage during imaging. Surprisingly, the results show that the nucleation dominated EDLi (five minutes at 0.5 mA cm-2) is amorphous while there is some crystalline LiF present in the SEI. The EDLi grown from various electrolytes with different additives exhibits distinctive surface properties. Consequently, these results highlight the importance of the SEI and its relationship with the CE. Our findings not only illustrate the capabilities of cryogenic microscopy for beam (thermal)-sensitive materials, but it yields crucial structural information of the EDLi evolution with and without electrolyte additives.

Electrochemical characterization of glassy carbon electrode modified with 1,10-phenanthroline groups by two pathways: reduction of the corresponding diazonium ions and reduction of phenanthroline

International Nuclear Information System (INIS)

Shul, Galyna; Weissmann, Martin; Bélanger, Daniel

2015-01-01

The electrochemical behaviour of 1,10-phenanthroline molecules immobilized on a glassy carbon electrode surface by electrochemical reduction of the corresponding in-situ generated diazonium ions in an aqueous solution was investigated. Firstly, the derivatization of glassy carbon electrode was confirmed by the presence of the barrier effect in the solution of a redox probe. Secondly, atomic force microscopy measurements revealed the deposition of thin (< 2 nm) uniform 1,10-phenanthroline film on the surface of pyrolyzed photoresist film electrode. Thirdly, the initially electrochemically inactive grafted organic film became electroactive after being subjected to electrochemical reduction and oxidation. Fourthly, the electrochemical behaviour of phenanthroline modified electrode by electrochemical reduction of the corresponding diazonium cations was found to be similar to that of electrode modified by electrochemical reduction of only phenanthroline dissolved in an aqueous acid solution. Finally, cyclic voltammetry experiments using various methyl substituted phenanthroline derivatives provided direct evidence that functional groups responsible for the film electroactivity are formed at 5 or/and 6 positions of grafted phenanthroline molecules. On the other hand, a phenanthroline derivative having these positions blocked by methyl groups can also display electroactivity with position 7 being most likely involved in the observed redox process

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.

Chemical and electrochemical synthesis of nano-sized TiO{sub 2} anatase for large-area photon conversion

Energy Technology Data Exchange (ETDEWEB)

Babasaheb, Raghunath Sankapal; Shrikrishna, Dattatraya Sartale; Lux-Steiner, M.Ch.; Ennaoui, A. [Hahn-Meitner-Institut, Div. of Solar Energy Research, Berlin (Germany)

2006-05-15

We report on the synthesis of nanocrystalline titanium dioxide thin films and powders by chemical and electrochemical deposition methods. Both methods are simple, inexpensive and suitable for large-scale production. Air-annealing of the films and powders at T = 500 C leads to densely packed nanometer sized anatase TiO{sub 2} particles. The obtained layers are characterized by different methods such as: X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). Titanium dioxide TiO{sub 2} (anatase) phase with (101) preferred orientation has been obtained for the films deposited on glass; indium doped tin oxide (ITO) and quartz substrates. The powder obtained as the byproduct consists of TiO{sub 2} with anatase-phase as well. (authors)

Quadratic electromechanical strain in silicon investigated by scanning probe microscopy

Science.gov (United States)

Yu, Junxi; Esfahani, Ehsan Nasr; Zhu, Qingfeng; Shan, Dongliang; Jia, Tingting; Xie, Shuhong; Li, Jiangyu

2018-04-01

Piezoresponse force microscopy (PFM) is a powerful tool widely used to characterize piezoelectricity and ferroelectricity at the nanoscale. However, it is necessary to distinguish microscopic mechanisms between piezoelectricity and non-piezoelectric contributions measured by PFM. In this work, we systematically investigate the first and second harmonic apparent piezoresponses of a silicon wafer in both vertical and lateral modes, and we show that it exhibits an apparent electromechanical response that is quadratic to the applied electric field, possibly arising from ionic electrochemical dipoles induced by the charged probe. As a result, the electromechanical response measured is dominated by the second harmonic response in the vertical mode, and its polarity can be switched by the DC voltage with the evolving coercive field and maximum amplitude, in sharp contrast to typical ferroelectric materials we used as control. The ionic activity in silicon is also confirmed by the scanning thermo-ionic microscopy measurement, and the work points toward a set of methods to distinguish true piezoelectricity from the apparent ones.

Structure and electrochemical hydrogen storage properties of Ti2Ni alloy synthesized by ball milling

International Nuclear Information System (INIS)

Hosni, B.; Li, X.; Khaldi, C.; ElKedim, O.; Lamloumi, J.

2014-01-01

Highlights: • The Ti 2 Ni alloy activation requires only one cycle of charge and discharge, regardless of the temperature. • By increasing the temperature the capacity loss, undergoes an increase and it is more pronounced for the 60 °C. • A good correlation is found between the evolutions of the different electrochemical parameters according to the temperature. - Abstract: The structure and the electrochemical hydrogen storage properties of amorphous Ti 2 Ni alloy synthesized by ball milling and used as an anode in nickel–metal hydride batteries were studied. Nominal Ti 2 Ni was synthesized under argon atmosphere at room temperature using a planetary high-energy ball mill. The structural and morphological characterization of the amorphous Ti 2 Ni alloy is carried out by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The electrochemical characterization of the Ti 2 Ni electrodes is carried out by the galvanostatic charging and discharging, the constant potential discharge, the open circuit potential and the potentiodynamic polarization techniques. The Ti 2 Ni alloy activation requires only one cycle of charge and discharge, regardless of the temperature. The electrochemical discharge capacity of the Ti 2 Ni alloy, during the first eight cycles, and at a temperature of 30 °C, remained practically unchanged and a good held cycling is observed. By increasing the temperature, the electrochemical discharge capacity loss after eight cycles undergoes an increase and it is more pronounced for the temperature 60 °C. At 30 °C, the anodic corrosion current density is 1 mA cm −2 and then it undergoes a rapid drop, remaining substantially constant (0.06 mA cm −2 ) in the range 40–60 °C, before undergoing a slight increase to 70 °C (0.3 mA cm −2 ). This variation is in good agreement with the maximum electrochemical discharge capacity values found for the different temperatures. By increasing the

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.

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.

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.

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...

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.

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

Microstructural, mechanical and electrochemical behaviour of a 7017 Al–Zn–Mg alloy of different tempers

Energy Technology Data Exchange (ETDEWEB)

Rout, Prasanta Kumar, E-mail: prasantonnet55@yahoo.com; Ghosh, M.M.; Ghosh, K.S., E-mail: ksghosh2001@yahoo.co.uk

2015-06-15

The aim of the investigation is to assess the microstructural features and associated physical, mechanical and electrochemical properties of a 7017 Al–Zn–Mg alloy of various tempers. A 7017 Al–Zn–Mg alloy was subjected to different ageing schedules to produce under-(T4), peak-(T6), over-(T7) and highly over-aged tempers. Optical microscopy, hardness measurement, electrical conductivity measurement, tensile testing and SEM fractographs, differential scanning calorimetry (DSC), transmission electron microscopy (TEM), and electrochemical polarization studies have been used to characterize the alloy tempers. Hardness measurement and tensile testing showed the characteristic age hardening phenomenon of aluminium alloys. Optical and TEM micrographs have revealed the variation in size of matrix strengthening η′ (MgZn{sub 2}) and also the size and distribution of grain boundary η (MgZn{sub 2}) precipitate with ageing time. DSC thermograms exhibiting exothermic and endothermic peaks indicated the characteristic solid state reaction sequence of the 7017 alloy. Potentiodynamic polarization study of the 7017 alloy of various tempers in 3.5 wt.% NaCl solution at near neutral pH showed typical active metal dissolution behaviour, but at pH 12 an active–passive–transpassive transition behaviour has been observed. - Graphical abstract: TEM micrograph of the 7017 aluminium alloy of various tempers (a, b) under aged (T4), (c, d) peak aged (T6), (e, f) over aged (T7) and (g, h) highly over-aged. Display Omitted - Highlights: • 7017 Al-Zn-Mg alloy was subjected to different artificial ageing treatments. • Characterization of 7017 alloy tempers by hardness, tensile, DSC, TEM and electrochemical behaviour. • Structure-properties relationship of the 7017 Al-Zn-Mg alloy of various tempers.

Microwave synthesis and electrochemical characterization of mesoporous carbon@Bi{sub 2}O{sub 3} composites

Energy Technology Data Exchange (ETDEWEB)

Xia, Nannan [Department of Chemistry and Institute of Nanochemistry, Jinan University, Guangzhou 510632 (China); Yuan, Dingsheng, E-mail: tydsh@jnu.edu.cn [Department of Chemistry and Institute of Nanochemistry, Jinan University, Guangzhou 510632 (China); Zhou, Tianxiang; Chen, Jingxing; Mo, Shanshan; Liu, Yingliang [Department of Chemistry and Institute of Nanochemistry, Jinan University, Guangzhou 510632 (China)

2011-05-15

Graphical abstract: An efficient and quick microwave method has been employed to prepare worm-like mesoporous carbon@Bi{sub 2}O{sub 3} composites for the first time. The electrochemical measurement shows the worm-like mesoporous carbon@Bi{sub 2}O{sub 3} composites exhibits excellent capacitance performance and the maximum specific capacitance is up to 386 F g{sup -1}. Research highlights: {yields} An efficient and quick microwave method has been employed. {yields} A worm-like mesoporous carbon@Bi{sub 2}O{sub 3} composites have been successfully prepared. {yields} This composite exhibits excellent capacitance performance. {yields} This composite could be a potential electrode material for the supercapacitors. -- Abstract: An efficient and quick microwave method has been employed to prepare worm-like mesoporous carbon@Bi{sub 2}O{sub 3} composites for the first time. As-prepared products have been characterized by X-ray diffraction, N{sub 2} adsorption-desorption, scanning electron microscopy, transmission electron microscopy and inductive coupled plasma atomic emission spectroscopy. The electrochemical measurement shows the worm-like mesoporous carbon@Bi{sub 2}O{sub 3} composites exhibits excellent capacitance performance and the maximum specific capacitance reaches 386 F g{sup -1}, three times more than the pure worm-like mesoporous carbon.

Plasmonic optical antenna design for performing tip-enhanced Raman spectroscopy and microscopy

International Nuclear Information System (INIS)

Kharintsev, S S; Fishman, A I; Salakhov, M Kh; Hoffmann, G G

2013-01-01

This paper highlights optical plasmonic antennas designed with dc-pulsed low-voltage electrochemical etching of a gold wire for implementing tip-enhanced Raman scattering (TERS) measurements. We demonstrate a versatile electrochemical system that allows one to engineer TERS-active metallic gold tips with diverse shapes and sizes in a highly reproducible fashion. The underlying etching mechanism at a voltage-driven meniscus around a gold wire immersed into an electrolyte is discussed in detail. We show that the developed method is suitable to produce not only the simplest geometries such as cones and spheroids, but more complex designs. Attempts have been made to design plasmonic tapered antennas with quasi-uniformly spaced nano-sized bumps on the mesoscopic zone for the extra surface plasmon-light coupling. The capability of the patterned antenna to enhance and localize optical fields is demonstrated with near-field Raman microscopy and spectroscopy of single-walled carbon nanotubes bundles. (paper)

In situ study of Li-ions diffusion and deformation in Li-rich cathode materials by using scanning probe microscopy techniques

Science.gov (United States)

Zeng, Kaiyang; Li, Tao; Tian, Tian

2017-08-01

In this paper, the scanning probe microscopy (SPM) based techniques, namely, conductive-AFM, electrochemical strain microscopy (ESM) and AM-FM (amplitude modulation-frequency modulation) techniques, are used to in situ characterize the changes in topography, conductivity and elastic properties of Li-rich layered oxide cathode (Li1.2Mn0.54Ni0.13Co0.13O2) materials, in the form of nanoparticles, when subject to the external electric field. Nanoparticles are the basic building blocks for composite cathode in a Li-ion rechargeable battery. Characterization of the structure and electrochemical properties of the nanoparticles is very important to understand the performance and reliability of the battery materials and devices. In this study, the conductivity, deformation and mechanical properties of the Li-rich oxide nanoparticles under different polarities of biases are studied using the above-mentioned SPM techniques. This information can be correlated with the Li+-ion diffusion and migration in the particles under external electrical field. The results also confirm that the SPM techniques are ideal tools to study the changes in various properties of electrode materials at nano- to micro-scales during or after the ‘simulated’ battery operation conditions. These techniques can also be used to in situ characterize the electrochemical performances of other energy storage materials, especially in the form of the nanoparticles.

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.

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.

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.

Rapid preparation of α-FeOOH and α-Fe{sub 2}O{sub 3} nanostructures by microwave heating and their application in electrochemical sensors

Energy Technology Data Exchange (ETDEWEB)

Marinho, J.Z.; Montes, R.H.O. [Universidade Federal de Uberlândia, Instituto de Química, 38400-902 Uberlândia, MG (Brazil); Moura, A.P. de; Longo, E.; Varela, J.A. [Universidade Estadual Paulista, Instituto de Química, 14800-900 Araraquara, SP (Brazil); Munoz, R.A.A. [Universidade Federal de Uberlândia, Instituto de Química, 38400-902 Uberlândia, MG (Brazil); Lima, R.C., E-mail: rclima@iqufu.ufu.br [Universidade Federal de Uberlândia, Instituto de Química, 38400-902 Uberlândia, MG (Brazil)

2014-01-01

Graphical abstract: - Highlights: • Simple microwave method leads to the rapid formation of the goethite and hematite. • Homogenous nucleation and growth of particles are controlled by synthesis time. • Modified electrode with α-FeOOH nanoplates improved the electrochemical response. • The sample is directly heated by microwaves and its crystallization is accelerated. • Fe{sup 3+} nanostructures are promising for development of electrochemical sensors. - Abstract: α-FeOOH (goethite) and α-Fe{sub 2}O{sub 3} (hematite) nanostructures have been successfully synthesized using the microwave-assisted hydrothermal (MAH) method and by the rapid burning in a microwave oven of the as-prepared goethite, respectively. The orthorhombic α-FeOOH to rhombohedralα-Fe{sub 2}O{sub 3} structural transformation was observed by X-ray diffraction (XRD) and Raman spectroscopy results. Plates-like α-FeOOH prepared in 2 min and rounded and quasi-octahedral shaped α-Fe{sub 2}O{sub 3} particles obtained in 10 min were observed using field emission gun scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The use of microwave heating allowed iron oxides to be prepared with shorter reaction times when compared to other synthesis methods. α-FeOOH nanoplates were incorporated into graphite-composite electrodes, which presented electrocatalytic properties towards the electrochemical oxidation of ascorbic acid in comparison with unmodified electrodes. This result demonstrates that such α-FeOOH nanostructures are very promising chemical modifiers for the development of improved electrochemical sensors.

Studying the Kinetics of Crystalline Silicon Nanoparticle Lithiation with In Situ Transmission Electron Microscopy

KAUST Repository

McDowell, Matthew T.; Ryu, Ill; Lee, Seok Woo; Wang, Chongmin; Nix, William D.; Cui, Yi

2012-01-01

In situ transmission electron microscopy (TEM) is used to study the electrochemical lithiation of high-capacity crystalline Si nanoparticles for use in Li-ion battery anodes. The lithiation reaction slows down as it progresses into the particle interior, and analysis suggests that this behavior is due not to diffusion limitation but instead to the influence of mechanical stress on the driving force for reaction. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Studying the Kinetics of Crystalline Silicon Nanoparticle Lithiation with In Situ Transmission Electron Microscopy

KAUST Repository

McDowell, Matthew T.