Electrochemical Approach for Effective Antifouling and Antimicrobial Surfaces.

Science.gov (United States)

Gaw, Sheng Long; Sarkar, Sujoy; Nir, Sivan; Schnell, Yafit; Mandler, Daniel; Xu, Zhichuan J; Lee, Pooi See; Reches, Meital

2017-08-09

Biofouling, the adsorption of organisms to a surface, is a major problem today in many areas of our lives. This includes: (i) health, as biofouling on medical device leads to hospital-acquired infections, (ii) water, since the accumulation of organisms on membranes and pipes in desalination systems harms the function of the system, and (iii) energy, due to the heavy load of the organic layer that accumulates on marine vessels and causes a larger consumption of fuel. This paper presents an effective electrochemical approach for generating antifouling and antimicrobial surfaces. Distinct from previously reported antifouling or antimicrobial electrochemical studies, we demonstrate the formation of a hydrogen gas bubble layer through the application of a low-voltage square-waveform pulses to the conductive surface. This electrochemically generated gas bubble layer serves as a separation barrier between the surroundings and the target surface where the adhesion of bacteria can be deterred. Our results indicate that this barrier could effectively reduce the adsorption of bacteria to the surface by 99.5%. We propose that the antimicrobial mechanism correlates with the fundamental of hydrogen evolution reaction (HER). HER leads to an arid environment that does not allow the existence of live bacteria. In addition, we show that this drought condition kills the preadhered bacteria on the surface due to water stress. This work serves as the basis for the exploration of future self-sustainable antifouling techniques such as incorporating it with photocatalytic and photoelectrochemical reactions.

Effects of water plasma immersion ion implantation on surface electrochemical behavior of NiTi shape memory alloys in simulated body fluids

International Nuclear Information System (INIS)

Liu, X.M.; Wu, S.L.; Chu, Paul K.; Chung, C.Y.; Chu, C.L.; Yeung, K.W.K.; Lu, W.W.; Cheung, K.M.C.; Luk, K.D.K.

2007-01-01

Water plasma immersion ion implantation (PIII) was conducted on orthopedic NiTi shape memory alloy to enhance the surface electrochemical characteristics. The surface composition of the NiTi alloy before and after H 2 O-PIII was determined by X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM) was utilized to determine the roughness and morphology of the NiTi samples. Potentiodynamic polarization tests and electrochemical impedance spectroscopy (EIS) were carried out to investigate the surface electrochemical behavior of the control and H 2 O-PIII NiTi samples in simulated body fluids (SBF) at 37 deg. C as well as the mechanism. The H 2 O-PIII NiTi sample showed a higher breakdown potential (E b ) than the control sample. Based on the AFM results, two different physical models with related equivalent electrical circuits were obtained to fit the EIS data and explain the surface electrochemical behavior of NiTi in SBF. The simulation results demonstrate that the higher resistance of the oxide layer produced by H 2 O-PIII is primarily responsible for the improvement in the surface corrosion resistance

Electrochemical Properties of Alkanethiol Monolayers Adsorbed on Nanoporous Au Surfaces

International Nuclear Information System (INIS)

Chu, Yeon Yi; Seo, Bora; Kim, Jong Won

2010-01-01

We investigated the electrochemical properties of alkanethiol monolayers adsorbed on NPG surfaces by cyclic voltammetry and electrochemical impedance spectroscopy, and the results are compared to those on flat Au surfaces. The reductive desorption of alkanethiols on NPG surfaces is observed in more negative potential regions than that on flat Au surfaces due the stronger S-Au interaction on NPG surfaces. While the electron transfer through alkanethiol monolayers on flat Au surfaces occurs via a tunneling process through the monolayer films, the redox species can permeate through the monolayers on NPG surfaces to transfer the electrons to the Au surfaces. The results presented here will help to elucidate the intrinsic electrochemical properties of alkanethiol monolayers adsorbed on curved Au surfaces, particularly on the surface of AuNPs. Self-assembled monolayers (SAMs) of thiolate molecules on Au surfaces have been the subject of intensive research for the last few decades due to their unique physical and chemical properties. The well-organized surface structures of thiolate SAMs with various end-group functionalities can be further utilized for many applications in biology and nanotechnology. In addition to the practical applications, SAMs of thiolate molecules on Au surfaces also provide unique opportunities to address fundamental issues in surface chemistry such as self-organized surface structures, electron transfer behaviors, and moleculesubstrate interactions. Although there have been numerous reports on the fundamental physical and chemical properties of thiolate SAMs on Au surfaces, most of them were investigated on flat Au surfaces, typically on well-defined Au(111) surfaces

Nanotubular surface modification of metallic implants via electrochemical anodization technique.

Science.gov (United States)

Wang, Lu-Ning; Jin, Ming; Zheng, Yudong; Guan, Yueping; Lu, Xin; Luo, Jing-Li

2014-01-01

Due to increased awareness and interest in the biomedical implant field as a result of an aging population, research in the field of implantable devices has grown rapidly in the last few decades. Among the biomedical implants, metallic implant materials have been widely used to replace disordered bony tissues in orthopedic and orthodontic surgeries. The clinical success of implants is closely related to their early osseointegration (ie, the direct structural and functional connection between living bone and the surface of a load-bearing artificial implant), which relies heavily on the surface condition of the implant. Electrochemical techniques for modifying biomedical implants are relatively simple, cost-effective, and appropriate for implants with complex shapes. Recently, metal oxide nanotubular arrays via electrochemical anodization have become an attractive technique to build up on metallic implants to enhance the biocompatibility and bioactivity. This article will thoroughly review the relevance of electrochemical anodization techniques for the modification of metallic implant surfaces in nanoscale, and cover the electrochemical anodization techniques used in the development of the types of nanotubular/nanoporous modification achievable via electrochemical approaches, which hold tremendous potential for bio-implant applications. In vitro and in vivo studies using metallic oxide nanotubes are also presented, revealing the potential of nanotubes in biomedical applications. Finally, an outlook of future growth of research in metallic oxide nanotubular arrays is provided. This article will therefore provide researchers with an in-depth understanding of electrochemical anodization modification and provide guidance regarding the design and tuning of new materials to achieve a desired performance and reliable biocompatibility.

Reversible Compositional Control of Oxide Surfaces by Electrochemical Potentials

KAUST Repository

Mutoro, Eva

2012-01-05

Perovskite oxides can exhibit a wide range of interesting characteristics such as being catalytically active and electronically/ionically conducting, and thus, they have been used in a number of solid-state devices such as solid oxide fuel cells (SOFCs) and sensors. As the surface compositions of perovskites can greatly influence the catalytic properties, knowing and controlling their surface compositions is crucial to enhance device performance. In this study, we demonstrate that the surface strontium (Sr) and cobalt (Co) concentrations of perovskite-based thin films can be controlled reversibly at elevated temperatures by applying small electrical potential biases. The surface compositional changes of La 0.8Sr 0.2CoO 3-δ (LSC 113), (La 0.5Sr 0.5) 2CoO 4±δ (LSC 214), and LSC 214-decorated LSC 113 films (LSC 113/214) were investigated in situ by utilizing synchrotron-based X-ray photoelectron spectroscopy (XPS), where the largest changes of surface Sr were found for the LSC 113/214 surface. These findings offer the potential of reversibly controlling the surface functionality of perovskites. © 2011 American Chemical Society.

A mathematical model for surface roughness of fluidic channels produced by grinding aided electrochemical discharge machining (G-ECDM

Directory of Open Access Journals (Sweden)

Ladeesh V. G.

2017-01-01

Full Text Available Grinding aided electrochemical discharge machining is a hybrid technique, which combines the grinding action of an abrasive tool and thermal effects of electrochemical discharges to remove material from the workpiece for producing complex contours. The present study focuses on developing fluidic channels on borosilicate glass using G-ECDM and attempts to develop a mathematical model for surface roughness of the machined channel. Preliminary experiments are conducted to study the effect of machining parameters on surface roughness. Voltage, duty factor, frequency and tool feed rate are identified as the significant factors for controlling surface roughness of the channels produced by G-ECDM. A mathematical model was developed for surface roughness by considering the grinding action and thermal effects of electrochemical discharges in material removal. Experiments are conducted to validate the model and the results obtained are in good agreement with that predicted by the model.

MEMS-based dynamic cell-to-cell culture platforms using electrochemical surface modifications

International Nuclear Information System (INIS)

Chang, Jiyoung; Lin, Liwei; Yoon, Sang-Hee; Mofrad, Mohammad R K

2011-01-01

MEMS-based biological platforms with the capability of both spatial placements and time releases of living cells for cell-to-cell culture experiments have been designed and demonstrated utilizing electrochemical surface modification effects. The spatial placement is accomplished by electrochemical surface modification of substrate surfaces to be either adhesive or non-adhesive for living cells. The time control is achieved by the electrical activation of the selective indium tin oxide co-culture electrode to allow the migration of living cells onto the electrode to start the cell-to-cell culture studies. Prototype devices have a three-electrode design with an electrode size of 50 × 50 µm 2 and the separation gaps of 2 µm between them. An electrical voltage of −1.5 V has been used to activate the electrodes independently and sequentially to demonstrate the dynamic cell-to-cell culture experiments of NIH 3T3 fibroblast and Madin Darby canine kidney cells. As such, this MEMS platform could be a basic yet versatile tool to characterize transient cell-to-cell interactions

Unobstructed electron transfer on porous polyelectrolyte nanostructures and its characterization by electrochemical surface plasmon resonance

Energy Technology Data Exchange (ETDEWEB)

Davis, Bryce W.; Linman, Matthew J.; Linley, Kamara S.; Hare, Christopher D. [Department of Chemistry, University of California, Riverside, CA 92521 (United States); Cheng Quan, E-mail: quan.cheng@ucr.ed [Department of Chemistry, University of California, Riverside, CA 92521 (United States)

2010-06-01

Thin organic films with desirable redox properties have long been sought in biosensor research. We report here the development of a polymer thin film interface with well-defined hierarchical nanostructure and electrochemical behavior, and its characterization by electrochemical surface plasmon resonance (ESPR) spectroscopy. The nano-architecture build-up is monitored in real time with SPR, while the redox response is characterized by cyclic voltammetry in the same flow cell. The multilayer assembly is built on a self-assembled monolayer (SAM) of 1:1 (molar ratio) 11-ferrocenyl-1-undecanethiolate (FUT) and mercaptoundecanoic acid (MUA), and constructed using a layer-by-layer deposition of cationic poly(allylamine hydrochloride) (PAH) and anionic poly(sodium 4-styrenesulfonate) (PSS). Electron transfer (ET) on the mixed surface and the effect of the layer structures on ET are systematically studied. Under careful control, multiple layers can be deposited onto the 1:1 FUT/MUA SAM that presents unobstructed redox chemistry, indicating a highly ordered, extensively porous structure obtained under this condition. The use of SPR to trace the minute change during the electrochemical process offers neat characterization of local environment at the interface, in particular double layer region, allowing for better control over the redox functionality of the multilayers. The 1:1 SAM has a surface coverage of 4.1 +- 0.3 x 10{sup -10} mol cm{sup -2} for ferrocene molecules and demonstrates unperturbed electrochemistry activity even in the presence of a 13 nm polymer film adhered to the electrode surface. This thin layer possesses some desirable properties similar to those on a SAM while presenting approx15 nm exceedingly porous structure for high loading capacity. The high porosity allows perchlorate to freely partition into the film, leading to high current density that is useful for sensitive electrochemical measurements.

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-04-15

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

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.

Improved electrochemical properties of morphology-controlled titania/titanate nanostructures prepared by in-situ hydrothermal surface modification of self-source Ti substrate for high-performance supercapacitors.

Science.gov (United States)

Banerjee, Arghya Narayan; Anitha, V C; Joo, Sang W

2017-10-16

Ti substrate surface is modified into two-dimensional (2D) TiO 2 nanoplatelet or one-dimensional (1D) nanorod/nanofiber (or a mixture of both) structure in a controlled manner via a simple KOH-based hydrothermal technique. Depending on the KOH concentration, different types of TiO 2 nanostructures (2D platelets, 1D nanorods/nanofibers and a 2D+1D mixed sample) are fabricated directly onto the Ti substrate surface. The novelty of this technique is the in-situ modification of the self-source Ti surface into titania nanostructures, and its direct use as the electrochemical microelectrode without any modifications. This leads to considerable improvement in the interfacial properties between metallic Ti and semiconducting TiO 2 . Since interfacial states/defects have profound effect on charge transport properties of electronic/electrochemical devices, therefore this near-defect-free interfacial property of Ti-TiO 2 microelectrode has shown high supercapacitive performances for superior charge-storage devices. Additionally, by hydrothermally tuning the morphology of titania nanostructures, the electrochemical properties of the electrodes are also tuned. A Ti-TiO 2 electrode comprising of a mixture of 2D-platelet+1D-nanorod structure reveals very high specific capacitance values (~7.4 mF.cm -2 ) due to the unique mixed morphology which manifests higher active sites (hence, higher utilization of the active materials) in terms of greater roughness at the 2D-platelet structures and higher surface-to-volume-ratio in the 1D-nanorod structures.

Controllable Electrochemical Activities by Oxidative Treatment toward Inner-Sphere Redox Systems at N-Doped Hydrogenated Amorphous Carbon Films

Directory of Open Access Journals (Sweden)

Yoriko Tanaka

2012-01-01

Full Text Available The electrochemical activity of the surface of Nitrogen-doped hydrogenated amorphous carbon thin films (a-CNH, N-doped DLC toward the inner sphere redox species is controllable by modifying the surface termination. At the oxygen plasma treated N-doped DLC surface (O-DLC, the surface functional groups containing carbon doubly bonded to oxygen (C=O, which improves adsorption of polar molecules, were generated. By oxidative treatment, the electron-transfer rate for dopamine (DA positively charged inner-sphere redox analyte could be improved at the N-doped DLC surface. For redox reaction of 2,4-dichlorophenol, which induces an inevitable fouling of the anode surface by forming passivating films, the DLC surfaces exhibited remarkably higher stability and reproducibility of the electrode performance. This is due to the electrochemical decomposition of the passive films without the interference of oxygen evolution by applying higher potential. The N-doped DLC film can offer benefits as the polarizable electrode surface with the higher reactivity and higher stability toward inner-sphere redox species. By making use of these controllable electrochemical reactivity at the O-DLC surface, the selective detection of DA in the mixed solution of DA and uric acid could be achieved.

Electrochemical Properties of High Surface Area Vanadium Oxide Aerogels

National Research Council Canada - National Science Library

Dong, Winny

2001-01-01

.... Traditional composite electrode structures have prevented truly quantitative analysis of surface area effects in nanoscale battery materials, as well as a study of their innate electrochemical behavior...

Surface and electrochemical characterization of electrodeposited PtRu alloys

Science.gov (United States)

Richarz, Frank; Wohlmann, Bernd; Vogel, Ulrich; Hoffschulz, Henning; Wandelt, Klaus

1995-07-01

PtRu alloys of different compositions were electrodeposited on Au. Twelve alloys between 0% and 100% Pt were characterized with surface sensitive spectroscopies (XPS, LEIS) after transfer from an electrochemical cell to an ultra high vaccum chamber without contact to air. The composition of the thus prepared alloys showed a linear dependence on the concentrations of the deposition solution, but was Pt-enriched both in the bulk and (even more so) at the surface. During the electrochemical reduction of the metal cations, sulfur from the supporting electrolyte 1N H 2SO 4 was found to be incorporated into the electrodes. Cyclic voltammetry was used for the determination of the electrocatalytic activity of the electrodes for the oxidation of carbon monoxide. The highest activity for this oxidation as measured by the (peak) potential of the CO oxidation cyclovoltammograms was found for a surface concentration of ˜ 50%Pt. The asymmetry of this "activity curve" (oxidation potential versus Pt surface concentration) is tentatively explained in terms of a surface structural phase separation.

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

Science.gov (United States)

Sulyma, Christopher Michael

structures. The surface reactions that form the basis of this CMP strategy are investigated here in detail using the electrochemical techniques of cyclic voltammetry, open circuit potential analysis, polarization resistance measurements, and Fourier transform impedance spectroscopy. The results suggest that forming structurally weak oxide layers on the CMP samples is a key to achieving the goal of chemically controlled CMP of Ta/TaN at low down-pressures. (Abstract shortened by UMI.)

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

Lubricant-impregnated surfaces for electrochemical applications, and devices and systems using same

Energy Technology Data Exchange (ETDEWEB)

Solomon, Brian Richmond; Chen, Xinwei; Chiang, Yet-Ming; Varanasi, Kripa K.

2018-04-17

In certain embodiments, the invention relates to an electrochemical device having a liquid lubricant impregnated surface. At least a portion of the interior surface of the electrochemical device includes a portion that includes a plurality of solid features disposed therein. The plurality of solid features define a plurality of regions therebetween. A lubricant is disposed in the plurality of regions which retain the liquid lubricant in the plurality of regions during operation of the device. An electroactive phase comes in contact with at least the portion of the interior surface. The liquid lubricant impregnated surface introduces a slip at the surface when the electroactive phase flows along the surface. The electroactive phase may be a yield stress fluid.

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...

Effect of electrochemical treatments on the surface chemistry of activated carbon

OpenAIRE

Berenguer Betrián, Raúl; Marco Lozar, Juan Pablo; Quijada Tomás, César; Cazorla Amorós, Diego; Morallón Núñez, Emilia

2008-01-01

The effect of the electrochemical treatment (galvanostatic electrolysis in a filter-press electrochemical cell) on the surface chemistry and porous structure of a granular activated carbon (GAC) has been analyzed by means of temperature-programmed desorption and N2 (at 77 K) and CO2 (at 273 K) adsorption isotherms. The anodic and cathodic treatments, the applied current (between 0.2 and 2.0 A) and the type of electrolyte (NaOH, H2SO4 and NaCl)have been studied as electrochemical variables. Bo...

Experimental approach to controllably vary protein oxidation while minimizing electrode adsorption for boron-doped diamond electrochemical surface mapping applications.

Science.gov (United States)

McClintock, Carlee S; Hettich, Robert L

2013-01-02

Oxidative protein surface mapping has become a powerful approach for measuring the solvent accessibility of folded protein structures. A variety of techniques exist for generating the key reagent (i.e., hydroxyl radicals) for these measurements; however, these approaches range significantly in their complexity and expense of operation. This research expands upon earlier work to enhance the controllability of boron-doped diamond (BDD) electrochemistry as an easily accessible tool for producing hydroxyl radicals in order to oxidize a range of intact proteins. Efforts to modulate the oxidation level while minimizing the adsorption of protein to the electrode involved the use of relatively high flow rates to reduce protein residence time inside the electrochemical flow chamber. Additionally, a different cell activation approach using variable voltage to supply a controlled current allowed us to precisely tune the extent of oxidation in a protein-dependent manner. In order to gain perspective on the level of protein adsorption onto the electrode surface, studies were conducted to monitor protein concentration during electrolysis and gauge changes in the electrode surface between cell activation events. This report demonstrates the successful use of BDD electrochemistry for greater precision in generating a target number of oxidation events upon intact proteins.

Surface Modification of MXenes: A Pathway to Improve MXene Electrode Performance in Electrochemical Energy Storage Devices

KAUST Repository

Ahmed, Bilal

2017-12-31

The recent discovery of layered transition metal carbides (MXenes) is one of the most important developments in two-dimensional (2D) materials. Preliminary theoretical and experimental studies suggest a wide range of potential applications for MXenes. The MXenes are prepared by chemically etching ‘A’-layer element from layered ternary metal carbides, nitrides and carbonitrides (MAX phases) through aqueous acid treatment, which results in various surface terminations such as hydroxyl, oxygen or fluorine. It has been found that surface terminations play a critical role in defining MXene properties and affects MXene performance in different applications such as electrochemical energy storage, electromagnetic interference shielding, water purification, sensors and catalysis. Also, the electronic, thermoelectric, structural, plasmonic and optical properties of MXenes largely depend upon surface terminations. Thus, controlling the surface chemistry if MXenes can be an efficient way to improve their properties. This research mainly aims to perform surface modifications of two commonly studied MXenes; Ti2C and Ti3C2, via chemical, thermal or physical processes to enhance electrochemical energy storage properties. The as-prepared and surface modified MXenes have been studied as electrode materials in Li-ion batteries (LIBs) and supercapacitors (SCs). In pursuit of desirable MXene surface, we have developed an in-situ room temperature oxidation process, which resulted in TiO2/MXene nanocomposite and enhanced Li-ion storage. The idea of making metal oxide and MXene nanocomposites was taken to the next level by combining a high capacity anode materials – SnO2 – and MXene. By taking advantage of already existing surface functional groups (–OH), we have developed a composite of SnO2/MXene by atomic layer deposition (ALD) which showed enhanced capacity and excellent cyclic stability. Thermal annealing of MXene at elevated temperature under different atmospheres was

Electrochemical decontamination of metallic surfaces by means of a movable electrode

International Nuclear Information System (INIS)

Mihai, F.; Nicu, M.; Cazan, L.; Turcanu, C.

1998-01-01

Electrochemical decontamination can be considered to be a decontamination assisted by an electrochemical field. The method is applied to the metallic surface decontamination for contaminants of any physico-chemical nature. The physico-chemical phenomenon that is the basis for the electrochemical methods is the anodic layer dissolution. By dissolution of the superficial layer any radioactive contaminant on the surface or entrapped within the surface oxide is eliminated. Electrochemical decontamination, also known as electropolishing, involves the use of the object to be cleaned as an anode in an electrochemical cell. The passage of current results in anodic dissolution of the surface material. Generally, there are many methods of application for electropolishing. The most common method is immersing the object to be decontaminated in a tank filled with a suitable electrolyte. The electrochemical method with movable electrode involves the use of 'in situ' mobile devices that are able to electropolish punctual surfaces in places difficult to access. The advantages are the simplicity of the setup, short times of application and reduced waste volumes. Phosphoric and sulphuric acid mixture is used as the electrolyte in electropolishing because of its stability, safety and applicability to a variety of alloy systems. The method was applied to decontaminate carbon steel, aluminium and copper. Used contaminants are mixtures of 60 Co and 134 Cs; 60 Co and 65 Zn; 60 Co, 65 Zn and 134 Cs. After preparation, the samples were kept in laboratory conditions about one month, to simulate real conditions and to let the chemical reactions between contaminant and sample material constitution to complete. To calculate decontamination factor characteristic for each studied decontamination method the following radiometric measurements are necessary: - activity measurement after radioisotope solution contamination representing initial activity Λ in ; - activity measurement after

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.

Effects of Nanowire Length and Surface Roughness on the Electrochemical Sensor Properties of Nafion-Free, Vertically Aligned Pt Nanowire Array Electrodes

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Zhiyang Li

2015-09-01

Full Text Available In this paper, vertically aligned Pt nanowire arrays (PtNWA with different lengths and surface roughnesses were fabricated and their electrochemical performance toward hydrogen peroxide (H2O2 detection was studied. The nanowire arrays were synthesized by electroplating Pt in nanopores of anodic aluminum oxide (AAO template. Different parameters, such as current density and deposition time, were precisely controlled to synthesize nanowires with different surface roughnesses and various lengths from 3 μm to 12 μm. The PtNWA electrodes showed better performance than the conventional electrodes modified by Pt nanowires randomly dispersed on the electrode surface. The results indicate that both the length and surface roughness can affect the sensing performance of vertically aligned Pt nanowire array electrodes. Generally, longer nanowires with rougher surfaces showed better electrochemical sensing performance. The 12 μm rough surface PtNWA presented the largest sensitivity (654 μA·mM−1·cm−2 among all the nanowires studied, and showed a limit of detection of 2.4 μM. The 12 μm rough surface PtNWA electrode also showed good anti-interference property from chemicals that are typically present in the biological samples such as ascorbic, uric acid, citric acid, and glucose. The sensing performance in real samples (river water was tested and good recovery was observed. These Nafion-free, vertically aligned Pt nanowires with surface roughness control show great promise as versatile electrochemical sensors and biosensors.

Electro-chemical grinding

Science.gov (United States)

Feagans, P. L.

1972-01-01

Electro-chemical grinding technique has rotation speed control, constant feed rates, and contour control. Hypersonic engine parts of nickel alloys can be almost 100% machined, keeping tool pressure at virtual zero. Technique eliminates galling and permits constant surface finish and burr-free interrupted cutting.

Spatial and temporal control of the diazonium modification of sp2 carbon surfaces.

Science.gov (United States)

Kirkman, Paul M; Güell, Aleix G; Cuharuc, Anatolii S; Unwin, Patrick R

2014-01-08

Interest in the controlled chemical functionalization of sp(2) carbon materials using diazonium compounds has been recently reignited, particularly as a means to generate a band gap in graphene. We demonstrate local diazonium modification of pristine sp(2) carbon surfaces, with high control, at the micrometer scale through the use of scanning electrochemical cell microscopy (SECCM). Electrochemically driven diazonium patterning is investigated at a range of driving forces, coupled with surface analysis using atomic force microscopy (AFM) and Raman spectroscopy. We highlight how the film density, level of sp(2)/sp(3) rehybridization and the extent of multilayer formation can be controlled, paving the way for the use of localized electrochemistry as a route to controlled diazonium modification.

Pullulan as a potent green inhibitor for corrosion mitigation of aluminum composite: Electrochemical and surface studies.

Science.gov (United States)

B P, Charitha; Rao, Padmalatha

2018-06-01

This work emphasizes the corrosion inhibition ability of pullulan, an environmentally benign fungal polysaccharide on acid corrosion of 6061Aluminum-15% (v) SiC (P) composite material (Al-CM). The electrochemical measurements such as potentiodynamic polarization (PDP) and electrochemical impedance spectroscopy (EIS) studies were carried out for the corrosion inhibition studies. Conditions were optimized to obtain maximum inhibition efficiency, by performing the experiment at varying concentrations of inhibitor, in the temperature range of 308K- 323K. Surface morphology studies were done to reaffirm the adsorption of inhibitor on the surface of composite material. Pullulan acted as mixed type of inhibitor with a maximum efficiency of 89% at 303K for the addition of 1.0 gL -1 of inhibitor. Evaluation of kinetic and thermodynamic parameters revealed that inhibitor underwent physical adsorption onto the surface of Al-CM and obeyed Freundlich adsorption isotherm. The surface characterization like SEM-EDX, AFM confirmed the adsorption of pullulan molecule. Pullulan can be considered as effective, eco friendly green inhibitor for the corrosion control of Al-CM. Copyright © 2018 Elsevier B.V. All rights reserved.

An Experimental Approach to Controllably Vary Protein Oxidation While Minimizing Electrode Adsorption for Boron-Doped Diamond Electrochemical Surface Mapping Applications

Science.gov (United States)

McClintock, Carlee S; Hettich, Robert L.

2012-01-01

Oxidative protein surface mapping has become a powerful approach for measuring the solvent accessibility of folded protein structures. A variety of techniques exist for generating the key reagent – hydroxyl radicals – for these measurements; however, these approaches range significantly in their complexity and expense of operation. This research expands upon earlier work to enhance the controllability of boron-doped diamond (BDD) electrochemistry as an easily accessible tool for producing hydroxyl radicals in order to oxidize a range of intact proteins. Efforts to modulate oxidation level while minimizing the adsorption of protein to the electrode involved the use of relatively high flow rates to reduce protein residence time inside the electrochemical flow chamber. Additionally, a different cell activation approach using variable voltage to supply a controlled current allowed us to precisely tune the extent of oxidation in a protein-dependent manner. In order to gain perspective on the level of protein adsorption onto the electrode surface, studies were conducted to monitor protein concentration during electrolysis and gauge changes in the electrode surface between cell activation events. This report demonstrates the successful use of BDD electrochemistry for greater precision in generating a target number of oxidation events upon intact proteins. PMID:23210708

Electrochemical capacitor

Science.gov (United States)

Anderson, Marc A.; Liu, Kuo -Chuan; Mohr, Charles M.

1999-10-05

An inexpensive porous metal oxide material having high surface area, good conductivity and high specific capacitance is advantageously used in an electrochemical capacitor. The materials are formed in a sol-gel process which affords control over the properties of the resultant metal oxide materials.

Facile preparation of self-healing superhydrophobic CeO2 surface by electrochemical processes

Science.gov (United States)

Nakayama, Katsutoshi; Hiraga, Takuya; Zhu, Chunyu; Tsuji, Etsushi; Aoki, Yoshitaka; Habazaki, Hiroki

2017-11-01

Herein we report simple electrochemical processes to fabricate a self-healing superhydrophobic CeO2 coating on Type 304 stainless steel. The CeO2 surface anodically deposited on flat stainless steel surface is hydrophilic, although high temperature-sintered and sputter-deposited CeO2 surface was reported to be hydrophobic. The anodically deposited hydrophilic CeO2 surface is transformed to hydrophobic during air exposure. Specific accumulation of contaminant hydrocarbon on the CeO2 surface is responsible for the transformation to hydrophobic state. The deposition of CeO2 on hierarchically rough stainless steel surface produces superhydrophobic CeO2 surface, which also shows self-healing ability; the surface changes to superhydrophilic after oxygen plasma treatment but superhydrophobic state is recovered repeatedly by air exposure. This work provides a facile method for preparing a self-healing superhydrophobic surface using practical electrochemical processes.

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

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Jesús González-Cobos

2016-01-01

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

Electrochemical surface plasmon resonance sensor based on two-electrode configuration

International Nuclear Information System (INIS)

Zhang, Bing; Dong, Wei; Wen, Yizhang; Pang, Kai; Wang, Xiaoping; Li, Yazhuo; Zhan, Shuyue

2016-01-01

To obtain detailed information about electrochemistry reactions, a two-electrode electrochemical surface plasmon resonance (EC-SPR) sensor has been proposed. We describe the theory of potential modulation for this novel sensor and determine the factors that can change the SPR resonance angle. The reference electrode in three-electrode configuration was eliminated, and comparing with several other electrode materials, activated carbon (AC) is employed as the suitable counter electrode for its potential stability. Just like three-electrode configuration, the simpler AC two-electrode system can also obtain detailed information about the electrochemical reactions. (paper)

Controllably annealed CuO-nanoparticle modified ITO electrodes: Characterisation and electrochemical studies

Energy Technology Data Exchange (ETDEWEB)

Wang, Tong; Su, Wen; Fu, Yingyi [College of Chemistry, Beijing Normal University, Beijing 100875 (China); Hu, Jingbo, E-mail: hujingbo@bnu.edu.cn [College of Chemistry, Beijing Normal University, Beijing 100875 (China); Key Laboratory of Beam Technology and Material Modification of Ministry of Education, Beijing Normal University, Beijing 100875 (China)

2016-12-30

Graphical abstract: We report a simple and controllable synthesis of CuO-nanoparticle-modified ITO by employing a combination of ion-implantation and annealing methods for the first time. The optimum CuO/ITO electrode shows uniform morphology, highly accessible surface area, long-term stability and excellent electrochemical performance towards biomolecules such as glucose in alkaline solution. - Highlights: • Controllably annealed CuO/ITO electrode was synthesized for the first time. • The generation mechanism of CuO nanoparticles is revealed. • The optimum CuO/ITO electrode shows excellent electrochemical performance. • A reference for the controllable preparation of other metal oxide nanoparticles. - Abstract: In this paper, we report a facile and controllable two-step approach to produce indium tin oxide electrodes modified by copper(II) oxide nanoparticles (CuO/ITO) through ion implantation and annealing methods. After annealing treatment, the surface morphology of the CuO/ITO substrate changed remarkably and exhibited highly electroactive sites and a high specific surface area. The effects of annealing treatment on the synthesis of CuO/ITO were discussed based on various instruments’ characterisations, and the possible mechanism by which CuO nanoparticles were generated was also proposed in this work. Cyclic voltammetric results indicated that CuO/ITO electrodes exhibited effective catalytic responses toward glucose in alkaline solution. Under optimal experimental conditions, the proposed CuO/ITO electrode showed sensitivity of 450.2 μA cm{sup −2} mM{sup −1} with a linear range of up to ∼4.4 mM and a detection limit of 0.7 μM (S/N = 3). Moreover, CuO/ITO exhibited good poison resistance, reproducibility, and stability properties.

High-capacity conductive nanocellulose paper sheets for electrochemically controlled extraction of DNA oligomers.

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Aamir Razaq

Full Text Available Highly porous polypyrrole (PPy-nanocellulose paper sheets have been evaluated as inexpensive and disposable electrochemically controlled three-dimensional solid phase extraction materials. The composites, which had a total anion exchange capacity of about 1.1 mol kg(-1, were used for extraction and subsequent release of negatively charged fluorophore tagged DNA oligomers via galvanostatic oxidation and reduction of a 30-50 nm conformal PPy layer on the cellulose substrate. The ion exchange capacity, which was, at least, two orders of magnitude higher than those previously reached in electrochemically controlled extraction, originated from the high surface area (i.e. 80 m(2 g(-1 of the porous composites and the thin PPy layer which ensured excellent access to the ion exchange material. This enabled the extractions to be carried out faster and with better control of the PPy charge than with previously employed approaches. Experiments in equimolar mixtures of (dT(6, (dT(20, and (dT(40 DNA oligomers showed that all oligomers could be extracted, and that the smallest oligomer was preferentially released with an efficiency of up to 40% during the reduction of the PPy layer. These results indicate that the present material is very promising for the development of inexpensive and efficient electrochemically controlled ion-exchange membranes for batch-wise extraction of biomolecules.

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.

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

Energy Technology Data Exchange (ETDEWEB)

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

2008-09-07

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

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.

Polystyrene sphere monolayer assisted electrochemical deposition of ZnO nanorods with controlable surface density

Energy Technology Data Exchange (ETDEWEB)

Ramirez, D., E-mail: daniel.ramirez@ucv.c [Laboratorio de Electroquimica, Pontificia Universidad Catolica de Valparaiso, Valparaiso (Chile); Gomez, H. [Laboratorio de Electroquimica, Pontificia Universidad Catolica de Valparaiso, Valparaiso (Chile); Lincot, D. [Institute de Recherche et Developpement sur l' Energie Photovoltaique-IRDEP, 6 Quai Watier 78401, Chatou Cedex (France)

2010-02-15

In this paper we report the zinc oxide nanorods (ZnO NRs) growth by electrochemical deposition onto polycrystalline gold electrodes modified with assemblies of polystyrene sphere monolayers (PSSMs). Growth occurs through the interstitial spaces between the hexagonally close packed spheres. ZnO NRs nucleate in the region where three adjacent spheres leave a space, being able to grow and projected over the PSSMs. The nanorod surface density (N{sub NR}) shows a linear dependence with respect to a PS sphere diameter selected. XRD analysis shows these ZnO NRs are highly oriented along the (0 0 2) plane (c-axis). This open the possibility to have electronic devices with mechanically supported nanometric materials.

The role of surface defects in HOPG on the electrochemical and physical deposition of Ag

Directory of Open Access Journals (Sweden)

R. PETROVIC

1999-08-01

Full Text Available The role of defects on a substrate surface during the initial stages of nucleation and growth of Ag deposited electrochemically and physically on highly oriented pyrolytic graphite (HOPG has been observed ex situ by scanning tunneling microscopy (STM. The silver was electrodeposited under current controlled electrochemical conditions at 26 µA/cm2, which corresponded to a deposition rate of 0.1 monolayers (ML per second. For comparison, physical deposition of Ag on HOPG was performed by DC Ar+ ion sputtering, at the same deposition rate and for the same deposition times. In both cases, Ag grows in an island growth mode, but the distribution of the islands appears to be quite different. In physical deposition, the Ag islands are almost homogeneously distributed over the substrate surface and a slight accumulation of islands on steps does not contribute significantly to the overall morphology. This indicates the crucial role of point defects on the substrate in the initial stages of nucleation. In electrochemical deposition, more lined defects are observed after a flow of current, and their role in the beginning of the nucleation is more pronounced. Lined defects are responsible for the string-like shaped domains of deposited atoms. Also, the existence of string-like shaped nucleation exclusion zones is indicated. The problem of the formation of nucleation exclusion zones, which appear only in electrochemical deposition, has been reconsidered and a new explanaton of their formation is given. A mathematical model for the calculation of the radius of the nucleation exclusion zone has been developed.

Nanostructured surfaces for analysis of anticancer drug and cell diagnosis based on electrochemical and SERS tools

Science.gov (United States)

El-Said, Waleed A.; Yoon, Jinho; Choi, Jeong-Woo

2018-04-01

Discovering new anticancer drugs and screening their efficacy requires a huge amount of resources and time-consuming processes. The development of fast, sensitive, and nondestructive methods for the in vitro and in vivo detection of anticancer drugs' effects and action mechanisms have been done to reduce the time and resources required to discover new anticancer drugs. For the in vitro and in vivo detection of the efficiency, distribution, and action mechanism of anticancer drugs, the applications of electrochemical techniques such as electrochemical cell chips and optical techniques such as surface-enhanced Raman spectroscopy (SERS) have been developed based on the nanostructured surface. Research focused on electrochemical cell chips and the SERS technique have been reviewed here; electrochemical cell chips based on nanostructured surfaces have been developed for the in vitro detection of cell viability and the evaluation of the effects of anticancer drugs, which showed the high capability to evaluate the cytotoxic effects of several chemicals at low concentrations. SERS technique based on the nanostructured surface have been used as label-free, simple, and nondestructive techniques for the in vitro and in vivo monitoring of the distribution, mechanism, and metabolism of different anticancer drugs at the cellular level. The use of electrochemical cell chips and the SERS technique based on the nanostructured surface should be good tools to detect the effects and action mechanisms of anticancer drugs.

Electrochemical surface nitriding of pure iron by molten salt electrochemical process

Energy Technology Data Exchange (ETDEWEB)

Tsujimura, Hiroyuki; Goto, Takuya; Ito, Yasuhiko

2004-08-11

Electrochemical surface nitriding of pure iron was investigated in molten LiCl-KCl-Li{sub 3}N systems at 773 K. An outer compound layer and an inner diffusion layer were obtained by means of potentiostatic electrolysis at 1.00 V (versus Li{sup +}/Li). From XRD and SEM analyses, it was confirmed that the obtained compound layer consisted of {epsilon}-Fe{sub 2-3}N and {gamma}'-Fe{sub 4}N; the free energies of formation of the two nitrides are positive and the equilibrium nitrogen partial pressure of those are of the order of 10{sup 4} atm at 773 K. This result suggests that an apparent nitrogen partial pressure of at least the order of 10{sup 4} atm was imposed by the adsorbed nitrogen atoms (N{sub ads}) formed by anodic oxidation of nitride ion (N{sup 3-}) at the iron electrode surface.

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

Macro-mechanics controls quantum mechanics: mechanically controllable quantum conductance switching of an electrochemically fabricated atomic-scale point contact.

Science.gov (United States)

Staiger, Torben; Wertz, Florian; Xie, Fangqing; Heinze, Marcel; Schmieder, Philipp; Lutzweiler, Christian; Schimmel, Thomas

2018-01-12

Here, we present a silver atomic-scale device fabricated and operated by a combined technique of electrochemical control (EC) and mechanically controllable break junction (MCBJ). With this EC-MCBJ technique, we can perform mechanically controllable bistable quantum conductance switching of a silver quantum point contact (QPC) in an electrochemical environment at room temperature. Furthermore, the silver QPC of the device can be controlled both mechanically and electrochemically, and the operating mode can be changed from 'electrochemical' to 'mechanical', which expands the operating mode for controlling QPCs. These experimental results offer the perspective that a silver QPC may be used as a contact for a nanoelectromechanical relay.

Diamond surface functionalization with biomimicry - Amine surface tether and thiol moiety for electrochemical sensors

Science.gov (United States)

Sund, James B.; Causey, Corey P.; Wolter, Scott D.; Parker, Charles B.; Stoner, Brian R.; Toone, Eric J.; Glass, Jeffrey T.

2014-05-01

The surface of conducting diamond was functionalized with a terminal thiol group that is capable of binding and detecting nitrogen-oxygen species. The functionalization process employed multiple steps starting with doped diamond films grown by plasma enhanced chemical vapor deposition followed by hydrogen termination and photochemical attachment of a chemically protected amine alkene. The surface tether was deprotected to reveal the amine functionality, which enabled the tether to be extended with surface chemistry to add a terminal thiol moiety for electrochemical sensing applications. Each step of the process was validated using X-ray photoelectron spectroscopy analysis.

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.

TXRF study of electrochemical deposition of metals on glass-ceramic carbon electrode surfaces

International Nuclear Information System (INIS)

Alov, N.; Oskolok, K.; Wittershagen, A.; Mertens, M.; Rittmeyer, C.; Kolbesen, B.O.

2000-01-01

Nowadays the methods of solid surface analysis are widely used to study the thermodynamic and kinetic aspects of joint electrochemical deposition of metals on solid substrates. In this work the surfaces of some binary and ternary metal electrodeposits on disc glass-ceramic carbon electrodes were studied by total-reflection x-ray fluorescence spectroscopy (TXRF). Metal alloys were obtained as a result of electrochemical co-deposition of copper, cadmium and lead from n x 10 -4 M (Cu, Cd, Pb)(NO 3 ) 2 + 0.01 M HNO 3 solutions under mixing. TXRF measurements were performed with an ATOMIKA EXTRA II A spectrometer using Mo K α and W (Brems) primary excitation. The serious advantage of TXRF as a method of near-surface analysis is very high element sensitivity. Apart from main elements (Cu, Cd, Pb) we have detected trace elements (Cl, Ag, Pt, Hg) which are present in working solution and has an effect to the electrodeposit formation. The comparison of TXRF data with information obtained by X-ray photoelectron spectroscopy and electron-probe x-ray microanalysis permits to realize depth profiling electrochemical alloys. In particular it was found that in binary systems Cu-Pb and Cu-Cd the relative lead and cadmium content on the electrodeposit surface is considerably greater than in the bulk. These phenomena are due to the features of metal nucleation and growth mechanisms. High sensitivity of TXRF to surface morphology and the correlation of TXRF and scanning electron microscopy data allow to determine the area of prevailing location of metal in the heterogeneous alloy surface. So we have established that in Cu-Pb and Cu-Cd-Pb systems solid solution of copper and lead is formed: significant part of lead is deposited not only in specific 3D-clusters but also in copper thin film. It was demonstrated that the near-surface TXRF analysis of metal electrodeposits on solid electrodes is highly effective to study the mechanisms of metal nucleation, metal cluster and thin film

Layered Metal Nanoparticle Structures on Electrodes for Sensing, Switchable Controlled Uptake/Release, and Photo-electrochemical Applications.

Science.gov (United States)

Tel-Vered, Ran; Kahn, Jason S; Willner, Itamar

2016-01-06

Layered metal nanoparticle (NP) assemblies provide highly porous and conductive composites of unique electrical and optical (plasmonic) properties. Two methods to construct layered metal NP matrices are described, and these include the layer-by-layer deposition of NPs, or the electropolymerization of monolayer-functionalized NPs, specifically thioaniline-modified metal NPs. The layered NP composites are used as sensing matrices through the use of electrochemistry or surface plasmon resonance (SPR) as transduction signals. The crosslinking of the metal NP composites with molecular receptors, or the imprinting of molecular recognition sites into the electropolymerized NP matrices lead to selective and chiroselective sensing interfaces. Furthermore, the electrosynthesis of redox-active, imprinted, bis-aniline bridged Au NP composites yields electrochemically triggered "sponges" for the switchable uptake and release of electron-acceptor substrates, and results in conductive surfaces of electrochemically controlled wettability. Also, photosensitizer-relay-crosslinked Au NP composites, or electrochemically polymerized layered semiconductor quantum dot/metal NP matrices on electrodes, are demonstrated as functional nanostructures for photoelectrochemical applications. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Cold pressure welding of aluminium-steel blanks: Manufacturing process and electrochemical surface preparation

Science.gov (United States)

Schmidt, Hans Christian; Homberg, Werner; Orive, Alejandro Gonzalez; Grundmeier, Guido; Hordych, Illia; Maier, Hans Jürgen

2018-05-01

In this study the manufacture of aluminium-steel blanks by cold pressure welding and their preparation for a welding process through electrochemical surface treatment are investigated and discussed. The cold pressure welding process was done with an incremental rolling tool that allows for the partial pressure welding of two blanks along a prepared path. The influence of the surface preparation by electrochemical deposition of bond promoting organosilane-based agents and roughening on a nano-scale is investigated and compared to conventional surface treatments. Coating the surfaces with a thin organosilane-based film incorporating specific functional groups should promote additional bonding between the mating oxide layers; its influence on the total weld strength is studied. Pressure welding requires suitable process strategies, and the current advances in the proposed incremental rolling process for the combination of mild steel and aluminium are presented.

Constructing Functional Ionic Membrane Surface by Electrochemically Mediated Atom Transfer Radical Polymerization

Directory of Open Access Journals (Sweden)

Fen Ran

2016-01-01

Full Text Available The sodium polyacrylate (PAANa contained polyethersulfone membrane that was fabricated by preparation of PES-NH2 via nonsolvent phase separation method, the introduction of bromine groups as active sites by grafting α-Bromoisobutyryl bromide, and surface-initiated electrochemically atom transfer radical polymerization (SI-eATRP of sodium acrylate (AANa on the surface of PES membrane. The polymerization could be controlled by reaction condition, such as monomer concentration, electric potential, polymerization time, and modifier concentration. The membrane surface was uniform when the monomer concentration was 0.9 mol/L, the electric potential was −0.12 V, the polymerization time was 8 h, and the modifier concentration was 2 wt.%. The membrane showed excellent hydrophilicity and blood compatibility. The water contact angle decreased from 84° to 68° and activated partial thromboplastin increased from 51 s to 84 s after modification of the membranes.

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).

Development of graphene oxide/poly(3,4-ethylenedioxythiophene)/poly(styrene sulfonate) thin film-based electrochemical surface plasmon resonance immunosensor for detection of human immunoglobulin G

Science.gov (United States)

Pothipor, Chammari; Lertvachirapaiboon, Chutiparn; Shinbo, Kazunari; Kato, Keizo; Kaneko, Futao; Ounnunkad, Kontad; Baba, Akira

2018-02-01

An electrochemically synthesized graphene oxide (GO)/poly(3,4-ethylenedioxythiophene) (PEDOT)/poly(styrene sulfonate) (PSS) thin film-based electrochemical surface plasmon resonance (EC-SPR) sensor chip was developed and employed for the detection of human immunoglobulin G (IgG). GO introduced the carboxylic group on the film surface, which also allowed electrochemical control, for the immobilization of the anti-IgG antibody via covalent bonding through amide coupling reaction. The SPR sensitivity of the detection was improved under the control by applying an electrochemical potential, by which the sensitivity was increased by the increment in applied potential. Among the open-circuit and different applied potentials in the range of -1.0 to 0.50 V, the EC-SPR immunosensor at an applied potential of 0.50 V exhibited the highest sensitivity of 6.08 × 10-3 mL µg-1 cm-2 and linearity in the human IgG concentration range of 1.0 to 10 µg mL-1 with a relatively low detection limit of 0.35 µg mL-1. The proposed sensor chip is promising for immunosensing at the physiological level.

Switching Transient Generation in Surface Interrogation Scanning Electrochemical Microscopy and Time-of-Flight Techniques.

Science.gov (United States)

Ahn, Hyun S; Bard, Allen J

2015-12-15

In surface interrogation scanning electrochemical microscopy (SI-SECM), fine and accurate control of the delay time between substrate generation and tip interrogation (tdelay) is crucial because tdelay defines the decay time of the reactive intermediate. In previous applications of the SI-SECM, the resolution in the control of tdelay has been limited to several hundreds of milliseconds due to the slow switching of the bipotentiostat. In this work, we have improved the time resolution of tdelay control up to ca. 1 μs, enhancing the SI-SECM to be competitive in the time domain with the decay of many reactive intermediates. The rapid switching SI-SECM has been implemented in a substrate generation-tip collection time-of-flight (SG-TC TOF) experiment of a solution redox mediator, and the results obtained from the experiment exhibited good agreement with that obtained from digital simulation. The reaction rate constant of surface Co(IV) on oxygen-evolving catalyst film, which was inaccessible thus far due to the lack of tdelay control, has been measured by the rapid switching SI-SECM.

Control oriented 1D electrochemical model of lithium ion battery

International Nuclear Information System (INIS)

Smith, Kandler A.; Rahn, Christopher D.; Wang, Chao-Yang

2007-01-01

Lithium ion (Li-ion) batteries provide high energy and power density energy storage for diverse applications ranging from cell phones to hybrid electric vehicles (HEVs). For efficient and reliable systems integration, low order dynamic battery models are needed. This paper introduces a general method to generate numerically a fully observable/controllable state variable model from electrochemical kinetic, species and charge partial differential equations that govern the discharge/charge behavior of a Li-ion battery. Validated against a 313th order nonlinear CFD model of a 6 Ah HEV cell, a 12th order state variable model predicts terminal voltage to within 1% for pulse and constant current profiles at rates up to 50 C. The state equation is constructed in modal form with constant negative real eigenvalues distributed in frequency space from 0 to 10 Hz. Open circuit potential, electrode surface concentration/reaction distribution coupling and electrolyte concentration/ionic conductivity nonlinearities are explicitly approximated in the model output equation on a local, electrode-averaged and distributed basis, respectively. The balanced realization controllability/observability gramian indicates that the fast electrode surface concentration dynamics are more observable/controllable than the electrode bulk concentration dynamics (i.e. state of charge)

Surface Characterization and Electrochemical Oxidation of Metal Doped Uranium Dioxide

Energy Technology Data Exchange (ETDEWEB)

Lee, Jeongmook; Kim, Jandee; Youn, Young-Sang; Kim, Jong-Goo; Ha, Yeong-Keong; Kim, Jong-Yun [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

2016-10-15

Trivalent element in UO{sub 2} matrix makes the oxygen vacancy from loss of oxygen for charge compensation. Tetravalent element alters lattice parameter of UO{sub 2} due to diameter difference between the tetravalent element and replaced U. These structural changes have significant effect on not only relevant fuel performance but also the kinetics of fuel oxidation. Park and Olander explained the stabilization of Ln (III)-doped UO{sub 2} against oxidation based on oxygen potential calculations. In this work, we have been investigated the effect of Gd{sup 3+} and Th{sup 4+} doping on the UO{sub 2} structure with Raman spectroscopy and X-ray diffraction to characterize the surface structure of nuclear fuel material. For Gd doped UO{sub 2}, its electrochemical oxidation behaviors are also investigated. The Gd and Th doped uranium dioxide solid solution pellets with various doping level were investigated by XRD, Raman spectroscopy, SEM, electrochemical experiments to investigate surface structure and electro chemical oxidation behaviors. The lattice parameter evaluated from XRD spectra indicated the formation of solid solutions. Raman spectra showed the existence of the oxygen vacancy. SEM images showed the grain structure on the surface of Gd doped uranium dioxide depending on doping level and oxygen-to-metal ratio.

Application of electrochemical plasma techniques in surface engineering of iron based structural materials

International Nuclear Information System (INIS)

Coaca, E.; Rusu, O.; Mihalache, M.; Minca, M.; Tacica, M.; Florea, S.; Oncioiu, G.; Andrei, V.

2013-01-01

The surface of austenitic stainless steels 304 L and 316 L was modified by various complex surface treatments: - plasma electrolytic carbo-nitriding by means of Plasma electrolytic saturation (PES); the saturation of cathodic surfaces with C, N was performed using suitable electrolytes (aqueous solutions of inorganic acids, appropriate salts containing the desired elements and certain organic compounds); -electrodeposition of Al from ChCl based Ionic Liquid. The coatings obtained in various experimental conditions have been investigated by means of electron spectroscopy, scanning electron microscopy, energy dispersion x-ray spectrometry, electrochemical techniques, and the properties of the thin films have been correlated with the microstructure and the composition of the surface layers which are strongly dependents of the different regimes of diffusion treatments. The preliminary results on Electrochemical Plasma Technology (EPT) treatments demonstrate that we can select the processing parameters for essential improvement of corrosion behaviour in some aggressive medium and high values of microhardness. (authors)

Surface structured platinum electrodes for the electrochemical reduction of carbon dioxide in imidazolium based ionic liquids.

Science.gov (United States)

Hanc-Scherer, Florin A; Montiel, Miguel A; Montiel, Vicente; Herrero, Enrique; Sánchez-Sánchez, Carlos M

2015-10-07

The direct CO2 electrochemical reduction on model platinum single crystal electrodes Pt(hkl) is studied in [C2mim(+)][NTf2(-)], a suitable room temperature ionic liquid (RTIL) medium due to its moderate viscosity, high CO2 solubility and conductivity. Single crystal electrodes represent the most convenient type of surface structured electrodes for studying the impact of RTIL ion adsorption on relevant electrocatalytic reactions, such as surface sensitive electrochemical CO2 reduction. We propose here based on cyclic voltammetry and in situ electrolysis measurements, for the first time, the formation of a stable adduct [C2mimH-CO2(-)] by a radical-radical coupling after the simultaneous reduction of CO2 and [C2mim(+)]. It means between the CO2 radical anion and the radical formed from the reduction of the cation [C2mim(+)] before forming the corresponding electrogenerated carbene. This is confirmed by the voltammetric study of a model imidazolium-2-carboxylate compound formed following the carbene pathway. The formation of that stable adduct [C2mimH-CO2(-)] blocks CO2 reduction after a single electron transfer and inhibits CO2 and imidazolium dimerization reactions. However, the electrochemical reduction of CO2 under those conditions provokes the electrochemical cathodic degradation of the imidazolium based RTIL. This important limitation in CO2 recycling by direct electrochemical reduction is overcome by adding a strong acid, [H(+)][NTf2(-)], into solution. Then, protons become preferentially adsorbed on the electrode surface by displacing the imidazolium cations and inhibiting their electrochemical reduction. This fact allows the surface sensitive electro-synthesis of HCOOH from CO2 reduction in [C2mim(+)][NTf2(-)], with Pt(110) being the most active electrode studied.

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 Control of pH in Nanoliter Volumes

NARCIS (Netherlands)

Balakrishnan, Divya; Lamblin, Guillaume; Thomann, Jean Sebastien; Van Den Berg, Albert; Olthuis, Wouter; Pascual-García, César

2018-01-01

The electrochemical management of the proton concentration in miniaturized dimensions opens the way to control and parallelize multistep chemical reactions, but still it faces many challenges linked to the efficient proton generation and control of their diffusion. Here we present a device operated

Electrochemical immobilization of biomolecules on gold surface modified with monolayered L-cysteine

Energy Technology Data Exchange (ETDEWEB)

Honda, Mitsunori, E-mail: honda.mitsunori@jaea.go.jp; Baba, Yuji; Sekiguchi, Tetsuhiro; Shimoyama, Iwao; Hirao, Norie

2014-04-01

Immobilization of organic molecules on the top of a metal surface is not easy because of lattice mismatch between organic and metal crystals. Gold atoms bind to thiol groups through strong chemical bonds, and a self-assembled monolayer of sulfur-terminated organic molecules is formed on the gold surface. Herein, we suggested that a monolayer of L-cysteine deposited on a gold surface can act as a buffer layer to immobilize biomolecules on the metal surface. We selected lactic acid as the immobilized biomolecule because it is one of the simplest carboxyl-containing biomolecules. The immobilization of lactic acid on the metal surface was carried out by an electrochemical method in an aqueous environment under the potential range varying from − 0.6 to + 0.8 V. The surface chemical states before and after the electrochemical reaction were characterized using X-ray photoelectron spectroscopy (XPS). The N 1s and C 1s XPS spectra showed that the L-cysteine-modified gold surface can immobilize lactic acid via peptide bonds. This technique might enable the immobilization of large organic molecules and biomolecules. - Highlights: • Monolayer l-cysteine deposited on Au surface as a buffer layer to immobilize biomolecules. • Lactic acid as the immobilized biomolecule as it is simple carboxyl-containing biomolecule. • X-ray photoelectron spectroscopy (XPS) of surface chemical states, before and after. • L-cysteine-modified Au surface can immobilize lactic acid via peptide bonds.

Electrochemical immobilization of biomolecules on gold surface modified with monolayered L-cysteine

International Nuclear Information System (INIS)

Honda, Mitsunori; Baba, Yuji; Sekiguchi, Tetsuhiro; Shimoyama, Iwao; Hirao, Norie

2014-01-01

Immobilization of organic molecules on the top of a metal surface is not easy because of lattice mismatch between organic and metal crystals. Gold atoms bind to thiol groups through strong chemical bonds, and a self-assembled monolayer of sulfur-terminated organic molecules is formed on the gold surface. Herein, we suggested that a monolayer of L-cysteine deposited on a gold surface can act as a buffer layer to immobilize biomolecules on the metal surface. We selected lactic acid as the immobilized biomolecule because it is one of the simplest carboxyl-containing biomolecules. The immobilization of lactic acid on the metal surface was carried out by an electrochemical method in an aqueous environment under the potential range varying from − 0.6 to + 0.8 V. The surface chemical states before and after the electrochemical reaction were characterized using X-ray photoelectron spectroscopy (XPS). The N 1s and C 1s XPS spectra showed that the L-cysteine-modified gold surface can immobilize lactic acid via peptide bonds. This technique might enable the immobilization of large organic molecules and biomolecules. - Highlights: • Monolayer l-cysteine deposited on Au surface as a buffer layer to immobilize biomolecules. • Lactic acid as the immobilized biomolecule as it is simple carboxyl-containing biomolecule. • X-ray photoelectron spectroscopy (XPS) of surface chemical states, before and after. • L-cysteine-modified Au surface can immobilize lactic acid via peptide bonds

Controlling the properties of graphene produced by electrochemical exfoliation

International Nuclear Information System (INIS)

Hofmann, Mario; D Nguyễn, Tuân; Chiang, Wan-Yu; Hsieh, Ya-Ping

2015-01-01

The synthesis of graphene with controllable electronic and mechanical characteristics is of significant importance for its application in various fields ranging from drug delivery to energy storage. Electrochemical exfoliation of graphite has yielded graphene with widely varying behavior and could be a suitable approach. Currently, however the limited understanding of the exfoliation process obstructs targeted modification of graphene properties. We here investigate the process of electrochemical exfoliation and the impact of its parameters on the produced graphene. Using in situ optical and electrical measurements we determine that solvent intercalation is the required first step and the degree of intercalation controls the thickness of the exfoliated graphene. Electrochemical decomposition of water into gas bubbles causes the expansion of graphite and controls the functionalization and lateral size of the exfoliated graphene. Both process steps proceed at different time scales and can be individually addressed through application of pulsed voltages. The potential of the presented approach was demonstrated by improving the performance of graphene-based transparent conductors by 30times. (paper)

Controlled electrochemical doping of graphene-based 3D nanoarchitecture electrodes for supercapacitors and capacitive deionisation.

Science.gov (United States)

Abdelkader, A M; Fray, D J

2017-10-05

Chemically-doped graphenes are promising electrode materials for energy storage and electrosorption applications. Here, an affordable electrochemical green process is introduced to dope graphene with nitrogen. The process is based on reversing the polarity of two identical graphene oxide (GO) electrodes in molten KCl-LiCl-Li 3 N. During the cathodic step, the oxygen functional groups on the GO surface are removed through direct electro-deoxidation reactions or a reaction with the deposited lithium. In the anodic step, nitrogen is adsorbed onto the surface of graphene and subsequently reacts to form nitrogen-doped graphene. The doping process is controllable, and graphene with up to 7.4 at% nitrogen can be produced. The electrochemically treated electrodes show a specific capacitance of 320 F g -1 in an aqueous KOH electrolyte and maintain 96% of this value after 10 000 cycles. The electrodes also display excellent electrosorption performance in capacitive deionisation devices with the salt removal efficiency reaching up to 18.6 mg g -1 .

Optimization of Electrochemical Treatment Process Conditions for Distillery Effluent Using Response Surface Methodology

Directory of Open Access Journals (Sweden)

P. Arulmathi

2015-01-01

Full Text Available Distillery industry is recognized as one of the most polluting industries in India with a large amount of annual effluent production. In this present study, the optimization of electrochemical treatment process variables was reported to treat the color and COD of distillery spent wash using Ti/Pt as an anode in a batch mode. Process variables such as pH, current density, electrolysis time, and electrolyte dose were selected as operation variables and chemical oxygen demand (COD and color removal efficiency were considered as response variable for optimization using response surface methodology. Indirect electrochemical-oxidation process variables were optimized using Box-Behnken response surface design (BBD. The results showed that electrochemical treatment process effectively removed the COD (89.5% and color (95.1% of the distillery industry spent wash under the optimum conditions: pH of 4.12, current density of 25.02 mA/cm2, electrolysis time of 103.27 min, and electrolyte (NaCl concentration of 1.67 g/L, respectively.

Macro-mechanics controls quantum mechanics: mechanically controllable quantum conductance switching of an electrochemically fabricated atomic-scale point contact

Science.gov (United States)

Staiger, Torben; Wertz, Florian; Xie, Fangqing; Heinze, Marcel; Schmieder, Philipp; Lutzweiler, Christian; Schimmel, Thomas

2018-01-01

Here, we present a silver atomic-scale device fabricated and operated by a combined technique of electrochemical control (EC) and mechanically controllable break junction (MCBJ). With this EC-MCBJ technique, we can perform mechanically controllable bistable quantum conductance switching of a silver quantum point contact (QPC) in an electrochemical environment at room temperature. Furthermore, the silver QPC of the device can be controlled both mechanically and electrochemically, and the operating mode can be changed from ‘electrochemical’ to ‘mechanical’, which expands the operating mode for controlling QPCs. These experimental results offer the perspective that a silver QPC may be used as a contact for a nanoelectromechanical relay.

Allylic ionic liquid electrolyte-assisted electrochemical surface passivation of LiCoO2 for advanced, safe lithium-ion batteries

Science.gov (United States)

Mun, Junyoung; Yim, Taeeun; Park, Jang Hoon; Ryu, Ji Heon; Lee, Sang Young; Kim, Young Gyu; Oh, Seung M.

2014-01-01

Room-temperature ionic liquid (RTIL) electrolytes have attracted much attention for use in advanced, safe lithium-ion batteries (LIB) owing to their nonvolatility, high conductivity, and great thermal stability. However, LIBs containing RTIL-electrolytes exhibit poor cyclability because electrochemical side reactions cause problematic surface failures of the cathode. Here, we demonstrate that a thin, homogeneous surface film, which is electrochemically generated on LiCoO2 from an RTIL-electrolyte containing an unsaturated substituent on the cation (1-allyl-1-methylpiperidinium bis(trifluoromethanesulfonyl)imide, AMPip-TFSI), can avert undesired side reactions. The derived surface film comprised of a high amount of organic species from the RTIL cations homogenously covered LiCoO2 with a <25 nm layer and helped suppress unfavorable thermal reactions as well as electrochemical side reactions. The superior performance of the cell containing the AMPip-TFSI electrolyte was further elucidated by surface, electrochemical, and thermal analyses. PMID:25168309

Effect of Amine Adlayer on Electrochemical Uric Acid Sensor Conducted on Electrochemically Reduced Graphene Oxide

Energy Technology Data Exchange (ETDEWEB)

Park, Sumi; Kim, Kyuwon [Incheon National University, Incheon (Korea, Republic of)

2016-03-15

The electrochemical biosensing efficiency of uric acid (UA) detection on an electrochemically reduced graphene oxide (ERGO)-decorated electrode surface was studied by using various amine linkers used to immobilize ERGO. The amine linkers aminoethylphenyldiazonium , 2,2'-(ethylenedioxy)bis(ethylamine), 3-aminopro-pyltriethoxysilane, and polyethyleneimine were coated on indium-tin-oxide electrode surfaces through chemical or electrochemical deposition methods. ERGO-decorated surfaces were prepared by the electrochemical reduction of graphene oxide (GO), which was immobilized on the amine-coated electrode surfaces through the electrostatic interaction between GO and the ammonium ion of the linker on the surface. We monitored the sensing results of electrochemical UA detection with differential pulse voltammetry. The ERGO-modified surface presented electrocatalytic oxidation of UA and ascorbic acid. Among the different amines tested, 3-aminopropyltriethoxysilane provided the best biosensing performance in terms of sensitivity and reproducibility.

Effect of Amine Adlayer on Electrochemical Uric Acid Sensor Conducted on Electrochemically Reduced Graphene Oxide

International Nuclear Information System (INIS)

Park, Sumi; Kim, Kyuwon

2016-01-01

The electrochemical biosensing efficiency of uric acid (UA) detection on an electrochemically reduced graphene oxide (ERGO)-decorated electrode surface was studied by using various amine linkers used to immobilize ERGO. The amine linkers aminoethylphenyldiazonium , 2,2'-(ethylenedioxy)bis(ethylamine), 3-aminopro-pyltriethoxysilane, and polyethyleneimine were coated on indium-tin-oxide electrode surfaces through chemical or electrochemical deposition methods. ERGO-decorated surfaces were prepared by the electrochemical reduction of graphene oxide (GO), which was immobilized on the amine-coated electrode surfaces through the electrostatic interaction between GO and the ammonium ion of the linker on the surface. We monitored the sensing results of electrochemical UA detection with differential pulse voltammetry. The ERGO-modified surface presented electrocatalytic oxidation of UA and ascorbic acid. Among the different amines tested, 3-aminopropyltriethoxysilane provided the best biosensing performance in terms of sensitivity and reproducibility.

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

International Nuclear Information System (INIS)

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

2008-01-01

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

Electrochemical impedance spectroscopy and Surface Studies of Steel Corrosion by Sulphate-Reducing Bacteria

International Nuclear Information System (INIS)

Fathul Karim Sahrani; Zaharah Ibrahim; Madzlan Aziz; Adibah Yahya

2009-01-01

Sulphate-reducing bacteria (SRB), implicated in microbiologically influenced corrosion were isolated from the deep subsurface at the vicinity of Pasir Gudang, Johor, Malaysia. Electrochemical impedance spectroscopic (EIS) study was carried out to determine the polarization resistance in various types of culturing solutions, with SRB1, SRB2, combination of SRB1 and SRB2 and without SRBs inoculated (control). EIS results showed that in the presence of SRB1, SRB2 and mixed culture SRB1 and SRB2, polarisation resistance values were 7170, 6370 and 7190 ohms respectively compared to that of control, 92400 ohm. X-ray analysis (EDS) of the specimens indicated high sulphur content in the medium containing SRBs. Localized corrosion was observed on the metal surface which was associated with the SRB activity. (author)

Optical Sensing with Simultaneous Electrochemical Control in Metal Nanowire Arrays

Directory of Open Access Journals (Sweden)

Janos Vörös

2010-11-01

Full Text Available This work explores the alternative use of noble metal nanowire systems in large-scale array configurations to exploit both the nanowires’ conductive nature and localized surface plasmon resonance (LSPR. The first known nanowire-based system has been constructed, with which optical signals are influenced by the simultaneous application of electrochemical potentials. Optical characterization of nanowire arrays was performed by measuring the bulk refractive index sensitivity and the limit of detection. The formation of an electrical double layer was controlled in NaCl solutions to study the effect of local refractive index changes on the spectral response. Resonance peak shifts of over 4 nm, a bulk refractive index sensitivity up to 115 nm/RIU and a limit of detection as low as 4.5 × 10−4 RIU were obtained for gold nanowire arrays. Simulations with the Multiple Multipole Program (MMP confirm such bulk refractive index sensitivities. Initial experiments demonstrated successful optical biosensing using a novel form of particle-based nanowire arrays. In addition, the formation of an ionic layer (Stern-layer upon applying an electrochemical potential was also monitored by the shift of the plasmon resonance.

Plasma treatment of porous GaAs surface formed by electrochemical etching method: Characterization and properties

International Nuclear Information System (INIS)

Naddaf, M.; Saloum, S.

2008-12-01

Porous GaAs samples were formed by electrochemical anodic etching of Zn doped p-type GaAs (100) wafers at different etching parameters (time, mode of applied voltage or current and electrolyte). The effect of etching parameters and plasma surface treatment on the optical properties of the prepared sample has been investigated by using room temperature photoluminescence (PL), Raman spectroscopy and reflectance spectroscopic measurements in the range (400-800 nm). The surface morphological changes were studied by using atomic force microscope. It has been found that etching parameters can be controlled to produce a considerably low optical reflectivity porous GaAs layer, attractive for use in solar cells. In addition, it has been observed that the deposition of plasma polymerized HMDSO thin film on porous GaAs surface can be utilized to produce a surface with novel optical properties interesting for solar cells and optoelectronic devices. (author)

Direct electrical control of IgG conformation and functional activity at surfaces

Science.gov (United States)

Ghisellini, Paola; Caiazzo, Marialuisa; Alessandrini, Andrea; Eggenhöffner, Roberto; Vassalli, Massimo; Facci, Paolo

2016-11-01

We have devised a supramolecular edifice involving His-tagged protein A and antibodies to yield surface immobilized, uniformly oriented, IgG-type, antibody layers with Fab fragments exposed off an electrode surface. We demonstrate here that we can affect the conformation of IgGs, likely pushing/pulling electrostatically Fab fragments towards/from the electrode surface. A potential difference between electrode and solution acts on IgGs’ charged aminoacids modulating the accessibility of the specific recognition regions of Fab fragments by antigens in solution. Consequently, antibody-antigen affinity is affected by the sign of the applied potential: a positive potential enables an effective capture of antigens; a negative one pulls the fragments towards the electrode, where steric hindrance caused by neighboring molecules largely hampers the capture of antigens. Different experimental techniques (electrochemical quartz crystal microbalance, electrochemical impedance spectroscopy, fluorescence confocal microscopy and electrochemical atomic force spectroscopy) were used to evaluate binding kinetics, surface coverage, effect of the applied electric field on IgGs, and role of charged residues on the phenomenon described. These findings expand the concept of electrical control of biological reactions and can be used to gate electrically specific recognition reactions with impact in biosensors, bioactuators, smart biodevices, nanomedicine, and fundamental studies related to chemical reaction kinetics.

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.

Low-waste electrochemical decontamination of stainless-steel surface

International Nuclear Information System (INIS)

Babain, V.A.; Smirnov, I.V.; Shadrin, A.Yu.; Firsin, N.G.; Zakharchuk, G.A.; Pavlov, A.B.; Shilov, V.V.

2002-01-01

An electrochemical decontamination method using a formic acid-based recycling electrolyte was proposed to remove firmly fixed contaminants from stainless-steel surfaces. The following provisions make for minimisation of the amounts of waste: (i) use of specially designed electrodes with vacuum removal of spent electrolyte; (ii) inter-cycle removal of radionuclides from the electrolyte by using an inorganic sorbent; (iii) periodic regeneration of the spent electrolyte. the dissolved metals (Fe, Cr, Ni) being transformed into acidic phosphates; (iv) solidification of residues arising from the regeneration of the electrolyte and spent sorbent into iron-phosphate ceramics. The technology and equipment developed were used for decontamination of a plutonium glove-box. The level of surface contamination was reduced 100-fold in two decontamination cycles. The depth of metal skimming was 1.5 μ for the ceiling and walls and 4.5 μ for the table top. Each square meter of stainless-steel surface provides about 100 g of solid radioactive waste in the form of iron-phosphate ceramic blocks

Electrochemically controlled iron isotope fractionation

Science.gov (United States)

Black, Jay R.; Young, Edward D.; Kavner, Abby

2010-02-01

Variations in the stable isotope abundances of transition metals have been observed in the geologic record and trying to understand and reconstruct the physical/environmental conditions that produced these signatures is an area of active research. It is clear that changes in oxidation state lead to large fractionations of the stable isotopes of many transition metals such as iron, suggesting that transition metal stable isotope signatures could be used as a paleo-redox proxy. However, the factors contributing to these observed stable isotope variations are poorly understood. Here we investigate how the kinetics of iron redox electrochemistry generates isotope fractionation. Through a combination of electrodeposition experiments and modeling of electrochemical processes including mass-transport, we show that electron transfer reactions are the cause of a large isotope separation, while mass transport-limited supply of reactant to the electrode attenuates the observed isotopic fractionation. Furthermore, the stable isotope composition of electroplated transition metals can be tuned in the laboratory by controlling parameters such as solution chemistry, reaction overpotential, and solution convection. These methods are potentially useful for generating isotopically-marked metal surfaces for tracking and forensic purposes. In addition, our studies will help interpret stable isotope data in terms of identifying underlying electron transfer processes in laboratory and natural samples.

Electrochemical supercapacitor application of electroless surface polymerization of polyaniline nanostructures

International Nuclear Information System (INIS)

Amarnath, Chellachamy A.; Chang, Jin Ho; Kim, Doyoung; Mane, Rajaram S.; Han, Sung-Hwan; Sohn, Daewon

2009-01-01

Electrochemical supercapacitive behaviour of polyaniline nanostructures, i.e., nanorods and nanospheres fabricated on aniline-primed conducting indium-tin oxide substrate via electroless surface polymerization using ammonium persulfate as initiator and selenious acid as efficient dopant is investigated. The self-assembled monolayer of urea derivative in presence of 3-(triethoxysilyl)-propyl isocyanate and aniline plays role of aniline-primed substrate. Polyaniline electrode composed of nanorods of excess surface area responsible for large redox reactions has shown 592 F g -1 specific capacitance which is significantly greater than closely compact polyaniline nanospheres, i.e., 214 F g -1

Electrochemical formation and characterization of Au nanostructures on a highly ordered pyrolytic graphite surface

International Nuclear Information System (INIS)

Arroyo Gómez, José J.; Zubieta, Carolina; Ferullo, Ricardo M.; García, Silvana G.

2016-01-01

Graphical abstract: - Highlights: • The electrodeposition of Au on HOPG tends to follow the response predicted for a 3D instantaneous nucleation mechanism in the potential range considered. • By choosing suitable nucleation and growth pulses, one-dimensional deposits were possible, preferentially located on step edges of the HOPG substrate. • Quantum-mechanical calculations confirmed the tendency of Au atoms to join selectively on the HOPG step edges, at the early stages of Au electrodeposition. - Abstract: The electrochemical formation of Au nanoparticles on a highly ordered pyrolytic graphite (HOPG) substrate using conventional electrochemical techniques and ex-situ AFM is reported. From the potentiostatic current transients studies, the Au electrodeposition process on HOPG surfaces was described, within the potential range considered, by a model involving instantaneous nucleation and diffusion controlled 3D growth, which was corroborated by the microscopic analysis. Initially, three-dimensional (3D) hemispherical nanoparticles distributed on surface defects (step edges) of the substrate were observed, with increasing particle size at more negative potentials. The double potential pulse technique allowed the formation of rounded deposits at low deposition potentials, which tend to form lines of nuclei aligned in defined directions leading to 3D ordered structures. By choosing suitable nucleation and growth pulses, one-dimensional (1D) deposits were possible, preferentially located on step edges of the HOPG substrate. Quantum-mechanical calculations confirmed the tendency of Au atoms to join selectively on surface defects, such as the HOPG step edges, at the early stages of Au electrodeposition.

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.

Preparation, Modification, Characterization, and Biosensing Application of Nanoporous Gold Using Electrochemical Techniques.

Science.gov (United States)

Bhattarai, Jay K; Neupane, Dharmendra; Nepal, Bishal; Mikhaylov, Vasilii; Demchenko, Alexei V; Stine, Keith J

2018-03-16

Nanoporous gold (np-Au), because of its high surface area-to-volume ratio, excellent conductivity, chemical inertness, physical stability, biocompatibility, easily tunable pores, and plasmonic properties, has attracted much interested in the field of nanotechnology. It has promising applications in the fields of catalysis, bio/chemical sensing, drug delivery, biomolecules separation and purification, fuel cell development, surface-chemistry-driven actuation, and supercapacitor design. Many chemical and electrochemical procedures are known for the preparation of np-Au. Recently, researchers are focusing on easier and controlled ways to tune the pores and ligaments size of np-Au for its use in different applications. Electrochemical methods have good control over fine-tuning pore and ligament sizes. The np-Au electrodes that are prepared using electrochemical techniques are robust and are easier to handle for their use in electrochemical biosensing. Here, we review different electrochemical strategies for the preparation, post-modification, and characterization of np-Au along with the synergistic use of both electrochemistry and np-Au for applications in biosensing.

In situ electrochemical-mass spectroscopic investigation of solid electrolyte interphase formation on the surface of a carbon electrode

International Nuclear Information System (INIS)

Gourdin, Gerald; Zheng, Dong; Smith, Patricia H.; Qu, Deyang

2013-01-01

The energy density of an electrochemical capacitor can be significantly improved by utilizing a lithiated negative electrode and a high surface area positive electrode. During lithiation of the negative carbon electrode, the electrolyte reacts with the electrode surface and undergoes decomposition to form a solid electrolyte interphase (SEI) layer that passivates the surface of the carbon electrode from further reactions between Li and the electrolyte. The reduction reactions that the solvent undergoes also form insoluble and gaseous by-products. In this work, those gaseous by-products generated by reductive decomposition of a carbonate-based electrolyte, 1.2 M LiPF 6 in EC/PC/DEC (3:1:4), were analyzed at different stages during the lithiation process of an amorphous carbon electrode. The stages in the generation of gaseous by-products were determined to come as a result of two, 1-electron reduction steps of the cyclic carbonate components of the electrolyte. Electrochemical impedance spectroscopy was also used to investigate the two distinct electrochemical processes and the development of the two phases of the SEI structure. This is the first time that the state of an electrochemical cell during the formation of the SEI layer has been systematically correlated with theoretical reaction mechanisms through the use of in situ electrochemical-MS and impedance spectroscopy analyses

Diamond surface functionalization with biomimicry – Amine surface tether and thiol moiety for electrochemical sensors

Energy Technology Data Exchange (ETDEWEB)

Sund, James B., E-mail: jim@jamessund.com [Department of Electrical and Computer Engineering, Duke University, Durham, NC (United States); Causey, Corey P. [Departments of Chemistry and Biochemistry, Duke University, Durham, NC (United States); Wolter, Scott D. [Department of Physics, Elon University, Elon, NC 27244 (United States); Parker, Charles B., E-mail: charles.parker@duke.edu [Department of Electrical and Computer Engineering, Duke University, Durham, NC (United States); Stoner, Brian R. [Department of Electrical and Computer Engineering, Duke University, Durham, NC (United States); Research Triangle Institute (RTI) International, Research Triangle Park, NC (United States); Toone, Eric J. [Departments of Chemistry and Biochemistry, Duke University, Durham, NC (United States); Glass, Jeffrey T. [Department of Electrical and Computer Engineering, Duke University, Durham, NC (United States)

2014-05-01

Highlights: • Diamond surfaces were functionalized with organic molecules using a novel approach. • Used biomimicry to select a molecule to bind NO, similar to the human body. • Molecular orbital theory predicted the molecule-analyte oxidation behavior. • A thiol moiety was attached to an amine surface tether on the diamond surface. • XPS analysis verified each surface functionalization step. - Abstract: The surface of conducting diamond was functionalized with a terminal thiol group that is capable of binding and detecting nitrogen–oxygen species. The functionalization process employed multiple steps starting with doped diamond films grown by plasma enhanced chemical vapor deposition followed by hydrogen termination and photochemical attachment of a chemically protected amine alkene. The surface tether was deprotected to reveal the amine functionality, which enabled the tether to be extended with surface chemistry to add a terminal thiol moiety for electrochemical sensing applications. Each step of the process was validated using X-ray photoelectron spectroscopy analysis.

Diamond surface functionalization with biomimicry – Amine surface tether and thiol moiety for electrochemical sensors

International Nuclear Information System (INIS)

Sund, James B.; Causey, Corey P.; Wolter, Scott D.; Parker, Charles B.; Stoner, Brian R.; Toone, Eric J.; Glass, Jeffrey T.

2014-01-01

Highlights: • Diamond surfaces were functionalized with organic molecules using a novel approach. • Used biomimicry to select a molecule to bind NO, similar to the human body. • Molecular orbital theory predicted the molecule-analyte oxidation behavior. • A thiol moiety was attached to an amine surface tether on the diamond surface. • XPS analysis verified each surface functionalization step. - Abstract: The surface of conducting diamond was functionalized with a terminal thiol group that is capable of binding and detecting nitrogen–oxygen species. The functionalization process employed multiple steps starting with doped diamond films grown by plasma enhanced chemical vapor deposition followed by hydrogen termination and photochemical attachment of a chemically protected amine alkene. The surface tether was deprotected to reveal the amine functionality, which enabled the tether to be extended with surface chemistry to add a terminal thiol moiety for electrochemical sensing applications. Each step of the process was validated using X-ray photoelectron spectroscopy analysis

Biocompatibility of Mg Ion Doped Hydroxyapatite Films on Ti-6Al-4V Surface by Electrochemical Deposition.

Science.gov (United States)

Lee, Kang; Choe, Han-Cheol

2016-02-01

In this study, we prepared magnesium (Mg) doped nano-phase hydroxyapatite (HAp) films on the TiO2 nano-network surface using electrochemical deposition method. Ti-6Al-4V ELI surface was anodized in 5 M NaOH solution at 0.3 A for 10 min. Nano-network TiO2 surface were formed by these anodization steps which acted as templates and anchorage for growth of the Mg doped HAp during subsequent pulsed electrochemical deposition process at 85 degrees C. The phase and morphologies of HAp deposits were influenced by the Mg ion concentration.

Precise thickness control in recess etching of AlGaN/GaN hetero-structure using photocarrier-regulated electrochemical process

Science.gov (United States)

Kumazaki, Yusuke; Uemura, Keisuke; Sato, Taketomo; Hashizume, Tamotsu

2017-05-01

The photocarrier-regulated electrochemical (PREC) process was developed for fabricating recessed-gate AlGaN/GaN high-electron-mobility transistors (HEMTs) for normally off operation. The PREC process is based on photo-assisted electrochemical etching using low-energy chemical reactions. The fundamental photo-electrochemical measurements on AlGaN/GaN heterostructures revealed that the photo-carriers generated in the top AlGaN layer caused homogeneous etching of AlGaN with a smooth surface, but those generated in the GaN layer underneath caused inhomogeneous etching that roughens the surface. The concept of the PREC process is to supply the photo-carriers generated only in the AlGaN layer by selecting proper conditions on light wavelength and voltage. The phenomenon of self-termination etching has been observed during the PREC process, where the etching depth was controlled by light intensity. The recessed-gate AlGaN/GaN HEMT fabricated with the PREC process showed positive threshold voltage and improvement in transconductance compared to planar-gate AlGaN/GaN HEMTs.

Electrochemical investigations for understanding and controlling corrosion in nuclear reactor materials

International Nuclear Information System (INIS)

Gnanamoorthy, J.B.

1998-01-01

Electrochemical techniques such as potentiodynamic polarization have been used at the Indira Gandhi Centre for Atomic Research at Kalpakkam for understanding and controlling the corrosion of nuclear reactor materials such as austenitic stainless steels and chrome-moly steels. Results on the measurements of critical potentials for pitting and crevice corrosion of stainless steels and their weldments and of laser surface modified stainless steels in aqueous chloride solutions are discussed. Investigations carried out to correlate the degree of sensitization in types 304 and 316 stainless steels, measured by the electrochemical potentiokinetic reactivation technique, with the susceptibility to intergranular corrosion and intergranular stress corrosion cracking have been discussed. The stress corrosion cracking behaviour of weldments of type 316 stainless steel was studied in a boiling solution of a mixture of 5 M NaCl and 0.15 M Na 2 SO 4 acidified to give a pH of 1.3 by monitoring of the open circuit potential with time as well as by anodic polarization. Interesting information could also been obtained on the microbiologically influenced corrosion of type 304 stainless steels in a fresh water system by carrying out cyclic potentiodynamic polarization measurements as well as by monitoring the open circuit potential measurements with exposure time. Since secondary phases present (or developed during thermal ageing) in stainless steels have a significant influence on their corrosion behaviour, the estimation of these secondary phases by electrochemical methods has also been discussed. (author)

Electrochemical characterization of organosilane-functionalized nanostructured ITO surfaces

Energy Technology Data Exchange (ETDEWEB)

Pruna, R., E-mail: rpruna@el.ub.edu; Palacio, F.; López, M. [SIC, Departament d' Enginyeries: Electrònica, Universitat de Barcelona, C/ Martí i Franquès 1, E-08028 Barcelona (Spain); Pérez, J. [Nanobioengineering Group, Institute for Bioengineering of Catalonia (IBEC), Baldiri Reixac 15-21, E-08028 Barcelona (Spain); Mir, M. [Nanobioengineering Group, Institute for Bioengineering of Catalonia (IBEC), Baldiri Reixac 15-21, E-08028 Barcelona (Spain); Centro de Investigación Biomédica en Red en Bioingeniería, Biomateriales y Nanomedicina (CIBER-BBN), Monforte de Lemos 3-5 Pabellón 11, E-28029 Madrid (Spain); Blázquez, O.; Hernández, S.; Garrido, B. [MIND-IN" 2UB, Departament d' Enginyeries: Electrònica, Universitat de Barcelona, C/ Martí i Franquès 1, E-08028 Barcelona (Spain)

2016-08-08

The electroactivity of nanostructured indium tin oxide (ITO) has been investigated for its further use in applications such as sensing biological compounds by the analysis of redox active molecules. ITO films were fabricated by using electron beam evaporation at different substrate temperatures and subsequently annealed for promoting their crystallization. The morphology of the deposited material was monitored by scanning electron microscopy, confirming the deposition of either thin films or nanowires, depending on the substrate temperature. Electrochemical surface characterization revealed a 45 % increase in the electroactive surface area of nanostructured ITO with respect to thin films, one third lower than the geometrical surface area variation determined by atomic force microscopy. ITO surfaces were functionalized with a model organic molecule known as 6-(ferrocenyl)hexanethiol. The chemical attachment was done by means of a glycidoxy compound containing a reactive epoxy group, the so-called 3-glycidoxypropyltrimethoxy-silane. ITO functionalization was useful for determining the benefits of nanostructuration on the surface coverage of active molecules. Compared to ITO thin films, an increase in the total peak height of 140 % was observed for as-deposited nanostructured electrodes, whereas the same measurement for annealed electrodes resulted in an increase of more than 400 %. These preliminary results demonstrate the ability of nanostructured ITO to increase the surface-to-volume ratio, conductivity and surface area functionalization, features that highly benefit the performance of biosensors.

Electrochemical characterization of organosilane-functionalized nanostructured ITO surfaces

International Nuclear Information System (INIS)

Pruna, R.; Palacio, F.; López, M.; Pérez, J.; Mir, M.; 2UB, Departament d'Enginyeries: Electrònica, Universitat de Barcelona, C/ Martí i Franquès 1, E-08028 Barcelona (Spain))" data-affiliation=" (MIND-IN2UB, Departament d'Enginyeries: Electrònica, Universitat de Barcelona, C/ Martí i Franquès 1, E-08028 Barcelona (Spain))" >Blázquez, O.; 2UB, Departament d'Enginyeries: Electrònica, Universitat de Barcelona, C/ Martí i Franquès 1, E-08028 Barcelona (Spain))" data-affiliation=" (MIND-IN2UB, Departament d'Enginyeries: Electrònica, Universitat de Barcelona, C/ Martí i Franquès 1, E-08028 Barcelona (Spain))" >Hernández, S.; 2UB, Departament d'Enginyeries: Electrònica, Universitat de Barcelona, C/ Martí i Franquès 1, E-08028 Barcelona (Spain))" data-affiliation=" (MIND-IN2UB, Departament d'Enginyeries: Electrònica, Universitat de Barcelona, C/ Martí i Franquès 1, E-08028 Barcelona (Spain))" >Garrido, B.

2016-01-01

The electroactivity of nanostructured indium tin oxide (ITO) has been investigated for its further use in applications such as sensing biological compounds by the analysis of redox active molecules. ITO films were fabricated by using electron beam evaporation at different substrate temperatures and subsequently annealed for promoting their crystallization. The morphology of the deposited material was monitored by scanning electron microscopy, confirming the deposition of either thin films or nanowires, depending on the substrate temperature. Electrochemical surface characterization revealed a 45 % increase in the electroactive surface area of nanostructured ITO with respect to thin films, one third lower than the geometrical surface area variation determined by atomic force microscopy. ITO surfaces were functionalized with a model organic molecule known as 6-(ferrocenyl)hexanethiol. The chemical attachment was done by means of a glycidoxy compound containing a reactive epoxy group, the so-called 3-glycidoxypropyltrimethoxy-silane. ITO functionalization was useful for determining the benefits of nanostructuration on the surface coverage of active molecules. Compared to ITO thin films, an increase in the total peak height of 140 % was observed for as-deposited nanostructured electrodes, whereas the same measurement for annealed electrodes resulted in an increase of more than 400 %. These preliminary results demonstrate the ability of nanostructured ITO to increase the surface-to-volume ratio, conductivity and surface area functionalization, features that highly benefit the performance of biosensors.

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 analysis of the UV treated bactericidal Ti6Al4V surfaces

Energy Technology Data Exchange (ETDEWEB)

Pacha-Olivenza, Miguel A. [Networking Research Center on Bioengineering, Biomaterials and Nanomedicine (CIBER-BBN) (Spain); Department of Applied Physics, Faculty of Science, University of Extremadura, Av. Elvas s/n, 06071 Badajoz (Spain); Gallardo-Moreno, Amparo M., E-mail: amparogm@unex.es [Department of Applied Physics, Faculty of Science, University of Extremadura, Av. Elvas s/n, 06071 Badajoz (Spain); Networking Research Center on Bioengineering, Biomaterials and Nanomedicine (CIBER-BBN) (Spain); Vadillo-Rodríguez, Virginia; González-Martín, M. Luisa [Department of Applied Physics, Faculty of Science, University of Extremadura, Av. Elvas s/n, 06071 Badajoz (Spain); Networking Research Center on Bioengineering, Biomaterials and Nanomedicine (CIBER-BBN) (Spain); Pérez-Giraldo, Ciro [Department of Microbiology, Faculty of Medicine, University of Extremadura, Av. Elvas s/n, 06071 Badajoz (Spain); Networking Research Center on Bioengineering, Biomaterials and Nanomedicine (CIBER-BBN) (Spain); Galván, Juan C. [National Centre for Metallurgical Research (CENIM-CSIC), Av. Gregorio del Amo 8, 28040-Madrid (Spain)

2013-04-01

This research investigates in detail the bactericidal effect exhibited by the surface of the biomaterial Ti6Al4V after being subjected to UV-C light. It has been recently hypothesized that small surface currents, occurring as a consequence of the electron–hole pair recombination taking place after the excitation process, are behind the bactericidal properties displayed by this UV-treated material. To corroborate this hypothesis we have used different electrochemical techniques, such as electrochemical impedance spectroscopy (EIS), potentiodynamic polarization plots and Mott–Schottky plots. EIS and Mott–Schottky plots have shown that UV-C treatment causes an initial increase on the surface electrical conduction of this material. In addition, EIS and polarization plots demonstrated that higher corrosion currents occur at the UV treated than at the non-irradiated samples. Despite this increase in the corrosion currents, EIS has also shown that such currents are not likely to affect the good stability of this material oxide film since the irradiated samples completely recovered the control values after being stored in dark conditions for a period not longer than 24 h. These results agree with the already-published in vitro transitory behavior of the bactericidal effect, which was shown to be present at initial times after the biomaterial implantation, a crucial moment to avoid a large number of biomaterial associated infections. Highlights: ► Bactericidal response of UV-treated Ti6Al4V is explained through electrochemistry. ► There is an increase in the superficial electrical conduction after UV-treatment. ► Higher corrosion currents for UV-treated against non-UV-treated samples are shown. ► EIS shows the recuperation on irradiated samples in agreement with microbial tests.

Electrochemical analysis of the UV treated bactericidal Ti6Al4V surfaces

International Nuclear Information System (INIS)

Pacha-Olivenza, Miguel A.; Gallardo-Moreno, Amparo M.; Vadillo-Rodríguez, Virginia; González-Martín, M. Luisa; Pérez-Giraldo, Ciro; Galván, Juan C.

2013-01-01

This research investigates in detail the bactericidal effect exhibited by the surface of the biomaterial Ti6Al4V after being subjected to UV-C light. It has been recently hypothesized that small surface currents, occurring as a consequence of the electron–hole pair recombination taking place after the excitation process, are behind the bactericidal properties displayed by this UV-treated material. To corroborate this hypothesis we have used different electrochemical techniques, such as electrochemical impedance spectroscopy (EIS), potentiodynamic polarization plots and Mott–Schottky plots. EIS and Mott–Schottky plots have shown that UV-C treatment causes an initial increase on the surface electrical conduction of this material. In addition, EIS and polarization plots demonstrated that higher corrosion currents occur at the UV treated than at the non-irradiated samples. Despite this increase in the corrosion currents, EIS has also shown that such currents are not likely to affect the good stability of this material oxide film since the irradiated samples completely recovered the control values after being stored in dark conditions for a period not longer than 24 h. These results agree with the already-published in vitro transitory behavior of the bactericidal effect, which was shown to be present at initial times after the biomaterial implantation, a crucial moment to avoid a large number of biomaterial associated infections. Highlights: ► Bactericidal response of UV-treated Ti6Al4V is explained through electrochemistry. ► There is an increase in the superficial electrical conduction after UV-treatment. ► Higher corrosion currents for UV-treated against non-UV-treated samples are shown. ► EIS shows the recuperation on irradiated samples in agreement with microbial tests

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.

Electrochemical removal of biofilms from titanium dental implant surfaces.

Science.gov (United States)

Schneider, Sebastian; Rudolph, Michael; Bause, Vanessa; Terfort, Andreas

2018-06-01

The infection of dental implants may cause severe inflammation of tissue and even bone degradation if not treated. For titanium implants, a new, minimally invasive approach is the electrochemical removal of the biofilms including the disinfection of the metal surface. In this project, several parameters, such as electrode potentials and electrolyte compositions, were varied to understand the underlying mechanisms. Optimal electrolytes contained iodide as well as lactic acid. Electrochemical experiments, such as cyclic voltammetry or measurements of open circuit potentials, were performed in different cell set-ups to distinguish between different possible reactions. At the applied potentials of E species are formed at the anode, such as triiodide and hydrogen peroxide. Ex situ tests with model biofilms of E. coli clearly demonstrated the effectiveness of the respective anolytes in killing the bacteria, as determined by the LIVE/DEAD™ assay. Using optimized electrolysis parameters of 30 s at 7.0 V and 300 mA, a 14-day old wildtype biofilm could be completely removed from dental implants in vitro. Copyright © 2018 Elsevier B.V. All rights reserved.

Effect of passive film on electrochemical surface treatment for indium tin oxide

International Nuclear Information System (INIS)

Wu, Yung-Fu; Chen, Chi-Hao

2013-01-01

Highlights: ► Oxalic, tartaric, and citric acid baths accompanying with applied voltages were used to treat the ITO surface. ► We investigated the changes in ITO surfaces by examining the potentiodynamic behavior of ITO films. ► AFM analysis showed the formation of a passive layer could assist to planarize surface. ► XPS analysis indicated this passive layer was mainly composed of SnO 2. ► A better planarization was obtained by treating in 3.0 wt.% tartaric acid at 0.5 V due to weak complexation strength. - Abstract: Changes in indium tin oxide (ITO) film surface during electrochemical treatment in oxalic acid, tartaric acid, and citric acid were investigated. Controlling the voltage applied on ITO film allows the formation of a passive layer, effectively protecting the film surface. X-ray photoelectron spectrometry showed that the passive layer composition was predominantly SnO 2 in tartaric acid, while a composite of tin oxide and tin carboxylate in citric or oxalic acid. Even though the passive films on ITO surface generated in these organic acids, the indium or tin could complex with the organic acid anions, enhancing the dissolution of ITO films. The experimental results show that the interaction between the dissolution and passivation could assist to planarize the ITO surface. We found that the optimal treatment at 0.5 V in 3 wt.% tartaric acid could provide the ITO surface with root-mean-squared roughness less than 1.0 nm, due to the weak complexing characteristics of tartaric acid.

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

Energy Technology Data Exchange (ETDEWEB)

Jalili, M. [Nanomaterials and Nanocoatings Department, Institute for Color Science and Technology (ICST), PO 16765-654, Tehran (Iran, Islamic Republic of); Surface Coatings and Corrosion Department, Institute for Color Science and Technology (ICST), PO 16765-654, Tehran (Iran, Islamic Republic of); Rostami, M. [Nanomaterials and Nanocoatings Department, Institute for Color Science and Technology (ICST), PO 16765-654, Tehran (Iran, Islamic Republic of); Ramezanzadeh, B., E-mail: ramezanzadeh-bh@icrc.ac.ir [Surface Coatings and Corrosion Department, Institute for Color Science and Technology (ICST), PO 16765-654, Tehran (Iran, Islamic Republic of)

2015-02-15

Highlights: • Aluminum nanoparticle was modified with amino trimethylene phosphonic acid. • 2 wt% of zinc dust in zinc-rich paint was substituted by aluminum nanoparticles. • Surface modified aluminum nanoparticle improved the cathodic period of protection. • Aluminum nanoparticles enhanced the corrosion protection of the zinc-rich coating. - Abstract: 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.

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

International Nuclear Information System (INIS)

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

2015-01-01

Highlights: • Aluminum nanoparticle was modified with amino trimethylene phosphonic acid. • 2 wt% of zinc dust in zinc-rich paint was substituted by aluminum nanoparticles. • Surface modified aluminum nanoparticle improved the cathodic period of protection. • Aluminum nanoparticles enhanced the corrosion protection of the zinc-rich coating. - Abstract: 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

Preparation, Modification, Characterization, and Biosensing Application of Nanoporous Gold Using Electrochemical Techniques

Directory of Open Access Journals (Sweden)

Jay K. Bhattarai

2018-03-01

Full Text Available Nanoporous gold (np-Au, because of its high surface area-to-volume ratio, excellent conductivity, chemical inertness, physical stability, biocompatibility, easily tunable pores, and plasmonic properties, has attracted much interested in the field of nanotechnology. It has promising applications in the fields of catalysis, bio/chemical sensing, drug delivery, biomolecules separation and purification, fuel cell development, surface-chemistry-driven actuation, and supercapacitor design. Many chemical and electrochemical procedures are known for the preparation of np-Au. Recently, researchers are focusing on easier and controlled ways to tune the pores and ligaments size of np-Au for its use in different applications. Electrochemical methods have good control over fine-tuning pore and ligament sizes. The np-Au electrodes that are prepared using electrochemical techniques are robust and are easier to handle for their use in electrochemical biosensing. Here, we review different electrochemical strategies for the preparation, post-modification, and characterization of np-Au along with the synergistic use of both electrochemistry and np-Au for applications in biosensing.

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.

[The effect of epigallocatechin gallate (EGCG) on the surface properties of nickel-chromium dental casting alloys after electrochemical corrosion].

Science.gov (United States)

Qiao, Guang-yan; Zhang, Li-xia; Wang, Jue; Shen, Qing-ping; Su, Jian-sheng

2014-08-01

To investigate the effect of epigallocatechin gallate (EGCG) on the surface properties of nickel-chromium dental alloys after electrochemical corrosion. The surface morphology and surface structure of nickel-chromium dental alloys were examined by stereomicroscope and scanning electron microscopy before and after electrochemical tests in 0 g/L and 1.0 g/L EGCG artificial saliva. The surface element component and chemical states of nickel-chromium dental alloys were analyzed by X-ray photoelectron spectrograph after electrochemical tests in 0 g/L and 1.0 g/L EGCG artificial saliva. More serious corrosion happened on the surface of nickel-chromium alloy in 1.0 g/L EGCG artificial saliva than in 0 g/L EGCG. The diameters of corrosion pits were smaller, and the dendrite structure of the alloy surface was not affected in 0 g/L EGCG. While the diameters of corrosion pits were larger, the dendritic interval of the alloy surface began to merge, and the dendrite structure was fuzzy in 1.0 g/L EGCG. In addition, the O, Ni, Cr, Be, C and Mo elements were detected on the surface of nickel-chromium alloys after sputtered for 120 s in 0 g/L EGCG and 1.0 g/L EGCG artificial saliva after electrochemical corrosion, and the surface oxides were mainly NiO and Cr(2)O(3). Compared with 0 g/L EGCG artificial saliva, the content of O, NiO and Cr(2)O(3) were lower in 1.0 g/L EGCG. The results of surface morphology and the corrosion products both show that the corrosion resistance of nickel-chromium alloys become worse and the oxide content of corrosion products on the surface reduce in 1.0 g/L EGCG artificial saliva.

Optically Designed Anodised Aluminium Surfaces: Microstructural and Electrochemical Aspects

DEFF Research Database (Denmark)

Gudla, Visweswara Chakravarthy

is not possible as the anodic pore sizes are an order of magnitude smaller than the traditional white pigments. The approaches presented in this thesis focus on different techniques like modification of the aluminium microstructure, engineering of the aluminium surface, and application on non...... the microstructure in order to impart light scattering ability to the anodised layer. Coatings based on Al-Zr and Al-Ti binary system were studied for their anodising behaviour with and without heat treatment. The structure evolution of the Al-Zr sputtered coatings and the effect of Si during heat treatment...... Emission Spectroscopy, and Scanning Kelvin Probe Force Microscopy. Optical characterization was performed using integrating sphere measurements. Combining the results and understanding obtained from anodising of magnetron sputtered coatings, Al-TiO2 surface composites and their electrochemical behaviour...

DFT and electrochemical studies of tris(benzimidazole-2-ylmethyl)amine as an efficient corrosion inhibitor for carbon steel surface

Energy Technology Data Exchange (ETDEWEB)

Roque, Jacinto Morales [Facultad de Quimica, Universidad Nacional Autonoma de Mexico, Mexico D.F. 04510 (Mexico); Pandiyan, T. [Facultad de Quimica, Universidad Nacional Autonoma de Mexico, Mexico D.F. 04510 (Mexico)], E-mail: pandiyan@servidor.unam.mx; Cruz, J. [Centro de Investigaciones Quimicas, Universidad Autonoma del Estado de Hidalgo, Unidad Universitaria, Km 4.5 Carretera Pachuca-Tulancingo, C.P. 42184 Pachuca-Hidalgo (Mexico); Garcia-Ochoa, E. [Centro de Investigacion en Corrosion, Universidad Autonoma de Campeche, Mexico, Av. Agustin Melgar s/n, Colonia Buenavista, San Francisco de Campeche, Cam. C.P. 24030 (Mexico)

2008-03-15

The corrosion inhibition properties of tris(benzimidazole-2-ylmethyl)amine (TBMA) were analyzed by DFT and electrochemical techniques such as polarization curves and electrochemical impedance spectroscopy (EIS). DFT results clearly show that TBMA posses corrosion inhibition properties by having a delocalization region (N{sub 1}=C{sub 2}=N{sub 3}) in the benzimidazole ring that gives up their {pi} electron density through its HOMO orbital to the metal LUMO to form a adsorption layer over the metallic surface; this has been proved by interacting the TBMA and its protonated structures with the surface of Fe{sub 13} cluster, showing that the protonated moiety adsorbs strongly on the iron surface than that of the neutral structure. Electrochemical impedance data demonstrate that the interface between the electrode and the TBMA solution decreases the charge capacitance and simultaneously increases the function of the charge/discharge of the interface, facilitating the formation of adsorption layer over the iron surface.

DFT and electrochemical studies of tris(benzimidazole-2-ylmethyl)amine as an efficient corrosion inhibitor for carbon steel surface

International Nuclear Information System (INIS)

Roque, Jacinto Morales; Pandiyan, T.; Cruz, J.; Garcia-Ochoa, E.

2008-01-01

The corrosion inhibition properties of tris(benzimidazole-2-ylmethyl)amine (TBMA) were analyzed by DFT and electrochemical techniques such as polarization curves and electrochemical impedance spectroscopy (EIS). DFT results clearly show that TBMA posses corrosion inhibition properties by having a delocalization region (N 1 =C 2 =N 3 ) in the benzimidazole ring that gives up their π electron density through its HOMO orbital to the metal LUMO to form a adsorption layer over the metallic surface; this has been proved by interacting the TBMA and its protonated structures with the surface of Fe 13 cluster, showing that the protonated moiety adsorbs strongly on the iron surface than that of the neutral structure. Electrochemical impedance data demonstrate that the interface between the electrode and the TBMA solution decreases the charge capacitance and simultaneously increases the function of the charge/discharge of the interface, facilitating the formation of adsorption layer over the iron surface

Electrochemical Glucose Biosensor Based on Glucose Oxidase Displayed on Yeast Surface.

Science.gov (United States)

Wang, Hongwei; Lang, Qiaolin; Liang, Bo; Liu, Aihua

2015-01-01

The conventional enzyme-based biosensor requires chemical or physical immobilization of purified enzymes on electrode surface, which often results in loss of enzyme activity and/or fractions immobilized over time. It is also costly. A major advantage of yeast surface display is that it enables the direct utilization of whole cell catalysts with eukaryote-produced proteins being displayed on the cell surface, providing an economic alternative to traditional production of purified enzymes. Herein, we describe the details of the display of glucose oxidase (GOx) on yeast cell surface and its application in the development of electrochemical glucose sensor. In order to achieve a direct electrochemistry of GOx, the entire cell catalyst (yeast-GOx) was immobilized together with multiwalled carbon nanotubes on the electrode, which allowed sensitive and selective glucose detection.

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

Swift heavy ions induced surface modifications in Ag-polypyrrole composite films synthesized by an electrochemical route

International Nuclear Information System (INIS)

Kumar, Vijay; Ali, Yasir; Sharma, Kashma; Kumar, Vinod; Sonkawade, R.G.; Dhaliwal, A.S.; Swart, H.C.

2014-01-01

Highlights: • Two steps electrochemical synthesis for the fabrication of Ag-polypyrrole composite films. • Surface modifications by swift heavy ion beam. • SEM image shows the formation of craters and humps after irradiation. • Detailed structural analysis by Raman spectroscopy. - Abstract: The general aim of this work was to study the effects of swift heavy ions on the properties of electrochemically synthesized Ag-polypyrrole composite thin films. Initially, polypyrrole (PPy) films were electrochemically synthesized on indium tin oxide coated glass surfaces using a chronopotentiometery technique, at optimized process conditions. The prepared PPy films have functioned as working electrodes for the decoration of submicron Ag particles on the surface of the PPy films through a cyclicvoltammetry technique. Towards probing the effect of swift heavy ion irradiation on the structural and morphological properties, the composite films were subjected to a 40 MeV Li 3+ ion beam irradiation for various fluences (1 × 10 11 , 1 × 10 12 and 1 × 10 13 ions/cm 2 ). Comparative microstructural investigations were carried out after the different ion fluences using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy and micro-Raman spectroscopy techniques. Raman and SEM studies revealed that the structure of the films became disordered after irradiation. The SEM studies of irradiated composite films show significant changes in their surface morphologies. The surface was smoother at lower fluence but craters were observed at higher fluence

Swift heavy ions induced surface modifications in Ag-polypyrrole composite films synthesized by an electrochemical route

Energy Technology Data Exchange (ETDEWEB)

Kumar, Vijay, E-mail: vijays_phy@rediffmail.com [Department of Physics, University of the Free State, P.O. Box 339, Bloemfontein ZA 9300 (South Africa); Ali, Yasir [Department of Physics, Sant Longowal Institute of Engineering and Technology, Longowal, District Sangrur 148106, Punjab (India); Sharma, Kashma [Department of Physics, University of the Free State, P.O. Box 339, Bloemfontein ZA 9300 (South Africa); Department of Chemistry, Shoolini University of Biotechnology and Management Sciences, Solan 173212 (India); Kumar, Vinod [Department of Physics, University of the Free State, P.O. Box 339, Bloemfontein ZA 9300 (South Africa); Sonkawade, R.G. [Inter University Accelerator Center, Aruna Asif Ali Marg, New Delhi 110067 (India); Dhaliwal, A.S. [Department of Physics, Sant Longowal Institute of Engineering and Technology, Longowal, District Sangrur 148106, Punjab (India); Swart, H.C., E-mail: swarthc@ufs.ac.za [Department of Physics, University of the Free State, P.O. Box 339, Bloemfontein ZA 9300 (South Africa)

2014-03-15

Highlights: • Two steps electrochemical synthesis for the fabrication of Ag-polypyrrole composite films. • Surface modifications by swift heavy ion beam. • SEM image shows the formation of craters and humps after irradiation. • Detailed structural analysis by Raman spectroscopy. - Abstract: The general aim of this work was to study the effects of swift heavy ions on the properties of electrochemically synthesized Ag-polypyrrole composite thin films. Initially, polypyrrole (PPy) films were electrochemically synthesized on indium tin oxide coated glass surfaces using a chronopotentiometery technique, at optimized process conditions. The prepared PPy films have functioned as working electrodes for the decoration of submicron Ag particles on the surface of the PPy films through a cyclicvoltammetry technique. Towards probing the effect of swift heavy ion irradiation on the structural and morphological properties, the composite films were subjected to a 40 MeV Li{sup 3+} ion beam irradiation for various fluences (1 × 10{sup 11}, 1 × 10{sup 12} and 1 × 10{sup 13} ions/cm{sup 2}). Comparative microstructural investigations were carried out after the different ion fluences using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy and micro-Raman spectroscopy techniques. Raman and SEM studies revealed that the structure of the films became disordered after irradiation. The SEM studies of irradiated composite films show significant changes in their surface morphologies. The surface was smoother at lower fluence but craters were observed at higher fluence.

Electrochemical gate-controlled electron transport of redox-active single perylene bisimide molecular junctions

International Nuclear Information System (INIS)

Li, C; Mishchenko, A; Li, Z; Pobelov, I; Wandlowski, Th; Li, X Q; Wuerthner, F; Bagrets, A; Evers, F

2008-01-01

We report a scanning tunneling microscopy (STM) experiment in an electrochemical environment which studies a prototype molecular switch. The target molecules were perylene tetracarboxylic acid bisimides modified with pyridine (P-PBI) and methylthiol (T-PBI) linker groups and with bulky tert-butyl-phenoxy substituents in the bay area. At a fixed bias voltage, we can control the transport current through a symmetric molecular wire Au|P-PBI(T-PBI)|Au by variation of the electrochemical 'gate' potential. The current increases by up to two orders of magnitude. The conductances of the P-PBI junctions are typically a factor 3 larger than those of T-PBI. A theoretical analysis explains this effect as a consequence of shifting the lowest unoccupied perylene level (LUMO) in or out of the bias window when tuning the electrochemical gate potential VG. The difference in on/off ratios reflects the variation of hybridization of the LUMO with the electrode states with the anchor groups. I T -E S(T) curves of asymmetric molecular junctions formed between a bare Au STM tip and a T-PBI (P-PBI) modified Au(111) electrode in an aqueous electrolyte exhibit a pronounced maximum in the tunneling current at -0.740, which is close to the formal potential of the surface-confined molecules. The experimental data were explained by a sequential two-step electron transfer process

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

DEFF Research Database (Denmark)

Afshar, F. Norouzi; Ambat, R.; Kwakernaak, C.

2012-01-01

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 1wt% 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...

Electrochemical deposition on surface nanometric defects: Thermodynamics and grand canonical Monte Carlo simulations

International Nuclear Information System (INIS)

Luque, Noelia B.; Reinaudi, Luis; Serra, Pablo; Leiva, Ezequiel P.M.

2009-01-01

A thermodynamic analysis is performed on electrochemical metal deposition in the cavity of a foreign substrate. In particular, the deposition of Cu and Ag in nanometer-sized holes on Au(1 1 1) is studied by means of off-lattice atomistic Grand Canonical Monte Carlo simulations, using embedded atom method potentials. The present simulation conditions emulate experiments of electrochemical metal deposition in nanocavities, as performed in the literature. Depending on the system, remarkable differences are found in the way in which the defects are decorated, as well as in their energetics. When the interaction of the adsorbate atoms with the substrate is less favorable than the bulk interaction of the adsorbate, clusters are found that grow stepwise over the level of the surface. In the opposite case, the filling of the cavity occurs stepwise, without the occurrence of cluster growth above the surface level. The results of the simulations present a good qualitative agreement with experimental results from the literature

Electrochemical Cathodic Polarization, a Simplified Method That Can Modified and Increase the Biological Activity of Titanium Surfaces: A Systematic Review.

Directory of Open Access Journals (Sweden)

Jose Carlos Bernedo Alcazar

Full Text Available The cathodic polarization seems to be an electrochemical method capable of modifying and coat biomolecules on titanium surfaces, improving the surface activity and promoting better biological responses.The aim of the systematic review is to assess the scientific literature to evaluate the cellular response produced by treatment of titanium surfaces by applying the cathodic polarization technique.The literature search was performed in several databases including PubMed, Web of Science, Scopus, Science Direct, Scielo and EBSCO Host, until June 2016, with no limits used. Eligibility criteria were used and quality assessment was performed following slightly modified ARRIVE and SYRCLE guidelines for cellular studies and animal research.Thirteen studies accomplished the inclusion criteria and were considered in the review. The quality of reporting studies in animal models was low and for the in vitro studies it was high. The in vitro and in vivo results reported that the use of cathodic polarization promoted hydride surfaces, effective deposition, and adhesion of the coated biomolecules. In the experimental groups that used the electrochemical method, cellular viability, proliferation, adhesion, differentiation, or bone growth were better or comparable with the control groups.The use of the cathodic polarization method to modify titanium surfaces seems to be an interesting method that could produce active layers and consequently enhance cellular response, in vitro and in vivo animal model studies.

Surface-reconstructed Cu Electrode via a Facile Electrochemical Anodization-Reduction Process for Low Overpotential CO 2 reduction

KAUST Repository

Min, Shixiong

2017-03-21

A high-surface-area Cu electrode, fabricated by a simple electrochemical anodization-reduction method, exhibits high activity and selectivity for CO2 reduction at low overpotential in 0.1 M KHCO3 solution. A faradaic efficiency of 37% for HCOOH and 27% for CO production was achieved with the current density of 1.5 mA cm-2 at −0.64 V vs. RHE, much higher than that of polycrystalline Cu. The enhanced catalytic performance is a result of the formation of the high electrochemical active surface area and high density of preferred low-index facets.

Characterization of surface-modified LiMn2O4 cathode materials with indium tin oxide (ITO) coatings and their electrochemical performance

International Nuclear Information System (INIS)

Kim, Chang-Sam; Kwon, Soon-Ho; Yoon, Jong-Won

2014-01-01

Graphical abstract: -- Highlights: • Indium tin oxide (ITO) is used to modify the surface of LiMn 2 O 4 by a sol–gel method. • The surface-modified layer was observed at a scale of several nanometers on LiMn 2 O 4 . • The ITO-coated LiMn 2 O 4 shows better capacity retention at 30 and 55 °C than pristine LiMn 2 O 4 . -- Abstract: Indium tin oxide (ITO) is used to modify the surface of LiMn 2 O 4 by a sol–gel method in an attempt to improve its electrochemical performance at elevated temperatures. The surface-modified LiMn 2 O 4 is characterized via XRD, FE-SEM, TEM, Auger electron spectroscopy (AES) and inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The surface layer modified by substitution with indium was observed at a scale of several nanometers near the surface on LiMn 2 O 4 . The concentration of ITO for electrochemical performance was varied from 0.3 wt% to 0.8 wt%. The 0.5 wt% ITO coated LiMn 2 O 4 showed the best electrochemical performance. This enhancement in electrochemical performance is mainly attributed to the effect of the surface layer modified through ITO, which could suppress Mn dissolution and reduce the charge transfer resistance at the solid electrolyte interface

Mechanism of glucose electrochemical oxidation on gold surface

KAUST Repository

Pasta, Mauro; La Mantia, Fabio; Cui, Yi

2010-01-01

The complex oxidation of glucose at the surface of gold electrodes was studied in detail in different conditions of pH, buffer and halide concentration. As observed in previous studies, an oxidative current peak occurs during the cathodic sweep showing a highly linear dependence on glucose concentration, when other electrolyte conditions are unchanged. The effect of the different conditions on the intensity of this peak has stressed the limitations of the previously proposed mechanisms. A mechanism able to explain the presence of this oxidative peak was proposed. The mechanism takes into account ion-sorption and electrochemical adsorption of OH-, buffer species (K2HPO4/KH2PO4) and halides. © 2010 Elsevier Ltd. All rights reserved.

Mechanism of glucose electrochemical oxidation on gold surface

KAUST Repository

Pasta, Mauro

2010-08-01

The complex oxidation of glucose at the surface of gold electrodes was studied in detail in different conditions of pH, buffer and halide concentration. As observed in previous studies, an oxidative current peak occurs during the cathodic sweep showing a highly linear dependence on glucose concentration, when other electrolyte conditions are unchanged. The effect of the different conditions on the intensity of this peak has stressed the limitations of the previously proposed mechanisms. A mechanism able to explain the presence of this oxidative peak was proposed. The mechanism takes into account ion-sorption and electrochemical adsorption of OH-, buffer species (K2HPO4/KH2PO4) and halides. © 2010 Elsevier Ltd. All rights reserved.

Surface modification of titanium membrane by chemical vapor deposition and its electrochemical self-cleaning

Energy Technology Data Exchange (ETDEWEB)

Li, X.W., E-mail: lynnww@sohu.com [School of Electronic and Information Engieering, Tianjin university, Tianjin, 300072 (China); School of Electronics Information Engieering, Tianjin University of Technology, Tianjin, 300384 (China); Li, J.X. [Tianjin Polytechnic University, Tianjin 300160 (China); Gao, C.Y. [Chinese Peoples Armed Police Forces Academy, Langfang 065000 (China); Chang, M. [School of Electronic and Information Engieering, Tianjin university, Tianjin, 300072 (China); School of Electronics Information Engieering, Tianjin University of Technology, Tianjin, 300384 (China)

2011-10-15

Membrane separation is applied widely in many fields, while concentration polarization and membrane fouling, limiting its promotion and application greatly, are the bottlenecks in membrane application. Among which, membrane fouling is irreversible, membrane must be periodically cleaned or even replaced to restore permeability. Membrane cleaning has become one of Key issues in membrane separation areas. Considering incomparable electrochemical advantages of boron-doped diamond (BDD) film electrode over conventional electrode, a new composite membrane Ti/BDD, made by depositing CVD (chemical vapor deposition) boron-doped diamond film on titanium(Ti) membrane to modify porous titanium surface, that can be cleaned electrochemically is proposed. Feasibility of its preparation and application is discussed in this paper. Results shows that based on the unique electrochemical properties of diamond, cleaning level of this composite Ti/BDD membrane is significantly increased, making membrane life and efficiency improved prominently.

Surface modification of titanium membrane by chemical vapor deposition and its electrochemical self-cleaning

International Nuclear Information System (INIS)

Li, X.W.; Li, J.X.; Gao, C.Y.; Chang, M.

2011-01-01

Membrane separation is applied widely in many fields, while concentration polarization and membrane fouling, limiting its promotion and application greatly, are the bottlenecks in membrane application. Among which, membrane fouling is irreversible, membrane must be periodically cleaned or even replaced to restore permeability. Membrane cleaning has become one of Key issues in membrane separation areas. Considering incomparable electrochemical advantages of boron-doped diamond (BDD) film electrode over conventional electrode, a new composite membrane Ti/BDD, made by depositing CVD (chemical vapor deposition) boron-doped diamond film on titanium(Ti) membrane to modify porous titanium surface, that can be cleaned electrochemically is proposed. Feasibility of its preparation and application is discussed in this paper. Results shows that based on the unique electrochemical properties of diamond, cleaning level of this composite Ti/BDD membrane is significantly increased, making membrane life and efficiency improved prominently.

Silver deposition on titanium surface by electrochemical anodizing process reduces bacterial adhesion of Streptococcus sanguinis and Lactobacillus salivarius.

Science.gov (United States)

Godoy-Gallardo, Maria; Rodríguez-Hernández, Ana G; Delgado, Luis M; Manero, José M; Javier Gil, F; Rodríguez, Daniel

2015-10-01

The aim of this study was to determine the antibacterial properties of silver-doped titanium surfaces prepared with a novel electrochemical anodizing process. Titanium samples were anodized with a pulsed process in a solution of silver nitrate and sodium thiosulphate at room temperature with stirring. Samples were processed with different electrolyte concentrations and treatment cycles to improve silver deposition. Physicochemical properties were determined by X-ray photoelectron spectroscopy, contact angle measurements, white-light interferometry, and scanning electron microscopy. Cellular cytotoxicity in human fibroblasts was studied with lactate dehydrogenase assays. The in vitro effect of treated surfaces on two oral bacteria strains (Streptococcus sanguinis and Lactobacillus salivarius) was studied with viable bacterial adhesion measurements and growth curve assays. Nonparametric statistical Kruskal-Wallis and Mann-Whitney U-tests were used for multiple and paired comparisons, respectively. Post hoc Spearman's correlation tests were calculated to check the dependence between bacteria adhesion and surface properties. X-ray photoelectron spectroscopy results confirmed the presence of silver on treated samples and showed that treatments with higher silver nitrate concentration and more cycles increased the silver deposition on titanium surface. No negative effects in fibroblast cell viability were detected and a significant reduction on bacterial adhesion in vitro was achieved in silver-treated samples compared with control titanium. Silver deposition on titanium with a novel electrochemical anodizing process produced surfaces with significant antibacterial properties in vitro without negative effects on cell viability. © 2014 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

Controlled synthesis and electrochemical properties of vanadium ...

Indian Academy of Sciences (India)

Vanadium oxides (V3O7·H2O and VO2) with different morphologies have been selectively synthesized ... appeared at around 68 ◦C. Furthermore, the electrochemical properties of V3O7·H2O nanobelts, VO2(B) .... morphologies of shape-controlled orthorhombic V3O7·H2O ..... condition, as shown in figures S14i and j.

Surface modification and electrochemical properties of activated carbons for supercapacitor electrodes

Science.gov (United States)

Yang, Dan; Qiu, Wenmei; Xu, Jingcai; Han, Yanbing; Jin, Hongxiao; Jin, Dingfeng; Peng, Xiaoling; Hong, Bo; Li, Ji; Ge, Hongliang; Wang, Xinqing

2015-12-01

Modifications with different acids (HNO3, H2SO4, HCl and HF, respectively) were introduced to treat the activated carbons (ACs) surface. The microstructures and surface chemical properties were discussed by X-ray diffraction (XRD), thermogravimetric analysis (TGA), ASAP, Raman spectra and Fourier transform infrared (FTIR) spectra. The ACs electrode-based supercapacitors were assembled with 6 mol ṡ L-1 KOH electrolyte. The electrochemical properties were studied by galvanostatic charge-discharge and cyclic voltammetry. The results indicated that although the BET surface area of modified ACs decreased, the functional groups were introduced and the ash contents were reduced on the surface of ACs, receiving larger specific capacitance to initial AC. The specific capacitance of ACs modified with HCl, H2SO4, HF and HNO3 increased by 31.4%, 23%, 21% and 11.6%, respectively.

Electrochemical treatment of simulated sugar industrial effluent: Optimization and modeling using a response surface methodology

Directory of Open Access Journals (Sweden)

P. Asaithambi

2016-11-01

Full Text Available The removal of organic compounds from a simulated sugar industrial effluent was investigated through the electrochemical oxidation technique. Effect of various experimental parameters such as current density, concentration of electrolyte and flow rate in a batch electrochemical reactor was studied on the percentage of COD removal and power consumption. The electrochemical reactor performance was analyzed based on with and without recirculation of the effluent having constant inter-electrodes distance. It was found out that the percentage removal of COD increased with the increase of electrolyte concentration and current density. The maximum percentage removal of COD was achieved at 80.74% at a current density of 5 A/dm2 and 5 g/L of electrolyte concentration in the batch electrochemical reactor. The recirculation electrochemical reactor system parameters like current density, concentration of COD and flow rate were optimized using response surface methodology, while COD removal percents were maximized and power consumption minimized. It has been observed from the present analysis that the predicted values are in good agreement with the experimental data with a correlation coefficient of 0.9888.

The atomic force microscope as a mechano–electrochemical pen

Directory of Open Access Journals (Sweden)

Christian Obermair

2011-10-01

Full Text Available We demonstrate a method that allows the controlled writing of metallic patterns on the nanometer scale using the tip of an atomic force microscope (AFM as a “mechano–electrochemical pen”. In contrast to previous experiments, no voltage is applied between the AFM tip and the sample surface. Instead, a passivated sample surface is activated locally due to lateral forces between the AFM tip and the sample surface. In this way, the area of tip–sample interaction is narrowly limited by the mechanical contact between tip and sample, and well-defined metallic patterns can be written reproducibly. Nanoscale structures and lines of copper were deposited, and the line widths ranged between 5 nm and 80 nm, depending on the deposition parameters. A procedure for the sequential writing of metallic nanostructures is introduced, based on the understanding of the passivation process. The mechanism of this mechano–electrochemical writing technique is investigated, and the processes of site-selective surface depassivation, deposition, dissolution and repassivation of electrochemically deposited nanoscale metallic islands are studied in detail.

Block Copolymer Patterns as Templates for the Electrocatalyzed Deposition of Nanostructures on Electrodes and for the Generation of Surfaces of Controlled Wettability.

Science.gov (United States)

Chandaluri, Chanchayya Gupta; Pelossof, Gilad; Tel-Vered, Ran; Shenhar, Roy; Willner, Itamar

2016-01-20

ITO electrodes modified with a nanopatterned film of polystyrene-block-poly(2-vinylpyridine), PS-b-P2VP, where the P2VP domains are quaternized with iodomethane, are used for selective deposition of redox-active materials. Electrochemical studies (cyclic voltammetry, Faradaic impedance measurements) indicate that the PS domains insulate the conductive surface toward redox labels in solution. In turn, the quaternized P2VP domains electrostatically attract negatively charged redox labels solubilized in the electrolyte solution, resulting in an effective electron transfer between the electrode and the redox label. This phenomenon is implemented for the selective deposition of the electroactive Prussian blue on the nanopatterned surface and for the electrochemical deposition of Au nanoparticles, modified with a monolayer of p-aminothiophenol/2-mercaptoethanesulfonic acid, on the quaternized P2VP domains. The patterned Prussian blue-modified surface enables controlling the wettability properties by the content of the electrochemically deposited Prussian blue. Controlled wettability is unattainable with the homopolymer-modified surface, attesting to the role of the nanopattern.

Kinetic mechanism for modeling of electrochemical reactions.

Science.gov (United States)

Cervenka, Petr; Hrdlička, Jiří; Přibyl, Michal; Snita, Dalimil

2012-04-01

We propose a kinetic mechanism of electrochemical interactions. We assume fast formation and recombination of electron donors D- and acceptors A+ on electrode surfaces. These mediators are continuously formed in the electrode matter by thermal fluctuations. The mediators D- and A+, chemically equivalent to the electrode metal, enter electrochemical interactions on the electrode surfaces. Electrochemical dynamics and current-voltage characteristics of a selected electrochemical system are studied. Our results are in good qualitative agreement with those given by the classical Butler-Volmer kinetics. The proposed model can be used to study fast electrochemical processes in microsystems and nanosystems that are often out of the thermal equilibrium. Moreover, the kinetic mechanism operates only with the surface concentrations of chemical reactants and local electric potentials, which facilitates the study of electrochemical systems with indefinable bulk.

SURFACE PROPERTIES OF ELECTROCHEMICALLY REDUCED ...

African Journals Online (AJOL)

DJFLEX

A viscose rayon based activated carbon cloth (ACC) was electrochemically reduced ..... bath of liquid nitrogen at a temperature of 77 K. ... that above 59,400 c/g extent of oxidation, the ..... ACC react with aldehyde groups to produce ether.

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.

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.

DC-pulsed voltage electrochemical method based on duty cycle self-control for producing TERS gold tips

International Nuclear Information System (INIS)

Vasilchenko, V E; Kharintsev, S S; Salakhov, M Kh

2013-01-01

This paper presents a modified dc-pulsed low voltage electrochemical method in which a duty cycle is self tuned while etching. A higher yield of gold tips suitable for performing tip-enhanced Raman scattering (TERS) measurements is demonstrated. The improvement is caused by the self-control of the etching rate along the full surface of the tip. A capability of the gold tips to enhance a Raman signal is exemplified by TERS spectroscopy of single walled carbon nanotubes bundle, sulfur and vanadium oxide

Preparation of anti-adhesion surfaces on aluminium substrates of rubber plastic moulds using a coupling method of liquid plasma and electrochemical machining

Science.gov (United States)

Meng, Jianbing; Dong, Xiaojuan; Wei, Xiuting; Yin, Zhanmin

2014-03-01

Hard anti-adhesion surfaces, with low roughness and wear resistance, on aluminium substrates of rubber plastic moulds were fabricated via a new coupling method of liquid plasma and electrochemical machining. With the aid of liquid plasma thermal polishing and electrochemical anodic dissolution, micro/nano-scale binary structures were prepared as the base of the anti-adhesion surfaces. The anti-adhesion behaviours of the resulting aluminium surfaces were analysed by a surface roughness measuring instrument, a scanning electron microscope (SEM), a Fourier-transform infrared spectrophotometer (FTIR), an X-ray diffractometer (XRD), an optical contact angle meter, a digital Vickers micro-hardness (Hv) tester, and electronic universal testing. The results show that, after the liquid plasma and electrochemical machining, micro/nano-scale binary structures composed of micro-scale pits and nano-scale elongated boss structures were present on the sample surfaces. As a result, the anti-adhesion surfaces fabricated by the above coupling method have good anti-adhesion properties, better wear resistance and lower roughness.

Preparation of anti-adhesion surfaces on aluminium substrates of rubber plastic moulds using a coupling method of liquid plasma and electrochemical machining

Directory of Open Access Journals (Sweden)

Jianbing Meng

2014-02-01

Full Text Available Hard anti-adhesion surfaces, with low roughness and wear resistance, on aluminium substrates of rubber plastic moulds were fabricated via a new coupling method of liquid plasma and electrochemical machining. With the aid of liquid plasma thermal polishing and electrochemical anodic dissolution, micro/nano-scale binary structures were prepared as the base of the anti-adhesion surfaces. The anti-adhesion behaviours of the resulting aluminium surfaces were analysed by a surface roughness measuring instrument, a scanning electron microscope (SEM, a Fourier-transform infrared spectrophotometer (FTIR, an X-ray diffractometer (XRD, an optical contact angle meter, a digital Vickers micro-hardness (Hv tester, and electronic universal testing. The results show that, after the liquid plasma and electrochemical machining, micro/nano-scale binary structures composed of micro-scale pits and nano-scale elongated boss structures were present on the sample surfaces. As a result, the anti-adhesion surfaces fabricated by the above coupling method have good anti-adhesion properties, better wear resistance and lower roughness.

Preparation of anti-adhesion surfaces on aluminium substrates of rubber plastic moulds using a coupling method of liquid plasma and electrochemical machining

Energy Technology Data Exchange (ETDEWEB)

Meng, Jianbing, E-mail: jianbingmeng@126.com; Dong, Xiaojuan; Wei, Xiuting; Yin, Zhanmin [School of Mechanical Engineering, Shandong University of Technology, Zibo, 255049 (China)

2014-03-15

Hard anti-adhesion surfaces, with low roughness and wear resistance, on aluminium substrates of rubber plastic moulds were fabricated via a new coupling method of liquid plasma and electrochemical machining. With the aid of liquid plasma thermal polishing and electrochemical anodic dissolution, micro/nano-scale binary structures were prepared as the base of the anti-adhesion surfaces. The anti-adhesion behaviours of the resulting aluminium surfaces were analysed by a surface roughness measuring instrument, a scanning electron microscope (SEM), a Fourier-transform infrared spectrophotometer (FTIR), an X-ray diffractometer (XRD), an optical contact angle meter, a digital Vickers micro-hardness (Hv) tester, and electronic universal testing. The results show that, after the liquid plasma and electrochemical machining, micro/nano-scale binary structures composed of micro-scale pits and nano-scale elongated boss structures were present on the sample surfaces. As a result, the anti-adhesion surfaces fabricated by the above coupling method have good anti-adhesion properties, better wear resistance and lower roughness.

Engineering the Surface/Interface Structures of Titanium Dioxide Micro and Nano Architectures towards Environmental and Electrochemical Applications

DEFF Research Database (Denmark)

Wang, Xiaoliang; Zhao, Yanyan; Mølhave, Kristian

2017-01-01

advances in the surface and interface engineering and applications in environmental and electrochemical applications. We analyze the advantages of surface/interface engineered TiO₂ micro and nano structures, and present the principles and growth mechanisms of TiO₂ nanostructures via different strategies...

Effect of surface states on the electrochemical behaviour of single crystal n-ZnSe photoelectrode

International Nuclear Information System (INIS)

El-Dessouki, M.S.

1987-10-01

Surface Photovoltage Spectroscopy (SPS) technique has been used to detect the surface states of ZnSe (110) surfaces. Aqueous electrolyte/ZnSe junction has been electrochemically investigated in dark and under illumination. The effect of surface states on the kinetics of charge transfer through the semiconductor-electrolyte (S/E) junction has been discussed. The low leakage and photocurrents measured by the application of DC bias were referred to the blocking nature of S/E interface, in which the localized and induced surface states play an important role. (author). 19 refs, 4 figs

Noncovalent Pi-Pi Stacking at the Carbon-Electrolyte Interface: Controlling the Voltage Window of Electrochemical Supercapacitors.

Science.gov (United States)

Li, Mengya; Westover, Andrew S; Carter, Rachel; Oakes, Landon; Muralidharan, Nitin; Boire, Timothy C; Sung, Hak-Joon; Pint, Cary L

2016-08-03

A key parameter in the operation of an electrochemical double-layer capacitor is the voltage window, which dictates the device energy density and power density. Here we demonstrate experimental evidence that π-π stacking at a carbon-ionic liquid interface can modify the operation voltage of a supercapacitor device by up to 30%, and this can be recovered by steric hindrance at the electrode-electrolyte interface introduced by poly(ethylene oxide) polymer electrolyte additives. This observation is supported by Raman spectroscopy, electrochemical impedance spectroscopy, and differential scanning calorimetry that each independently elucidates the signature of π-π stacking between imidazole groups in the ionic liquid and the carbon surface and the role this plays to lower the energy barrier for charge transfer at the electrode-electrolyte interface. This effect is further observed universally across two separate ionic liquid electrolyte systems and is validated by control experiments showing an invariant electrochemical window in the absence of a carbon-ionic liquid electrode-electrolyte interface. As interfacial or noncovalent interactions are usually neglected in the mechanistic picture of double-layer capacitors, this work highlights the importance of understanding chemical properties at supercapacitor interfaces to engineer voltage and energy capability.

Electrochemical machining of internal built-up surfaces of large-sized vessels for nuclear power plants

Energy Technology Data Exchange (ETDEWEB)

Ryabchenko, N N; Pulin, V Ya [Vsesoyuznyj Proektno-Tekhnologicheskij Inst. Atomnogo Mashinostroeniya i Kotlostroeniya, Rostov-na-Donu (USSR)

1977-01-01

Electrochemical machining (ECM) has been employed for finishing of mechanically processed inner surfaces of large lateral parts of construction bodies with welded 0Kh18N10T steel overlayer. The finishing technology developed reduces the surface roughness from 10 mcm to the standard 2.5 mcm at the efficiency of machining of 2-4 m/sup 2/ per hour.

Microfluidic electrochemical device and process for chemical imaging and electrochemical analysis at the electrode-liquid interface in-situ

Science.gov (United States)

Yu, Xiao-Ying; Liu, Bingwen; Yang, Li; Zhu, Zihua; Marshall, Matthew J.

2016-03-01

A microfluidic electrochemical device and process are detailed that provide chemical imaging and electrochemical analysis under vacuum at the surface of the electrode-sample or electrode-liquid interface in-situ. The electrochemical device allows investigation of various surface layers including diffuse layers at selected depths populated with, e.g., adsorbed molecules in which chemical transformation in electrolyte solutions occurs.

Novel method for controllable fabrication of a superhydrophobic CuO surface on AZ91D magnesium alloy.

Science.gov (United States)

She, Zuxin; Li, Qing; Wang, Zhongwei; Li, Longqin; Chen, Funan; Zhou, Juncen

2012-08-01

A novel method for controllable fabrication of a superhydrophobic CuO surface on AZ91D magnesium alloy is reported in this paper. Hierarchical structure composed of micro/nano-featherlike CuO was obtained by electrodeposition of Cu-Zn alloy coating and subsequently an electrochemical anodic treatment in alkaline solution. After modification with lauric acid, the surface became hydrophobicity/superhydrophobicity. The formation of featherlike CuO structures was controllable by varying the coating composition. By applying SEM, ICP-AES, and water contact angle analysis, the effects of coating composition on the surface morphology and hydrophobicity of the as-prepared surfaces were detailedly studied. The results indicated that at the optimal condition, the surface showed a good superhydrophobicity with a water contact angle as high as 155.5 ± 1.3° and a sliding angle as low as about 3°. Possible growth mechanism of featherlike CuO hierarchical structure was discussed. Additionally, the anticorrosion effect of the superhydrophobic surface was studied by potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) measurements. The interface model for anticorrosion mechanism of superhydrophobic surface in corrosive medium was proposed. Besides, the mechanical stability test indicated that the resulting superhydrophobic surfaces have good mechanical stability.

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.

Disposable screen printed graphite electrode for the direct electrochemical determination of ibuprofen in surface water

KAUST Repository

Amin, Sidra; Soomro, M. Tahir; Memon, Najma; Solangi, Amber R.; Sirajuddin; Qureshi, Tahira; Behzad, Ali Reza

2014-01-01

The potential of square wave voltammetry (SWV) for the determination of ibuprofen in aqueous solution, applying baseline correction, is reported. A screen printed graphite electrodes (SPGEs), especially pretreated for this purpose, were used to investigate the electrochemical oxidation and detection of ibuprofen. After optimization of SWV parameters, measurements were carried out at 200 Hz modulation frequency, 4 mV step potential and 40 mV pulse amplitude for the determination of ibuprofen. The surfaces of both untreated and pretreated SPGEs were characterized by scanning electron microscopy (SEM) and electrochemical impedance spectroscopy (EIS). The electro-catalytic properties of both the electrodes were correlated with the surface treatment. The pretreated screen printed graphite electrode exhibited a high sensitivity toward ibuprofen even in low concentration. The developed method was found rapid, cost-effective and reproducible for in-field ibuprofen detection.

Disposable screen printed graphite electrode for the direct electrochemical determination of ibuprofen in surface water

KAUST Repository

Amin, Sidra

2014-08-01

The potential of square wave voltammetry (SWV) for the determination of ibuprofen in aqueous solution, applying baseline correction, is reported. A screen printed graphite electrodes (SPGEs), especially pretreated for this purpose, were used to investigate the electrochemical oxidation and detection of ibuprofen. After optimization of SWV parameters, measurements were carried out at 200 Hz modulation frequency, 4 mV step potential and 40 mV pulse amplitude for the determination of ibuprofen. The surfaces of both untreated and pretreated SPGEs were characterized by scanning electron microscopy (SEM) and electrochemical impedance spectroscopy (EIS). The electro-catalytic properties of both the electrodes were correlated with the surface treatment. The pretreated screen printed graphite electrode exhibited a high sensitivity toward ibuprofen even in low concentration. The developed method was found rapid, cost-effective and reproducible for in-field ibuprofen detection.

Electrochemical and materials aspects of tribocorrosion systems

International Nuclear Information System (INIS)

Landolt, D

2006-01-01

Tribocorrosion involves mechanical and chemical/electrochemical interactions between surfaces in relative motion in the presence of a corrosive environment. Tribocorrosion phenomena are encountered in many technological areas where they cause damage to installations, machines and devices. Often tribocorrosion damage is a problem for safety or for human health. In other applications tribocorrosion phenomena are put to good use in manufacturing. The chemo-mechanical mechanisms of tribocorrosion are still incompletely understood, they involve the properties of contacting material surfaces, the mechanics of the contact and the corrosion conditions. Electrochemical methods are widely used for the study of tribocorrosion reactions. To yield information about synergistic and antagonistic mechanisms they must be applied in situ under strictly controlled mechanical conditions, using materials with well-characterized surface properties. Recent progress in modelling and understanding of tribocorrosion systems is discussed and some challenges and opportunities for future research are identified

Enzyme-Gelatin Electrochemical Biosensors: Scaling Down

Directory of Open Access Journals (Sweden)

Hendrik A. Heering

2012-03-01

Full Text Available In this article we investigate the possibility of scaling down enzyme-gelatin modified electrodes by spin coating the enzyme-gelatin layer. Special attention is given to the electrochemical behavior of the selected enzymes inside the gelatin matrix. A glassy carbon electrode was used as a substrate to immobilize, in the first instance, horse heart cytochrome c (HHC in a gelatin matrix. Both a drop dried and a spin coated layer was prepared. On scaling down, a transition from diffusion controlled reactions towards adsorption controlled reactions is observed. Compared to a drop dried electrode, a spin coated electrode showed a more stable electrochemical behavior. Next to HHC, we also incorporated catalase in a spin coated gelatin matrix immobilized on a glassy carbon electrode. By spincoating, highly uniform sub micrometer layers of biocompatible matrices can be constructed. A full electrochemical study and characterization of the modified surfaces has been carried out. It was clear that in the case of catalase, gluteraldehyde addition was needed to prevent leaking of the catalase from the gelatin matrix.

A multimodal optical and electrochemical device for monitoring surface reactions: redox active surfaces in porous silicon Rugate filters.

Science.gov (United States)

Ciampi, Simone; Guan, Bin; Darwish, Nadim A; Zhu, Ying; Reece, Peter J; Gooding, J Justin

2012-12-21

Herein, mesoporous silicon (PSi) is configured as a single sensing device that has dual readouts; as a photonic crystal sensor in a Rugate filter configuration, and as a high surface area porous electrode. The as-prepared PSi is chemically modified to provide it with stability in aqueous media and to allow for the subsequent coupling of chemical species, such as via Cu(I)-catalyzed cycloaddition reactions between 1-alkynes and azides ("click" reactions). The utility of the bimodal capabilities of the PSi sensor for monitoring surface coupling procedures is demonstrated by the covalent coupling of a ferrocene derivative, as well as by demonstrating ligand-exchange reactions (LER) at the PSi surface. Both types of reactions were monitored through optical reflectivity measurements, as well as electrochemically via the oxidation/reduction of the surface tethered redox species.

Electrochemical tuning of optical properties of graphitic quantum dots

International Nuclear Information System (INIS)

Ge, Juan; Li, Yan; Zhang, Bo-Ping; Ma, Ning; Wang, Jun; Pu, Chang; Xiang, Ying-Chang

2015-01-01

Graphitic quantum dots (GQDs), as a new class of quantum dots, possess unique properties. Among the various reported approaches for their fabrication, electrochemical method possesses numerous advantages compared with others. In particular, the formation process of the GQDs could be precisely controlled by this method through adjusting the electrochemical parameters and environment. In this study, GQDs with multi-color fluorescence (FL) were obtained by this method through tuning only the applied potential window of cycling voltammetry. The luminescence mechanism of those GQDs was discussed and explained by the ultraviolet (UV)–visible, photoluminescence (PL), and photoluminescence excitation (PLE) spectra. The influence of the applied potential window on the PL properties of GQDs and the relationship between the degree of surface oxidation and PL properties were also investigated. - Highlights: • We produced the graphite quantum dots (GQDs) by an electrochemical method. • We changed the applied potentials of cycling voltammetry (CV). • Varying of applied potentials changed surface oxygen-containing groups of GQDs. • Higher surface oxidation degree resulted in the red-shift of PL spectra

Surface Initiated Polymerizations via e-ATRP in Pure Water

Directory of Open Access Journals (Sweden)

Seyed Schwan Hosseiny

2013-10-01

Full Text Available Here we describe the combined process of surface modification with electrochemical atom transfer radical polymerization (e-ATRP initiated from the surface of a modified gold-electrode in a pure aqueous solution without any additional supporting electrolyte. This approach allows for a very controlled growth of the polymer chains leading towards a steady increase in film thickness. Electrochemical quartz crystal microbalance displayed a highly regular increase in surface confined mass only after the addition of the pre-copper catalyst which is reduced in situ and transformed into the catalyst. Even after isolation and washing of the modified electrode surface, reinitiation was achieved with retention of the controlled electrochemical ATRP reaction. This reinitiation after isolation proves the livingness of the polymerization. This approach has interesting potential for smart thin film materials and offers also the possibility of post-modification via additional electrochemical induced reactions.

Electrochemically shape-controlled synthesis in deep eutectic solvents of Pt nanoflowers with enhanced activity for ethanol oxidation

International Nuclear Information System (INIS)

Wei Lu; Fan Youjun; Wang Honghui; Tian Na; Zhou Zhiyou; Sun Shigang

2012-01-01

Highlights: ► The electrochemically shape-controlled synthesis in deep eutectic solvents (DESs) has been applied to produce the uniform Pt nanoflowers with sharp single crystal petals and high density of atomic steps. ► The as-prepared Pt nanoflowers exhibit higher electrocatalytic activity and stability than commercial Pt black catalyst toward ethanol electrooxidation. ► The growth of Pt nanoflowers in DESs by the simple electrochemical route is straightforward and controllable in terms of nanoflowers’ shape and size. - Abstract: The electrochemically shape-controlled synthesis in deep eutectic solvents (DESs) has been applied to produce the electrocatalyst of Pt nanoflowers. The uniform Pt nanoflowers with sharp single crystal petals and high density of atomic steps were characterized by SEM, TEM, XRD, XPS and electrochemical tests. The results illustrated that the as-prepared Pt nanoflowers exhibit higher electrocatalytic activity and stability than commercial Pt black catalyst toward ethanol electrooxidation. The growth of Pt nanoflowers in DESs by the simple electrochemical route is straightforward and controllable in terms of nanoflowers’ shape and size, which can be applied in shape-controlled synthesis of other noble metal nanoparticles with high catalytic activity.

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.

The impact of surface composition on Tafel kinetics leading to enhanced electrochemical insertion of hydrogen in palladium

Science.gov (United States)

Dmitriyeva, Olga; Hamm, Steven C.; Knies, David L.; Cantwell, Richard; McConnell, Matt

2018-05-01

Our previous work experimentally demonstrated the enhancement of electrochemical hydrogen insertion into palladium by modifying the chemical composition of the cathode surface with Pb, Pt and Bi, referred to as surface promoters. The experiment demonstrated that an optimal combination of the surface promoters led to an increase in hydrogen fugacity of more than three orders of magnitude, while maintaining the same current density. This manuscript discusses the application of Density Functional Theory (DFT) to elucidate the thermodynamics and kinetics of observed enhancement of electrochemical hydrogen insertion into palladium. We present theoretical simulations that: (1) establish the elevation of hydrogen's chemical potential on Pb and Bi surfaces to enhance hydrogen insertion, (2) confirm the increase of a Tafel activation barrier that results in a decrease of the reaction rate at the given hydrogen overpotential, and (3) explain why the surface promoter's coverage needs to be non-uniform, namely to allow hydrogen insertion into palladium bulk while simultaneously locking hydrogen below the surface (the corking effect). The discussed DFT-based method can be used for efficient scanning of different material configurations to design a highly effective hydrogen storage system.

The electrochemical behavior and surface structure of titanium electrodes modified by ion beams

International Nuclear Information System (INIS)

Huang, G.F.; Xie, Z.; Huang, W.Q.; Yang, S.B.; Zhao, L.H.

2004-01-01

Industrial grade titanium modified by ion implantation and sputtering was used as electrodes. The effect of ion beam modification on the electrochemical behavior and surface structure of electrodes was investigated. Also discussed is the hydrogen evolution process of the electrode in acidic solution. Several ions such as Fe + , C + , W + , Ni + and others, were implanted into the electrode. The electrochemical tests were carried out in 1N H 2 SO 4 solution at 30±1 deg. C. The electrode potential was measured versus a saturate calomel electrode as a function of immersion time. The cathodic polarization curves were measured by the stable potential static method. The surface layer composition and the chemical state of the electrodes were also investigated by Auger electron spectrometer (AES) and X-ray photoelectron spectroscopy (XPS) technique. The results show that: (1) the stability of modified electrodes depends on the active elements introduced by ion implantation and sputtering deposition. (2) The hydrogen evolution activity of industrial grade titanium may be improved greatly by ion beam modification. (3) Ion beam modification changed the composition and the surface state of electrodes over a certain depth range and forms an activity layer having catalytic hydrogen evolution, which inhibited the absorption of hydrogen and formation of titanium hydride. Thus promoted hydrogen evolution and improved the hydrogen evolution catalytic activity in industrial grade titanium

Template-Based Electrochemically Controlled Growth of Segmented Multimetal Nanorods

Directory of Open Access Journals (Sweden)

Mee Rahn Kim

2010-01-01

Full Text Available Multisegmented one-dimensional nanostructures composed of gold, copper, and nickel have been fabricated by depositing metals electrochemically in the pores of anodic aluminum oxide (AAO templates. The electrodeposition process has been carried out using a direct current in a two-electrode electrochemical cell, where a silver-evaporated AAO membrane and a platinum plate have served as a working electrode and a counter electrode, respectively. The striped multimetal rods with an average diameter of about 300 nm have tunable lengths ranging from a few hundred nanometers to a few micrometers. The lengths and the sequence of metal segments in a striped rod can be tailored readily by controlling the durations of electrodeposition and the order of electroplating solutions, respectively.

Controlling the Adhesion of Superhydrophobic Surfaces Using Electrolyte Jet Machining Techniques

Science.gov (United States)

Yang, Xiaolong; Liu, Xin; Lu, Yao; Zhou, Shining; Gao, Mingqian; Song, Jinlong; Xu, Wenji

2016-01-01

Patterns with controllable adhesion on superhydrophobic areas have various biomedical and chemical applications. Electrolyte jet machining technique (EJM), an electrochemical machining method, was firstly exploited in constructing dimples with various profiles on the superhydrophobic Al alloy surface using different processing parameters. Sliding angles of water droplets on those dimples firstly increased and then stabilized at a certain value with the increase of the processing time or the applied voltages of the EJM, indicating that surfaces with different adhesion force could be obtained by regulating the processing parameters. The contact angle hysteresis and the adhesion force that restricts the droplet from sliding off were investigated through experiments. The results show that the adhesion force could be well described using the classical Furmidge equation. On account of this controllable adhesion force, water droplets could either be firmly pinned to the surface, forming various patterns or slide off at designed tilting angles at specified positions on a superhydrophobic surface. Such dimples on superhydrophopbic surfaces can be applied in water harvesting, biochemical analysis and lab-on-chip devices. PMID:27046771

Correlations between electrochemical activity and heterogeneous catalysis for hydrogen dissociation on platinum

Energy Technology Data Exchange (ETDEWEB)

Ross, P N; Stonehart, P [Pratt and Whitney Aircraft, Middletown, Conn. (USA)

1975-02-01

Hydrogen-deuterium exchange rates on platinum surfaces have been compared to equivalent hydrogen molecule and adsorbed hydrogen atom electrochemical oxidation rates on the same surfaces. Over a temperature range of 293 to 360/sup 0/K the first order rate constants for H/sub 2/-D/sub 2/ exchange and hydrogen molecule electrochemical oxidation are the same, showing that the absorption-dissociation reaction (TAFEL, BONHOEFFER-FARKAS) is rate controlling. The rate of oxidation of the adsorbed hydrogen atom reaction involving electron transfer (VOLMER) is an order of magnitude larger.

Synthesis of Ni(OH)2 Nanoflakes Through a Novel Ion Diffusion Method Controlled by Ion Exchange Membrane and Electrochemical Supercapacitive Properties

International Nuclear Information System (INIS)

Zhao, Jiangshan; Zhang, Qiang

2015-01-01

Highlights: • We synthesized β-Ni(OH) 2 nanoflakes through a novel ion diffusion method. • The possible formation mechanism of the Ni(OH) 2 nanoflakes was discussed. • The temperature influence on growth of Ni(OH) 2 nanocrystals and its subsequent effect on electrochemical supercapacitive properties were examined. • The β-Ni(OH) 2 nanoflakes prepared at 50 °C for 12 h exhibits the highest specific capacitance of 2102 F g −1 . - Abstract: A novel method, ion diffusion method controlled by ion exchange membrane was reported for the synthesis of Ni(OH) 2 nanomaterials in the absence of any template or organic surfactant. The structure and morphology of as-prepared samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), BET specific surface area and pore size distribution analyzer. It can be observed that β-Ni(OH) 2 nanoflake-like structure was obtained, and the sheet size, thickness and pore size of as-prepared samples can be controlled by altering reaction time and reaction temperature. The BET specific surface area of Ni(OH) 2 nanomaterials obtained by this method can be up to 280.5 m 2 /g at 30 °C. The electrochemical supercapacitive properties of Ni(OH) 2 nanostructures have been investigated by cyclic voltammetry, chronopotentiometry and electrochemical impedance spectroscopy techniques. All these Ni(OH) 2 samples exhibit good capacity for electrochemical supercapacitor in KOH electrolyte. The flake nanostructures synthesized at 50 °C for 12 h exhibit a highest specific capacitance of 2102 F g −1 at a current density of 20 mA cm −2 within the potential range of 0.5 V and the Ni(OH) 2 sample retains 85.1% of the initial capacitance even after 1000 continuous charge–discharge cycles. The results indicate that ion diffusion method controlled by ion exchange membrane is a useful method for synthesizing inorganic nanomaterials.

Electrochemical quantification of the thermodynamic equilibrium constant of the tenoxicam-β-cyclodextrin inclusion complex formed on the surface of a poly-β cyclodextrin-modified carbon paste electrode

International Nuclear Information System (INIS)

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

2014-01-01

Graphical abstract: - Highlights: • A carbon paste electrode (CPE) was modified with a β-CD polymer. • Tenoxicam oxidation on the CPE/poly-β-CD was adsorption controlled. • Influence of pH, scan rate, angular velocity and concentration was evaluated. • Fittings of i-E plots were done considering an irreversible surface reaction. • Electrochemical evaluation of the surface inclusion constant is presented. - Abstract: In this work it is shown that when a carbon paste electrode, CPE, is modified with a β-cyclodextrin polymer, the tenoxicam oxidation becomes an adsorption controlled process due to formation of a surface inclusion complex with the β-CD molecules comprising the surface of the polymer. It was found that such surface inclusion complex can be formed independently of the tenoxicam predominant species, Tenox’, in the aqueous solution namely: H 2 Tenox + , HTenox or Tenox − , depending on the solution pH. The electrochemical quantification of the thermodynamic constant of the equilibrium Tenox’ + β-CD (polymer) = Tenox’-β-CD (polymer) was estimated as log K incl. = 4.26 ± 0.01. Furthermore, from the analyses of the experimental voltammograms according with Laviron's equation for an irreversible surface reaction [E. Laviron, J. Electroanal. Chem. 52 (1974) 355-393] it is shown that the surface concentration, Γ R , of tenoxicam increases as its concentration in solution does, reaching a maximum value of 1.51 × 10 −10 mol cm −2 at 64 μM

Electrochemical system for the control of oxigen atmospheres in UO2 sintering

International Nuclear Information System (INIS)

Caneiro, Alberto; Abriata, J.P.

1980-01-01

The behaviour of an electrochemical pump and of an oxygen sensor, allowing a precise control of the UO 2 stoichiometry in the preparation and analysis of gaseous mixtures of low oxygen contents is described. The correct functioning of the system can be tested by applying Faraday's law. The oxygen partial pressures can be continuously controlled by the sole varation of the current applied to the electrochemical pump. The partial pressure of the system is within the range between x 10 -1 atm and 10 -27 atm at 800 deg C. This system may be utilized for sintering experiments at a laboratory scale. (M.E.L) [es

In-situ polymerization of polyaniline on the surface of graphene oxide for high electrochemical capacitance

International Nuclear Information System (INIS)

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

2015-01-01

Conducting polymer polyaniline (PANI) was in-situ polymerized on the surface of graphene oxide (GO) to form PANI encapsulating GO nanocomposites. The morphology and microstructure were examined by scanning electron microscopy, X-ray diffraction and N 2 absorption/desorption analysis. Electrochemical properties were tested by cyclic voltammetry, galvanostatic charge/discharge cycles and electrochemical impedance spectroscopy. Experimental results showed that ethanol assisted the dispersion of GO in water and facilitated the diffusion of polymer monomers on GO. GO as a support material can provide sufficient reaction sites for the deposition of aniline to form the film-like GO/PANI composites. Capacitive performance illustrated that the in-situ polymerization of PANI on GO was effective in improving the specific capacitance and cycling stability. - Highlights: • GO/PANI nanocomposites were achieved by in-situ polymerization. • PANI was uniformly coated on the surface of GO with addition of ethanol. • GO/PANI show high specific capacitance and cycling stability

Investigation of Electrochemical Behaviour of Quercetin on the Modified Electrode Surfaces with Procaine and Aminophenyl in Non-Aquous Medium

Directory of Open Access Journals (Sweden)

Ibrahim Ender Mulazimoglu

2008-01-01

Full Text Available In this study, cyclic voltammetry and electrochemical ımpedance spectroscopy have been used to investigate the electrochemical behaviour of quercetin (3,3′,4′,5,7-pentahydroxyflavone on the procaine and aminophenyl modified electrode. The modification of procaine and aminophenyl binded electrode surface with quercetin was performed in +0,3/+2,8 V (for procaine and +0,4/+1,5 V (for aminophenyl potential range using 100 mV s-1 scanning rate having 10 cycle. A solution of 0.1 M tetrabutylammonium tetrafluoroborate in acetonitrile was used as a non-aquous solvent. For the modification process a solution of 1 mM quercetin in 0.1 M tetrabutylammonium tetrafluoroborate was used. In order to obtain these two surface, a solution of 1 mM procaine and 1 mM nitrophenyl diazonium salt in 0.1 M tetrabutylammonium tetrafluoroborate was used. By using these solutions bare glassy carbon electrode surface was modified. Nitrophenyl was reduced to amine group in 0.1 M HCl medium on the nitrophenyl modified glassy carbon elelctrode surface. Procaine modified glassy carbon electrode surface was quite electroactive. Although nitrophenyl modified glassy carbon elelctrode surface was electroinactive, it was activated by reducing nitro group into amine group. For the characterization of the modified surface 1 mM ferrocene in 0.1 M tetrabutylammonium tetrafluoroborate for cyclic voltammetry and 1 mM ferricyanide/ferrocyanide (1:1 mixture in 0,1 M KCl for electrochemical impedance spectroscopy were used.

Study on micro fabricated stainless steel surface to anti-biofouling using electrochemical fabrication

Science.gov (United States)

Hwang, Byeong Jun; Lee, Sung Ho

2017-12-01

Biofilm formed on the surface of the object by the microorganism resulting in fouling organisms. This has led to many problems in daily life, medicine, health and industrial community. In this study, we tried to prevent biofilm formation on the stainless steel (SS304) sheet surface with micro fabricated structure. After then forming the microscale colloid patterns on the surface of stainless steel by using an electrochemical etching forming a pattern by using a FeCl3 etching was further increase the surface roughness. Culturing the Pseudomonas aeruginosa on the stainless steel fabricated with a micro structure on the surface was observed a relationship between the surface roughness and the biological fouling of the micro structure. As a result, the stainless steel surface with a micro structure was confirmed to be the biological fouling occurs less. We expect to be able to solve the problems caused by biological fouling in various fields such as medicine, engineering, using this research.

Surface properties of nanostructured NiO undergoing electrochemical oxidation in 3-methoxy-propionitrile

International Nuclear Information System (INIS)

Bonomo, Matteo; Marrani, Andrea Giacomo; Novelli, Vittoria; Awais, Muhammad; Dowling, Denis P.; Vos, Johannes G.; Dini, Danilo

2017-01-01

Highlights: • NiO porous thin films were prepared via RDS technique. • NiO electrodes were characterized in a nitrile based electrochemical cell. • NiO electrodes were studied by means of XPS. • The XP spectra excluded the formation of phases other than NiO. • The presence of ClO 4 − as charge balancing species was evidenced. - Abstract: Nanostructured nickel oxide (NiO) was deposited in the configuration of thin film (thickness, l = 2–6 μm) onto fluorine-doped tin oxide (FTO) substrates via plasma-assisted rapid discharge sintering (RDS). Electrochemical cycling of RDS NiO in 3-methoxy-propionitrile (3-MPN) revealed two characteristic peaks of NiO oxidation which were associated to the surface-confined redox processes Ni(II) → Ni(III) and Ni(III) → Ni(IV). Grazing angle X-ray photoelectron spectroscopy (XPS) was conducted ex-situ on NiO electrodes in both pristine and oxidized states. Oxidized NiO samples for XPS experiments were obtained in the potentiostatic mode through the polarization of NiO at its two characteristic potentials of oxidation. The XPS analysis allowed to ascertain the electronic structure of the nanoporous NiO framework, and verify the adsorption of perchlorate and chloride anions onto NiO surface due to the compensation of the charge stored in oxidized NiO. XPS also revealed that the spectrum within the region characteristic of Ni 2p ionization does not vary considerably with the state of charge of the nickel centres. This finding is in evident contrast to what has been observed for the same system when it undergoes electrochemical oxidation in aqueous electrolyte.

Surface properties of nanostructured NiO undergoing electrochemical oxidation in 3-methoxy-propionitrile

Energy Technology Data Exchange (ETDEWEB)

Bonomo, Matteo [Department of Chemistry, University of Rome “La Sapienza”, Piazzale Aldo Moro 5, 00185 Rome (Italy); Marrani, Andrea Giacomo, E-mail: andrea.marrani@uniroma1.it [Department of Chemistry, University of Rome “La Sapienza”, Piazzale Aldo Moro 5, 00185 Rome (Italy); Novelli, Vittoria [Department of Chemistry, University of Rome “La Sapienza”, Piazzale Aldo Moro 5, 00185 Rome (Italy); Awais, Muhammad [Department of Industrial Engineering, “King Abdulaziz” University, Rabigh (Saudi Arabia); Solar Energy Conversion Strategic Research Cluster, University College Dublin (UCD), Belfield, Dublin 4 (Ireland); Dowling, Denis P. [Solar Energy Conversion Strategic Research Cluster, University College Dublin (UCD), Belfield, Dublin 4 (Ireland); School of Mechanical and Materials Engineering, University College Dublin (UCD), Belfield, Dublin 4 (Ireland); Vos, Johannes G. [School of Chemical Sciences, Dublin City University (DCU), Glasnevin, Dublin 9 (Ireland); Dini, Danilo [Department of Chemistry, University of Rome “La Sapienza”, Piazzale Aldo Moro 5, 00185 Rome (Italy); Solar Energy Conversion Strategic Research Cluster, University College Dublin (UCD), Belfield, Dublin 4 (Ireland)

2017-05-01

Highlights: • NiO porous thin films were prepared via RDS technique. • NiO electrodes were characterized in a nitrile based electrochemical cell. • NiO electrodes were studied by means of XPS. • The XP spectra excluded the formation of phases other than NiO. • The presence of ClO{sub 4}{sup −} as charge balancing species was evidenced. - Abstract: Nanostructured nickel oxide (NiO) was deposited in the configuration of thin film (thickness, l = 2–6 μm) onto fluorine-doped tin oxide (FTO) substrates via plasma-assisted rapid discharge sintering (RDS). Electrochemical cycling of RDS NiO in 3-methoxy-propionitrile (3-MPN) revealed two characteristic peaks of NiO oxidation which were associated to the surface-confined redox processes Ni(II) → Ni(III) and Ni(III) → Ni(IV). Grazing angle X-ray photoelectron spectroscopy (XPS) was conducted ex-situ on NiO electrodes in both pristine and oxidized states. Oxidized NiO samples for XPS experiments were obtained in the potentiostatic mode through the polarization of NiO at its two characteristic potentials of oxidation. The XPS analysis allowed to ascertain the electronic structure of the nanoporous NiO framework, and verify the adsorption of perchlorate and chloride anions onto NiO surface due to the compensation of the charge stored in oxidized NiO. XPS also revealed that the spectrum within the region characteristic of Ni 2p ionization does not vary considerably with the state of charge of the nickel centres. This finding is in evident contrast to what has been observed for the same system when it undergoes electrochemical oxidation in aqueous electrolyte.

In situ AFM investigation of electrochemically induced surface-initiated atom-transfer radical polymerization.

Science.gov (United States)

Li, Bin; Yu, Bo; Zhou, Feng

2013-02-12

Electrochemically induced surface-initiated atom-transfer radical polymerization is traced by in situ AFM technology for the first time, which allows visualization of the polymer growth process. It affords a fundamental insight into the surface morphology and growth mechanism simultaneously. Using this technique, the polymerization kinetics of two model monomers were studied, namely the anionic 3-sulfopropyl methacrylate potassium salt (SPMA) and the cationic 2-(metharyloyloxy)ethyltrimethylammonium chloride (METAC). The growth of METAC is significantly improved by screening the ammonium cations by the addition of ionic liquid electrolyte in aqueous solution. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Corrosion Behavior of Surface-Treated Implant Ti-6Al-4V by Electrochemical Polarization and Impedance Studies

Science.gov (United States)

Paul, Subir; Yadav, Kasturi

2011-04-01

Implant materials for orthopedic and heart surgical services demand a better corrosion resistance material than the presently used titanium alloys, where protective oxide layer breaks down on a prolonged stay in aqueous physiological human body, giving rise to localized corrosion of pitting, crevice, and fretting corrosion. A few surface treatments on Ti alloy, in the form of anodization, passivation, and thermal oxidation, followed by soaking in Hank solution have been found to be very effective in bringing down the corrosion rate as well as producing high corrosion resistance surface film as reflected from electrochemical polarization, cyclic polarization, and Electrochemical Impedance Spectroscopy (EIS) studies. The XRD study revealed the presence of various types of oxides along with anatase and rutile on the surface, giving rise to high corrosion resistance film. While surface treatment of passivation and thermal oxidation could reduce the corrosion rate by 1/5th, anodization in 0.3 M phosphoric acid at 16 V versus stainless steel cathode drastically brought down the corrosion rate by less than ten times. The mechanism of corrosion behavior and formation of different surface films is better understood from the determination of EIS parameters derived from the best-fit equivalent circuit.

Synthesis and electrochemical performance of surface-modified nano-sized core/shell tin particles for lithium ion batteries

International Nuclear Information System (INIS)

Schmuelling, Guido; Meyer, Hinrich-Wilhelm; Placke, Tobias; Winter, Martin; Oehl, Nikolas; Knipper, Martin; Kolny-Olesiak, Joanna; Plaggenborg, Thorsten; Parisi, Jürgen

2014-01-01

Tin is able to lithiate and delithiate reversibly with a high theoretical specific capacity, which makes it a promising candidate to supersede graphite as the state-of-the-art negative electrode material in lithium ion battery technology. Nevertheless, it still suffers from poor cycling stability and high irreversible capacities. In this contribution, we show the synthesis of three different nano-sized core/shell-type particles with crystalline tin cores and different amorphous surface shells consisting of SnO x and organic polymers. The spherical size and the surface shell can be tailored by adjusting the synthesis temperature and the polymer reagents in the synthesis, respectively. We determine the influence of the surface modifications with respect to the electrochemical performance and characterize the morphology, structure, and thermal properties of the nano-sized tin particles by means of high-resolution transmission electron microscopy, x-ray diffraction, and thermogravimetric analysis. The electrochemical performance is investigated by constant current charge/discharge cycling as well as cyclic voltammetry. (paper)

Engineering Cu surfaces for the electrocatalytic conversion of CO2: Controlling selectivity toward oxygenates and hydrocarbons

Science.gov (United States)

Hahn, Christopher; Hatsukade, Toru; Kim, Youn-Geun; Vailionis, Arturas; Baricuatro, Jack H.; Higgins, Drew C.; Nitopi, Stephanie A.; Soriaga, Manuel P.; Jaramillo, Thomas F.

2017-01-01

In this study we control the surface structure of Cu thin-film catalysts to probe the relationship between active sites and catalytic activity for the electroreduction of CO2 to fuels and chemicals. Here, we report physical vapor deposition of Cu thin films on large-format (∼6 cm2) single-crystal substrates, and confirm epitaxial growth in the , , and orientations using X-ray pole figures. To understand the relationship between the bulk and surface structures, in situ electrochemical scanning tunneling microscopy was conducted on Cu(100), (111), and (751) thin films. The studies revealed that Cu(100) and (111) have surface adlattices that are identical to the bulk structure, and that Cu(751) has a heterogeneous kinked surface with (110) terraces that is closely related to the bulk structure. Electrochemical CO2 reduction testing showed that whereas both Cu(100) and (751) thin films are more active and selective for C–C coupling than Cu(111), Cu(751) is the most selective for >2e− oxygenate formation at low overpotentials. Our results demonstrate that epitaxy can be used to grow single-crystal analogous materials as large-format electrodes that provide insights on controlling electrocatalytic activity and selectivity for this reaction. PMID:28533377

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 non-enzymatic glucose sensors

International Nuclear Information System (INIS)

Park, Sejin; Boo, Hankil; Chung, Taek Dong

2006-01-01

The electrochemical determination of glucose concentration without using enzyme is one of the dreams that many researchers have been trying to make come true. As new materials have been reported and more knowledge on detailed mechanism of glucose oxidation has been unveiled, the non-enzymatic glucose sensor keeps coming closer to practical applications. Recent reports strongly imply that this progress will be accelerated in 'nanoera'. This article reviews the history of unraveling the mechanism of direct electrochemical oxidation of glucose and making attempts to develop successful electrochemical glucose sensors. The electrochemical oxidation of glucose molecules involves complex processes of adsorption, electron transfer, and subsequent chemical rearrangement, which are combined with the surface reactions on the metal surfaces. The information about the direct oxidation of glucose on solid-state surfaces as well as new electrode materials will lead us to possible breakthroughs in designing the enzymeless glucose sensing devices that realize innovative and powerful detection. An example of those is to introduce nanoporous platinum as an electrode, on which glucose is oxidized electrochemically with remarkable sensitivity and selectivity. Better model of such glucose sensors is sought by summarizing and revisiting the previous reports on the electrochemistry of glucose itself and new electrode materials

Preparation of nitrogen-doped cotton stalk microporous activated carbon fiber electrodes with different surface area from hexamethylenetetramine-modified cotton stalk for electrochemical degradation of methylene blue

Directory of Open Access Journals (Sweden)

Kunquan Li

Full Text Available Cotton-stalk activated carbon fibers (CSCFs with controllable micropore area and nitrogen content were prepared as an efficient electrode from hexamethylenetetramine-modified cotton stalk by steam/ammonia activation. The influence of microporous area, nitrogen content, voltage and initial concentration on the electrical degradation efficiency of methylene blue (MB was evaluated by using CSCFs as anode. Results showed that the CSCF electrodes exhibited excellent MB electrochemical degradation ability including decolorization and COD removal. Increasing micropore surface area and nitrogen content of CSCF anode leaded to a corresponding increase in MB removal. The prepared CSCF-800-15-N, which has highest N content but lowest microporous area, attained the best degradation effect with 97% MB decolorization ratio for 5 mg/L MB at 12 V in 4 h, implying the doped nitrogen played a prominent role in improving the electrochemical degradation ability. The electrical degradation reaction was well described by first-order kinetics model. Overall, the aforesaid findings suggested that the nitrogen-doped CSCFs were potential electrode materials, and their electrical degradation abilities could be effectively enhanced by controlling the nitrogen content and micropore surface area. Keywords: Cotton stalk, Nitrogen content, Electrode, Surface area, Methylene blue

Controllable Electrochemical Synthesis of Reduced Graphene Oxide Thin-Film Constructed as Efficient Photoanode in Dye-Sensitized Solar Cells

Directory of Open Access Journals (Sweden)

Soon Weng Chong

2016-01-01

Full Text Available A controllable electrochemical synthesis to convert reduced graphene oxide (rGO from graphite flakes was introduced and investigated in detail. Electrochemical reduction was used to prepare rGO because of its cost effectiveness, environmental friendliness, and ability to produce rGO thin films in industrial scale. This study aimed to determine the optimum applied potential for the electrochemical reduction. An applied voltage of 15 V successfully formed a uniformly coated rGO thin film, which significantly promoted effective electron transfer within dye-sensitized solar cells (DSSCs. Thus, DSSC performance improved. However, rGO thin films formed in voltages below or exceeding 15 V resulted in poor DSSC performance. This behavior was due to poor electron transfer within the rGO thin films caused by poor uniformity. These results revealed that DSSC constructed using 15 V rGO thin film exhibited high efficiency (η = 1.5211% attributed to its higher surface uniformity than other samples. The addition of natural lemon juice (pH ~ 2.3 to the electrolyte accelerated the deposition and strengthened the adhesion of rGO thin film onto fluorine-doped tin oxide (FTO glasses.

Covalent attachment of pyridine-type molecules to glassy carbon surfaces by electrochemical reduction of in situ generated diazonium salts. Formation of ruthenium complexes on ligand-modified surfaces

International Nuclear Information System (INIS)

Yesildag, Ali; Ekinci, Duygu

2010-01-01

In this study, pyridine, quinoline and phenanthroline molecules were covalently bonded to glassy carbon (GC) electrode surfaces for the first time using the diazonium modification method. Then, the complexation ability of the modified films with ruthenium metal cations was investigated. The derivatization of GC surfaces with heteroaromatic molecules was achieved by electrochemical reduction of the corresponding in situ generated diazonium salts. X-ray photoelectron spectroscopy (XPS) was used to confirm the attachment of heteroaromatic molecules to the GC surfaces and to determine the surface concentration of the films. The barrier properties of the modified GC electrodes were studied in the presence of redox probes such as Fe(CN) 6 3- and Ru(NH 3 ) 6 3+ by cyclic voltammetry. Additionally, the presence of the resulting organometallic films on the surfaces was verified by XPS after the chemical transformation of the characterized ligand films to the ruthenium complex films. The electrochemical behavior of these films in acetonitrile solution was investigated using voltammetric methods, and the surface coverage of the organometallic films was determined from the reversible metal-based Ru(II)/Ru(III) oxidation waves.

Measurement of the specific surface area of loose copper deposit by electrochemical methods

Directory of Open Access Journals (Sweden)

E. A. Dolmatova

2016-07-01

Full Text Available In the work the surface area of the electrode with dispersed copper deposit obtained within 30 seconds was evaluated by techniques of chronopotentiometry (CPM and impedance spectroscopy. In method CPM the electrode surface available for measurement depends on the value of the polarizing current. At high currents during the transition time there is a change of surface relief that can not determine the full surface of loose deposit. The electrochemical impedance method is devoid of this shortcoming since the measurements are carried out in indifferent electrolyte in the absence of current. The area measured by the impedance is tens of times higher than the value obtained by chronopotentiometry. It is found that from a solution containing sulfuric acid the deposits form with a high specific surface area. Based on these data it was concluded that the method of impedance spectroscopy can be used to measure in situ the surface area of the dispersed copper deposits.

Morphological reason for enhancement of electrochemical double layer capacitances of various acetylene blacks by electrochemical polarization

International Nuclear Information System (INIS)

Kim, Taegon; Ham, Chulho; Rhee, Choong Kyun; Yoon, Seong-Ho; Tsuji, Masaharu; Mochida, Isao

2008-01-01

Enhancement of electrochemical capacitance and morphological variations of various acetylene blacks caused by electrochemical polarization are presented. Acetylene blacks of different mean particle diameters were modified by air-oxidation and heat treatment to diversify the morphologies of the acetylene blacks before electrochemical polarization. The various acetylene blacks were electrochemically oxidized at 1.6 V (vs. Ag/AgCl) for 10 s and the polarization step was repeated until the capacitance values did not change any longer. These polarization steps enhanced the capacitances of the acetylene blacks and the specific enhancement factors range from 2 to 5.5. Such an enhancement is strongly related to morphological modification as revealed by transmission electron microscopic observations. The electrochemical polarization resulted in formation of tiny graphene sheets on the wide graphitic carbon surfaces, which were most responsible for the observed capacitive enhancement. Although the pseudo-capacitance increased after polarization by forming oxygenated species on the surfaces, its contribution to the total capacitance was less than 10%. The mechanism of the formation of the tiny graphene sheets during the electrochemical oxidation is described schematically

On the changing electrochemical behaviour of boron-doped diamond surfaces with time after cathodic pre-treatments

International Nuclear Information System (INIS)

Salazar-Banda, Giancarlo R.; Andrade, Leonardo S.; Nascente, Pedro A.P.; Pizani, Paulo S.; Rocha-Filho, Romeu C.; Avaca, Luis A.

2006-01-01

The electrochemical response of the Fe(CN) 6 4-/3- redox couple on boron-doped diamond (BDD) electrodes immediately after a cathodic pre-treatment and as a function of time exposed to atmospheric conditions is reported here. After this pre-treatment the electrode exhibits a changing electrochemical behaviour, i.e., a loss of the reversibility for the Fe(CN) 6 4-/3- redox couple as a function of time. Raman spectra showed that neither important bulk structural differences nor significant changes in the sp 2 /sp 3 content are introduced into the BDD film by the cathodic pre-treatment indicating that H-terminated sites play an important role in the electrochemical response of the electrodes. Thus, the changing behaviour reflected by a progressive decrease of the electron transfer rate with time must be associated to a loss of superficial hydrogen due to oxidation by oxygen from the air, as confirmed by X-ray photoelectron spectroscopy (XPS) analysis. Moreover, it was also found that this changing electrochemical behaviour is inversely proportional to the doping level, suggesting that the boron content has a stabilizing effect on the H-terminated surface. These results point out the necessity of doing the cathodic pre-treatment just before the electrochemical experiments are carried out in order to ensure reliable and reproducible results

Application of a modified electrochemical system for surface decontamination of radioactive metal waste

International Nuclear Information System (INIS)

Lee, J.H.; Lim, Y.K.; Yang, H.Y.; Shin, S.W.; Song, M.J.

2003-01-01

Conventional and modified electrolytic decontamination experiments were performed in a solution of sodium sulfate for the decontamination of carbon steel as the simulated metal wastes which are generated in large amounts from nuclear power plants. The effect of reaction time, current density and concentration of electrolytes in the modified electrolytic decontamination system were examined to remove the surface contamination of the simulated radioactive metal wastes. As for the results of this research, the modified electrochemical decontamination process can decontaminate more effectively than the conventional decontamination process by applying different anode material which causes higher induced electro-motive forces. When 0.5 M sodium sulfate, 0.4 A/cm 2 current density and 30 minutes reaction time were applied in the modified process, a 16 μm thickness change that is expected to remove most surface contamination in radioactive metal wastes was achieved on carbon steel which is the main material of radioactive metal waste in nuclear power plants. The decontamination efficiency of metal waste showed similar results with the small and large lab-scale modified electrochemical system. The application of this modified electrolytic decontamination system is expected to play a considerable role for decontamination of radioactive metal waste in nuclear power plants in the near future. (author)

Surface properties of nanostructured NiO undergoing electrochemical oxidation in 3-methoxy-propionitrile

Science.gov (United States)

Bonomo, Matteo; Marrani, Andrea Giacomo; Novelli, Vittoria; Awais, Muhammad; Dowling, Denis P.; Vos, Johannes G.; Dini, Danilo

2017-05-01

Nanostructured nickel oxide (NiO) was deposited in the configuration of thin film (thickness, l = 2-6 μm) onto fluorine-doped tin oxide (FTO) substrates via plasma-assisted rapid discharge sintering (RDS). Electrochemical cycling of RDS NiO in 3-methoxy-propionitrile (3-MPN) revealed two characteristic peaks of NiO oxidation which were associated to the surface-confined redox processes Ni(II) → Ni(III) and Ni(III) → Ni(IV). Grazing angle X-ray photoelectron spectroscopy (XPS) was conducted ex-situ on NiO electrodes in both pristine and oxidized states. Oxidized NiO samples for XPS experiments were obtained in the potentiostatic mode through the polarization of NiO at its two characteristic potentials of oxidation. The XPS analysis allowed to ascertain the electronic structure of the nanoporous NiO framework, and verify the adsorption of perchlorate and chloride anions onto NiO surface due to the compensation of the charge stored in oxidized NiO. XPS also revealed that the spectrum within the region characteristic of Ni 2p ionization does not vary considerably with the state of charge of the nickel centres. This finding is in evident contrast to what has been observed for the same system when it undergoes electrochemical oxidation in aqueous electrolyte.

Plasma treatment of porous GaAs surface formed by electrochemical etching method: Characterization and properties

International Nuclear Information System (INIS)

Saloum, S.; Naddaf, M.

2010-01-01

Porous GaAs samples were formed by electrochemical anodic etching of Zn doped p-type GaAs (100) wafers at different etching parameters (time, mode of applied voltage or current and electrolyte). The effect of etching parameters and plasma surface treatment on the optical properties of the prepared sample has been investigated by using room temperature photoluminescence (PL), Raman spectroscopy and reflectance spectroscopic measurements in the range (400-800 nm). The surface morphological changes were studied by using atomic force microscope. (author)

Progress in electrochemical synthesis of magnetic iron oxide nanoparticles

International Nuclear Information System (INIS)

Ramimoghadam, Donya; Bagheri, Samira; Hamid, Sharifah Bee Abd

2014-01-01

Recently, magnetic iron oxide particles have been emerged as significant nanomaterials due to its extensive range of application in various fields. In this regard, synthesis of iron oxide nanoparticles with desirable properties and high potential applications are greatly demanded. Therefore, investigation on different iron oxide phases and their magnetic properties along with various commonly used synthetic techniques are remarked and thoroughly described in this review. Electrochemical synthesis as a newfound method with unique advantages is elaborated, followed by design approaches and key parameters to control the properties of the iron oxide nanoparticles. Additionally, since the dispersion of iron oxide nanoparticles is as important as its preparation, surface modification issue has been a serious challenge which is comprehensively discussed using different surfactants. Despite the advantages of the electrochemical synthesis method, this technique has been poorly studied and requires deep investigations on effectual parameters such as current density, pH, electrolyte concentration etc. - Highlights: • IONPs are applied in chemical industries, medicine, magnetic storage etc. • Electrochemical synthesis (EC) is convenient, eco-friendly, selective and low-cost. • EC key factors are current density, pH, electrolyte concentration, electrode type. • Organic, inorganic and biological materials can be used to modify IONPs’ surface. • The physicochemical properties of IONPs can be controlled by adding surfactants

Engineering the Surface/Interface Structures of Titanium Dioxide Micro and Nano Architectures towards Environmental and Electrochemical Applications

Directory of Open Access Journals (Sweden)

Xiaoliang Wang

2017-11-01

Full Text Available Titanium dioxide (TiO2 materials have been intensively studied in the past years because of many varied applications. This mini review article focuses on TiO2 micro and nano architectures with the prevalent crystal structures (anatase, rutile, brookite, and TiO2(B, and summarizes the major advances in the surface and interface engineering and applications in environmental and electrochemical applications. We analyze the advantages of surface/interface engineered TiO2 micro and nano structures, and present the principles and growth mechanisms of TiO2 nanostructures via different strategies, with an emphasis on rational control of the surface and interface structures. We further discuss the applications of TiO2 micro and nano architectures in photocatalysis, lithium/sodium ion batteries, and Li–S batteries. Throughout the discussion, the relationship between the device performance and the surface/interface structures of TiO2 micro and nano structures will be highlighted. Then, we discuss the phase transitions of TiO2 nanostructures and possible strategies of improving the phase stability. The review concludes with a perspective on the current challenges and future research directions.

Pulse electrochemical machining on Invar alloy: Optical microscopic/SEM and non-contact 3D measurement study of surface analyses

International Nuclear Information System (INIS)

Kim, S.H.; Choi, S.G.; Choi, W.K.; Yang, B.Y.; Lee, E.S.

2014-01-01

Highlights: • Invar alloy was electrochemically polished and then subjected to PECM (Pulse Electro Chemical Machining) in a mixture of NaCl, glycerin, and distilled water. • Optical microscopic/SEM and non-contact 3D measurement study of Invar surface analyses. • Analysis result shows that applied voltage and electrode shape are factors that affect the surface conditions. - Abstract: In this study, Invar alloy (Fe 63.5%, Ni 36.5%) was electrochemically polished by PECM (Pulse Electro Chemical Machining) in a mixture of NaCl, glycerin, and distilled water. A series of PECM experiments were carried out with different voltages and different electrode shapes, and then the surfaces of polished Invar alloy were investigated. The polished Invar alloy surfaces were investigated by optical microscope, scanning electron microscope (SEM), and non-contact 3D measurement (white light microscopes) and it was found that different applied voltages produced different surface characteristics on the Invar alloy surface because of the locally concentrated applied voltage on the Invar alloy surface. Moreover, we found that the shapes of electrode also have an effect on the surface characteristics on Invar alloy surface by influencing the applied voltage. These experimental findings provide fundamental knowledge for PECM of Invar alloy by surface analysis

Experimental Setup for Diamond Grinding Using Electrochemical InProcess Controlled Dressing (ECD of Grinding Wheel

Directory of Open Access Journals (Sweden)

M. A. Shavva

2014-01-01

Full Text Available The most effective method for finish machining of hard-metals and alloys is to use the diamond grinding wheels for grinding. An application of diamond wheels significantly increases the employee output, reduces costs, and raises manufacturing efficiency with achieving the high performance properties of treated surfaces.During grinding a working surface of diamond wheel wears out. It adversely affects the cutting capability of the diamond grains, and depending on the grinding conditions can occur through different mechanisms. Wear of diamond wheel causes distortion of its shape and reduces cutting properties. However, dressing of diamond wheels is a complicated and time-consuming operation in terms of manufacturing technique.Methods to make dressing of diamond grinding wheel have different types of classification. Classification of dressing methods by the type of energy used is as follows: mechanical, chemical, electrophysical, electromechanical, and electrochemical. All these methods have their advantages and disadvantages.Electrochemical method of dressing is the most productive and efficient. Electrochemical method comprises anode-mechanical dressing and electrochemical (electrolytic one. The paper presents the electrochemical in-process dressing (ECD and the electrolytic in-process dressing (ELID.The source of energy, grinding a wheel with metal bond, and an electrode are necessary for providing ELID. The ELID consists of several stages. The first stage is preliminary electrolytic dressing of diamond wheel. The electrolyte is placed into the gap between the wheel and electrode. The bond of the wheel is oxidized. An insulating layer is formed. It reduces an electrical conductivity of the wheel and controls consumption of diamond grains, as well as polishes the surface of the work piece. Further, the insulating layer is destroyed. The cycle of dressing begins anew.The ECD proceeds in the same way as ELID. However during the ECD-process there

Topographic and Electrochemical Ti6Al4V Alloy Surface Characterization in Dry and Wet Reciprocating Sliding

Directory of Open Access Journals (Sweden)

Z. Doni

2013-09-01

Full Text Available This present paper shows the behavior of functional integrity of the state Ti6Al4V alloy under reciprocating sliding wear conditions in acomparative way for two different counter materials, steel and ceramicballs in dry and corrosive environment (3.5% NaCl. The surface integrity analysis of the dry reciprocating wear tests was based on the evolution of The roughness parameters with the applied load. In the case of reciprocating wear tests in corrosive environment the surface integrity analysis was based on electrochemical parameters. Comparative analysis of the evolution of the roughness parameters with the applied load shows a higher stability of the Ti6Al4V/Al2O3 contact pair, while from the point of view of the electrochemical parameters the Tribological properties are worse than Ti6Al4V/steel ball contact pair.

Electrochemically controlled release of anticancer drug methotrexate using nanostructured polypyrrole modified with cetylpyridinium: Release kinetics investigation

International Nuclear Information System (INIS)

Alizadeh, Naader; Shamaeli, Ehsan

2014-01-01

A new simple strategy for direct electrochemical incorporation of chemotherapeutic methotrexate (MTX) into conductive polypyrrole (PPy) has been suggested for an electrochemically controlled loading and release system. Electropolymerization of MTX doped polypyrrole yielded poor quality with low efficiency of doping, but a well-doped, nanostructure and increased capacity of drug loading (24.5 mg g −1 ) has been obtained in the presence of cetylpyridinium (CP) as a modifier. When CP was preloaded onto PPy, the hydrophobic surface of the PPy serves as a backbone to which the hydrophobic chain of the CP can be attached. Electrostatic interaction between cationic CP with anionic MTX and aromatic interaction between pyridinium head of CP with pyrimidine and pyrazine rings of MTX increases drug doping. Then release kinetics were investigated at various applied potentials and temperatures. Kinetics analysis based on Avrami's equation showed that the drug release was controlled and accelerated by increasing temperature and negative potential and sustained by increasing positive potential. At open circuit condition, the release parameter (n) represented a diffusive mechanism and at applying electrochemical potentials, a first-order mode. Activation energy parameters (E a , ΔG ≠ , ΔH ≠ and ΔS ≠ ) and half-life time (t 1/2 ) of drug release are also analyzed as a function of applied potential. The nanostructured polymer films (PPy/CP/MTX) were characterized by several techniques: scanning electron microscopy, Furrier transforms Infrared, UV-vis spectroscopy. Overall, our results demonstrate that the PPy/CP/MTX films, combined with electrical stimulation, permit a programmable release of MTX by altering the interaction strength between the PPy/CP and MTX

A cell for the controllable thermal treatment and electrochemical characterisation of single crystal alloy electrodes

DEFF Research Database (Denmark)

Bondarenko, Alexander S.; Stephens, Ifan E.L.; Chorkendorff, Ib

2012-01-01

be performed in this cell. These include preparation and basic voltammetric characterisation of Cu/Pt(111) near-surface and surface alloys where monolayer amounts of Cu are located in the 1st and 2nd layers, respectively. The cell can also be useful for “electrochemical atomic layer epitaxy” to assemble...... multilayers using repetitive underpotential deposition....

Surface modification of 2014 aluminium alloy-Al2O3 particles composites by nickel electrochemical deposition

International Nuclear Information System (INIS)

Molina, J.M.; Saravanan, R.A.; Narciso, J.; Louis, E.

2004-01-01

A method to modify the surface of aluminium matrix composites (AMC) by electrochemical nickel deposition has been developed. Deposition was carried out in a stirred standard Watt's bath, whereas potential and time were varied to optimize coating characteristics. The method, that allowed to overcome the serious difficulties associated to electrochemical deposition of an inherently inhomogeneous material, was used to nickel coat composites of 2014 aluminium alloy-15 vol.% Al 2 O 3 particles. Coats with a good adherence and up to 60 μm thick were easily obtained. In order to improve surface properties, the coated composite was subjected to rather long (from 10 to 47.5 h) heat treatments at a temperature of 520 deg,C. The heat treatments improved the uniformity of the deposited layer and promoted the formation of Al-Ni intermetallics (mainly Al 3 Ni 2 , as revealed by X-ray diffraction and energy-dispersive X-ray analysis (EDX)). Experimental results indicate that growth of the intermetallic layer is diffusion limited

A Twice Electrochemical-Etching Method to Fabricate Superhydrophobic-Superhydrophilic Patterns for Biomimetic Fog Harvest.

Science.gov (United States)

Yang, Xiaolong; Song, Jinlong; Liu, Junkai; Liu, Xin; Jin, Zhuji

2017-08-18

Superhydrophobic-superhydrophilic patterned surfaces have attracted more and more attention due to their great potential applications in the fog harvest process. In this work, we developed a simple and universal electrochemical-etching method to fabricate the superhydrophobic-superhydrophilic patterned surface on metal superhydrophobic substrates. The anti-electrochemical corrosion property of superhydrophobic substrates and the dependence of electrochemical etching potential on the wettability of the fabricated dimples were investigated on Al samples. Results showed that high etching potential was beneficial for efficiently producing a uniform superhydrophilic dimple. Fabrication of long-term superhydrophilic dimples on the Al superhydrophobic substrate was achieved by combining the masked electrochemical etching and boiling-water immersion methods. A long-term wedge-shaped superhydrophilic dimple array was fabricated on a superhydrophobic surface. The fog harvest test showed that the surface with a wedge-shaped pattern array had high water collection efficiency. Condensing water on the pattern was easy to converge and depart due to the internal Laplace pressure gradient of the liquid and the contact angle hysteresis contrast on the surface. The Furmidge equation was applied to explain the droplet departing mechanism and to control the departing volume. The fabrication technique and research of the fog harvest process may guide the design of new water collection devices.

Highly reproducible surface-enhanced Raman scattering-active Au nanostructures prepared by simple electrodeposition: origin of surface-enhanced Raman scattering activity and applications as electrochemical substrates.

Science.gov (United States)

Choi, Suhee; Ahn, Miri; Kim, Jongwon

2013-05-24

The fabrication of effective surface-enhanced Raman scattering (SERS) substrates has been the subject of intensive research because of their useful applications. In this paper, dendritic gold (Au) rod (DAR) structures prepared by simple one-step electrodeposition in a short time were examined as an effective SERS-active substrate. The SERS activity of the DAR surfaces was compared to that of other nanostructured Au surfaces with different morphologies, and its dependence on the structural variation of DAR structures was examined. These comparisonal investigations revealed that highly faceted sharp edge sites present on the DAR surfaces play a critical role in inducing a high SERS activity. The SERS enhancement factor was estimated to be greater than 10(5), and the detection limit of rhodamine 6G at DAR surfaces was 10(-8)M. The DAR surfaces exhibit excellent spot-to-spot and substrate-to-substrate SERS enhancement reproducibility, and their long-term stability is very good. It was also demonstrated that the DAR surfaces can be effectively utilized in electrochemical SERS systems, wherein a reversible SERS behavior was obtained during the cycling to cathodic potential regions. Considering the straightforward preparation of DAR substrates and the clean nature of SERS-active Au surfaces prepared in the absence of additives, we expect that DAR surfaces can be used as cost-effective SERS substrates in analytical and electrochemical applications. Copyright © 2013 Elsevier B.V. All rights reserved.

Electrochemical, interfacial, and surface studies of the conversion of carbon dioxide to liquid fuels on tin electrodes

Science.gov (United States)

Wu, Jingjie

maximize the triple phase boundary length for simultaneous high current density and selectivity towards formate formation (Chapter 3). The Sn GDEs was incorporated into a home-designed scalable full electrochemical cell which features a buffer layer of circulating liquid electrolyte mediating the proton concentration at cathode electrode surface. The Sn GDEs exhibited excellent short-term performance for CO2 reduction with high selectivity towards formate formation at low overpotentials in the full electrochemical cell. Additionally, coupling water oxidation and CO2 reduction was demonstrated in this full electrochemical cell to mimic biosynthesis (Chapter 4). The rapid degradation of selectivity towards formate formation on Sn GDEs in the full electrochemical cell, however, was observed during long-term operation. The degradation mechanism was unraveled due to the decrease of electrode potential resulted from substantial increase of internal ohmic resistance of the full electrochemical cell. The unexpected rise of internal ohmic resistance was attributed to the pulverization of 100 nm Sn nanoparticles due to the hydrogen diffusion induced stress. Based on the understanding of the origin of Sn nanoparticles pulverization, SnO2 nanoparticles of 3˜3.5 nm close to the critical size were utilized and reduced in situ to form Sn catalyst for electrochemical reduction of CO2. The pulverization was suppressed and subsequently a stable performance of electrodes was obtained (Chapter 5). Due to the affinity to oxygen, Sn nanoparticle surface is covered by a native thin oxide layer. The performance of Sn GDEs towards CO2 reduction strongly depends on the initial thickness of the surface oxide layer. The selectivity towards formate production dropped while the hydrogen yield increased as the initial thickness of the oxide layer increased (Chapter 6). These results suggest the underlying of surface structure on the selectivity of Sn electrode for CO2 reduction and provide insight into

Surface-reconstructed Cu Electrode via a Facile Electrochemical Anodization-Reduction Process for Low Overpotential CO 2 reduction

KAUST Repository

Min, Shixiong; Yang, Xiulin; Lu, Ang-Yu; Tseng, Chien-Chih; Hedhili, Mohamed N.; Lai, Zhiping; Li, Lain-Jong; Huang, Kuo-Wei

2017-01-01

A high-surface-area Cu electrode, fabricated by a simple electrochemical anodization-reduction method, exhibits high activity and selectivity for CO2 reduction at low overpotential in 0.1 M KHCO3 solution. A faradaic efficiency of 37% for HCOOH

Electrochemical Insights into Platinum Catalysts for Fuel Cells

DEFF Research Database (Denmark)

Jensen, Kim Degn

. A preliminary electrochemical study of in-house synthesized Pt-Y nanoparticles have also been presented revealing specific mass actives of 0.3 ± 0.1A/mgPt in HClO4. The study revealed that extensive optimizations of the Pt-Y nanoparticles are required and their performance is severely impeded by poor......Development of sustainable energy production, conversion and storage technologies must be considered one of the major challenges of the 21st century. Insight and understanding of the oxygen reduction reaction is imperative in these pursuits. In this work electrochemical investigations and physical...... characterization of various model systems ranging from extended surfaces, to thin films and nanoparticle electrocatalysts have been presented and discussed. This have been done with a special focus on governing factors controlling the electroreduction of oxygen. Preparation of Cu/Pt(111) near-surface alloys...

Low-dimensional carbon and MXene-based electrochemical capacitor electrodes.

Science.gov (United States)

Yoon, Yeoheung; Lee, Keunsik; Lee, Hyoyoung

2016-04-29

Due to their unique structure and outstanding intrinsic physical properties such as extraordinarily high electrical conductivity, large surface area, and various chemical functionalities, low-dimension-based materials exhibit great potential for application in electrochemical capacitors (ECs). The electrical properties of electrochemical capacitors are determined by the electrode materials. Because energy charge storage is a surface process, the surface properties of the electrode materials greatly influence the electrochemical performance of the cell. Recently, graphene, a single layer of sp(2)-bonded carbon atoms arrayed into two-dimensional carbon nanomaterial, has attracted wide interest as an electrode material for electrochemical capacitor applications due to its unique properties, including a high electrical conductivity and large surface area. Several low-dimensional materials with large surface areas and high conductivity such as onion-like carbons (OLCs), carbide-derived carbons (CDCs), carbon nanotubes (CNTs), graphene, metal hydroxide, transition metal dichalcogenides (TMDs), and most recently MXene, have been developed for electrochemical capacitors. Therefore, it is useful to understand the current issues of low-dimensional materials and their device applications.

Low-dimensional carbon and MXene-based electrochemical capacitor electrodes

International Nuclear Information System (INIS)

Yoon, Yeoheung; Lee, Hyoyoung; Lee, Keunsik

2016-01-01

Due to their unique structure and outstanding intrinsic physical properties such as extraordinarily high electrical conductivity, large surface area, and various chemical functionalities, low-dimension-based materials exhibit great potential for application in electrochemical capacitors (ECs). The electrical properties of electrochemical capacitors are determined by the electrode materials. Because energy charge storage is a surface process, the surface properties of the electrode materials greatly influence the electrochemical performance of the cell. Recently, graphene, a single layer of sp 2 -bonded carbon atoms arrayed into two-dimensional carbon nanomaterial, has attracted wide interest as an electrode material for electrochemical capacitor applications due to its unique properties, including a high electrical conductivity and large surface area. Several low-dimensional materials with large surface areas and high conductivity such as onion-like carbons (OLCs), carbide-derived carbons (CDCs), carbon nanotubes (CNTs), graphene, metal hydroxide, transition metal dichalcogenides (TMDs), and most recently MXene, have been developed for electrochemical capacitors. Therefore, it is useful to understand the current issues of low-dimensional materials and their device applications. (topical review)

Active control of methanol carbonylation selectivity over Au/carbon anode by electrochemical potential.

Science.gov (United States)

Funakawa, Akiyasu; Yamanaka, Ichiro; Otsuka, Kiyoshi

2005-05-12

Electrochemical oxidative carbonylation of methanol was studied over Au supported carbon anode in CO. The major carbonylation products were dimethyl oxalate (DMO) and dimethyl carbonate (DMC). The minor oxidation products were dimethoxy methane (DMM) and methyl formate (MF) from methanol and CO(2). Influences of various reaction conditions were studied on carbonylation activities and selectivities. The selectivities to DMO and DMC can be controlled by the electrochemical potential. Electrocatalysis of Au/carbon anode was studied by cyclic voltammetry (CV), stoichiometric reactions among Au(3+), methanol, and CO, and UV-vis spectra. The Au/carbon anode was characterized by XRD, SEM, and BE images before and after the carbonylation. These experimental facts strongly suggest that transition of oxidation states of Au affects changing of the carbonylation selectivities to DMO and DMC. Au(0) is the active species for the selective DMO formation by direct electrochemical carbonylation at low potentials (selective DMC formation by indirect electrochemical carbonylation through Au(3+)/Au(+) redox at high potentials (>+1.3 V).

Electrochemical properties of ion implanted silicon

International Nuclear Information System (INIS)

Pham minh Tan.

1979-11-01

The electrochemical behaviour of ion implanted silicon in contact with hydrofluoric acid solution was investigated. It was shown that the implanted layer on silicon changes profoundly its electrochemical properties (photopotential, interface impedance, rest potential, corrosion, current-potential behaviour, anodic dissolution of silicon, redox reaction). These changes depend strongly on the implantation parameters such as ion dose, ion energy, thermal treatment and ion mass and are weakly dependent on the chemical nature of the implantation ion. The experimental results were evaluated and interpreted in terms of the semiconductor electrochemical concepts taking into account the interaction of energetic ions with the solid surface. The observed effects are thus attributed to the implantation induced damage of silicon lattice and can be used for profiling of the implanted layer and the electrochemical treatment of the silicon surface. (author)

Covalent attachment of pyridine-type molecules to glassy carbon surfaces by electrochemical reduction of in situ generated diazonium salts. Formation of ruthenium complexes on ligand-modified surfaces

Energy Technology Data Exchange (ETDEWEB)

Yesildag, Ali [Department of Chemistry, Faculty of Sciences, Atatuerk University, 25240 Erzurum (Turkey); Ekinci, Duygu, E-mail: dekin@atauni.edu.t [Department of Chemistry, Faculty of Sciences, Atatuerk University, 25240 Erzurum (Turkey)

2010-09-30

In this study, pyridine, quinoline and phenanthroline molecules were covalently bonded to glassy carbon (GC) electrode surfaces for the first time using the diazonium modification method. Then, the complexation ability of the modified films with ruthenium metal cations was investigated. The derivatization of GC surfaces with heteroaromatic molecules was achieved by electrochemical reduction of the corresponding in situ generated diazonium salts. X-ray photoelectron spectroscopy (XPS) was used to confirm the attachment of heteroaromatic molecules to the GC surfaces and to determine the surface concentration of the films. The barrier properties of the modified GC electrodes were studied in the presence of redox probes such as Fe(CN){sub 6}{sup 3-} and Ru(NH{sub 3}){sub 6}{sup 3+} by cyclic voltammetry. Additionally, the presence of the resulting organometallic films on the surfaces was verified by XPS after the chemical transformation of the characterized ligand films to the ruthenium complex films. The electrochemical behavior of these films in acetonitrile solution was investigated using voltammetric methods, and the surface coverage of the organometallic films was determined from the reversible metal-based Ru(II)/Ru(III) oxidation waves.

Enhanced electrochemical performances of mesoporous carbon microsphere/selenium composites by controlling the pore structure and nitrogen doping

International Nuclear Information System (INIS)

Liu, Lei; Wei, Yanju; Zhang, Chuanfang; Zhang, Chuan; Li, Xu; Wang, Jitong; Ling, Licheng; Qiao, Wenming; Long, Donghui

2015-01-01

Graphical abstract: Mesoporous carbon microspheres (MCMs) with tunable pore sizes have been prepared via a high-throughput spray drying-assisted hard template method and used as the hosts to load selenium (Se) for Li-Se batteries. - Abstract: Mesoporous carbon microspheres (MCMs) with tunable pore sizes have been prepared via a high-throughput spray drying-assisted hard template method and used as the hosts to load selenium (Se) for lithium-selenium (Li-Se) batteries. The pore size control of the MCMs (3.8, 5, 6.5, 9.5 nm) was achieved by in-situ polymerized colloid silica templates with different sizes, thus prompting us to focus on tracing the effects of mesopore size on electrochemical performance of MCMs/Se cathodes. The results reveal that relative higher capacity and better cycling performance are presented in MCMs with smaller pores size due to the more effective confinement effect. At an optimal pore size of 3.8 nm, the MCMs/Se with 50% Se loading delivers an initial capacity of 513 mAh g −1 and capacity retention of 300 mAh g −1 after 100 cycles at 0.5 C. Furthermore, it is concluded that nitrogen doping could assist MCMs to retard the diffusion of polyselenide species possibly via an enhanced surface adsorption. The composites thus increase the reversible capacity by 30% after 100 cycles compared with the nitrogen-free composite. These results indicate that controlling pore structure and surface chemistry are good strategies to optimize the electrochemical performance of C/Se based cathodes for Li–Se batteries

Electrochemical characteristics of polyacetylene in organic electrolytes

Energy Technology Data Exchange (ETDEWEB)

Padula, A.; Scrosati, B.

1985-01-15

The characteristics of the electrochemical doping process of polyacetylene have been investigated in lithium cells using lithium perchlorate in propylene carbonate as electrolytic solution. The kinetics of this process are controlled by the diffusion of the dopant species throughout the polymer. Therefore, polyacetylene samples with a highly porous, extended surface should be selected for the development of efficient, rechargeable lithium batteries. In line with this, we have considered foam-type polyacetylene electrodes which have a lower density than the 'classical' Shirakawa-type film electrodes. The electrochemical behaviour of the polyacetylene foam samples has been examined by cyclic voltametry response and constant current, charge-discharge cycles. The results are described in this work.

Evaluation of the Technical-Economic Potential of Particle- Reinforced Aluminum Matrix Composites and Electrochemical Machining

International Nuclear Information System (INIS)

Schubert, A; Hackert-Oschätzchen, M; Lehnert, N; Götze, U; Herold, F; Schmidt, A; Meichsner, G

2016-01-01

Compared to conventional cutting, the processing of materials by electrochemical machining offers some technical advantages like high surface quality, no thermal or mechanical impact on the work piece and preservation of the microstructure of the work piece material. From the economic point of view, the possibility of process parallelization and the absence of any process-related tool wear are mentionable advantages of electrochemical machining. In this study, based on experimental results, it will be evaluated to what extent the electrochemical machining is technically and economically suitable for the finish-machining of particle- reinforced aluminum matrix composites (AMCs). Initial studies showed that electrochemical machining - in contrast to other machining processes - has the potential to fulfil demanding requirements regarding precision and surface quality of products or components especially when applied to AMCs. In addition, the investigations show that processing of AMCs by electrochemical machining requires less energy than the electrochemical machining of stainless steel. Therefore, an evaluation of electrochemically machined AMCs - compared to stainless steel - from a technical and an economic perspective will be presented in this paper. The results show the potential of electro-chemically machined AMCs and contribute to the enhancement of instruments for technical-economic evaluations as well as a comprehensive innovation control. (paper)

Electrochemical synthesis of mesoporous Pt-Au binary alloys with tunable compositions for enhancement of electrochemical performance.

Science.gov (United States)

Yamauchi, Yusuke; Tonegawa, Akihisa; Komatsu, Masaki; Wang, Hongjing; Wang, Liang; Nemoto, Yoshihiro; Suzuki, Norihiro; Kuroda, Kazuyuki

2012-03-21

Mesoporous Pt-Au binary alloys were electrochemically synthesized from lyotropic liquid crystals (LLCs) containing corresponding metal species. Two-dimensional exagonally ordered LLC templates were prepared on conductive substrates from diluted surfactant solutions including water, a nonionic surfactant, ethanol, and metal species by drop-coating. Electrochemical synthesis using such LLC templates enabled the preparation of ordered mesoporous Pt-Au binary alloys without phase segregation. The framework composition in the mesoporous Pt-Au alloy was controlled simply by changing the compositional ratios in the precursor solution. Mesoporous Pt-Au alloys with low Au content exhibited well-ordered 2D hexagonal mesostructures, reflecting those of the original templates. With increasing Au content, however, the mesostructural order gradually decreased, thereby reducing the electrochemically active surface area. Wide-angle X-ray diffraction profiles, X-ray photoelectron spectra, and elemental mapping showed that both Pt and Au were atomically distributed in the frameworks. The electrochemical stability of mesoporous Pt-Au alloys toward methanol oxidation was highly improved relative to that of nonporous Pt and mesoporous Pt films, suggesting that mesoporous Pt-Au alloy films are potentially applicable as electrocatalysts for direct methanol fuel cells. Also, mesoporous Pt-Au alloy electrodes showed a highly sensitive amperometric response for glucose molecules, which will be useful in next-generation enzyme-free glucose sensors.

A Novel of Multi-wall Carbon Nanotubes/Chitosan Electrochemical Sensor for Determination of Cupric ion

Science.gov (United States)

Tan, Funeng; Li, Lei

2018-03-01

A multi-wall carbon nanotubes/Chitosan electrochemical sensor had been fabricated by dropping CHS/MWNT solution directly onto the GC surface. The sensor was charactered by cyclic voltammetry and AC impedance with K3Fe(CN)6 as a electrochemical probe; Cyclic voltammograms(CV) and electrochemical impedance spectroscopy(EIS) indicated that the active area and electrochemical behavior of the sensor increased and improved significantly after the electrode was modified by carbon nanotubes dispersed by the chitosan. The sensor showed good electrocatalytic activity of K3Fe(CN)6. Also, from the cyclic voltammograms, we can see the process was diffusion controlled on the bare electrode and kinetics and diffusion controlled on the modified electrode. Finally Cu2+ responsed sensitively at the sensor which supplied a new method for the detection of Cu2+.

Atomic layer deposition of highly dispersed Pt nanoparticles on a high surface area electrode backbone for electrochemical promotion of catalysis

NARCIS (Netherlands)

Hajar, Y.; di Palma, V.; Kyriakou, V.; Verheijen, M. A.; Baranova, E. A.; Vernoux, P.; Kessels, W. M. M.; Creatore, M.; van de Sanden, M. C. M.; Tsampas, M. N.

2017-01-01

A novel catalyst design for electrochemical promotion of catalysis (EPOC) is proposed which overcomes the main bottlenecks that limit EPOC commercialization, i.e., the low dispersion and small surface area of metal catalysts. We have increased the surface area by using a porous composite electrode

Surface-modified reduced graphene oxide electrodes for capacitors by ionic liquids and their electrochemical properties

International Nuclear Information System (INIS)

Kim, Jieun; Kim, Seok

2014-01-01

Highlights: • Reduced graphene oxide surface was modified by introduction of ionic liquids. • Microstructure and capacitance of modified electrode were dependent on the ionic liquids contents. • Modification gives electrode better charge transport and higher specific capacitance. • Modified electrode showed the better capacitive performance such as rate capability and cycle stability. - Abstract: In this work, reduced graphene oxide (rGO)/ionic liquids (IL) composites with different weight ratios of IL to rGO were synthesized by a simple method. In these composites, IL contributed to the exfoliation of rGO sheets and to the improvement of the electrochemical properties of the resulting composites by enhancing the ion diffusion and charge transport. The structure of the composites was examined by transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), and Raman spectroscopy. The TEM images showed that IL was coated on the surface of rGO in a translucent manner. The electrochemical analysis of the prepared composites was carried out by performing cyclic voltammetry (CV), galvanostatic charge–discharge, and electrochemical impedance spectroscopy (EIS). Among the prepared composites, the one with a weight ratio of rGO to IL of 1:7 showed the highest specific capacitance of 147.5 F g −1 at a scan rate of 10 mV s −1 . In addition, the rate capability and cycle performance of the composites were enhanced compared to pristine rGO. These enhanced properties make the composites suitable as electrode materials for the better performance supercapacitors

Electrochemically assisted deposition of strontium modified magnesium phosphate on titanium surfaces

International Nuclear Information System (INIS)

Meininger, M.; Wolf-Brandstetter, C.; Zerweck, J.; Wenninger, F.; Gbureck, U.; Groll, J.; Moseke, C.

2016-01-01

Electrochemically assisted deposition was utilized to produce ceramic coatings on the basis of magnesium ammonium phosphate (struvite) on corundum-blasted titanium surfaces. By the addition of defined concentrations of strontium nitrate to the coating electrolyte Sr 2+ ions were successfully incorporated into the struvite matrix. By variation of deposition parameters it was possible to fabricate coatings with different kinetics of Sr 2+ into physiological media, whereas the release of therapeutically relevant strontium doses could be sustained over several weeks. Morphological and crystallographic examinations of the immersed coatings revealed that the degradation of struvite and the release of Sr 2+ ions were accompanied by a transformation of the coating to a calcium phosphate based phase similar to low-crystalline hydroxyapatite. These findings showed that strontium doped struvite coatings may provide a promising degradable coating system for the local application of strontium or other biologically active metal ions in the implant–bone interface. - Highlights: • Sr-doped struvite coatings have been deposited on titanium by electrochemically assisted deposition. • Sr content can be adjusted by means of process time, current density and pulse mode. • Sr-doped coatings release therapeutically relevant Sr doses in physiological media for several weeks. • During immersion in physiological media Sr-doped struvite coatings transform into a low crystalline calcium phosphate phase.

Monitoring the electrochemical responses of neurotransmitters through localized surface plasmon resonance using nanohole array.

Science.gov (United States)

Li, Nantao; Lu, Yanli; Li, Shuang; Zhang, Qian; Wu, Jiajia; Jiang, Jing; Liu, Gang Logan; Liu, Qingjun

2017-07-15

In this study, a novel spectroelectrochemical method was proposed for neurotransmitters detection. The central sensing device was a hybrid structure of nanohole array and gold nanoparticles, which demonstrated good conductivity and high localized surface plasmon resonance (LSPR) sensitivity. By utilizing such specially-designed nanoplasmonic sensor as working electrode, both electrical and spectral responses on the surface of the sensor could be simultaneously detected during the electrochemical process. Cyclic voltammetry was implemented to activate the oxidation and recovery of dopamine and serotonin, while transmission spectrum measurement was carried out to synchronously record to LSPR responses of the nanoplasmonic sensor. Coupling with electrochemistry, LSPR results indicated good integrity and linearity, along with promising accuracy in qualitative and quantitative detection even for mixed solution and in brain tissue homogenates. Also, the detection results of other negatively-charged neurotransmitters like acetylcholine demonstrated the selectivity of our detection method for transmitters with positive charge. When compared with traditional electrochemical signals, LSPR signals provided better signal-to-noise ratio and lower detection limits, along with immunity against interference factors like ascorbic acid. Taking the advantages of such robustness, the coupled detection method was proved to be a promising platform for point-of-care testing for neurotransmitters. Copyright © 2016 Elsevier B.V. All rights reserved.

Controllable Fabrication of Amorphous Co-Ni Pyrophosphates for Tuning Electrochemical Performance in Supercapacitors.

Science.gov (United States)

Chen, Chen; Zhang, Ning; He, Yulu; Liang, Bo; Ma, Renzhi; Liu, Xiaohe

2016-09-07

Incorporation of two transition metals offers an effective method to enhance the electrochemical performance in supercapacitors for transition metal compound based electrodes. However, such a configuration is seldom concerned in pyrophosphates. Here, amorphous phase Co-Ni pyrophosphates are fabricated as electrodes in supercapacitors. Through controllably adjusting the ratios of Co and Ni as well as the calcination temperature, the electrochemical performance can be tuned. An optimized amorphous Ni-Co pyrophosphate exhibits much higher specific capacitance than monometallic Ni and Co pyrophosphates and shows excellent cycling ability. When employing Ni-Co pyrophosphates as positive electrode and activated carbon as a negative electrode, the fabricated asymmetric supercapacitor cell exhibits favorable capacitance and cycling ability. This study provides facile methods to improve the transition metal pyrophosphate electrodes for efficient electrodes in electrochemical energy storage devices.

On-line electrochemically controlled in-tube solid phase microextraction of inorganic selenium followed by hydride generation atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Asiabi, Hamid [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Yamini, Yadollah, E-mail: yyamini@modares.ac.ir [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Seidi, Shahram [Department of Analytical Chemistry, Faculty of Chemistry, K.N. Toosi University of Technology, Tehran (Iran, Islamic Republic of); Shamsayei, Maryam; Safari, Meysam; Rezaei, Fatemeh [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of)

2016-05-30

In this work, for the first time, a rapid, simple and sensitive microextraction procedure is demonstrated for the matrix separation, preconcentration and determination of inorganic selenium species in water samples using an electrochemically controlled in-tube solid phase microextraction (EC-in-tube SPME) followed by hydride generation atomic absorption spectrometry (HG-AAS). In this approach, in which EC-in-tube SPME and HG-AAS system were combined, the total analysis time, was decreased and the accuracy, repeatability and sensitivity were increased. In addition, to increases extraction efficiency, a novel nanostructured composite coating consisting of polypyrrole (PPy) doped with ethyleneglycol dimethacrylate (EGDMA) was prepared on the inner surface of a stainless-steel tube by a facile electrodeposition method. To evaluate the offered setup and the new PPy-EGDMA coating, it was used to extract inorganic selenium species in water samples. Extraction of inorganic selenium species was carried out by applying a positive potential through the inner surface of coated in-tube under flow conditions. Under the optimized conditions, selenium was detected in amounts as small as 4.0 parts per trillion. The method showed good linearity in the range of 0.012–200 ng mL{sup −1}, with coefficients of determination better than 0.9996. The intra- and inter-assay precisions (RSD%, n = 5) were in the range of 2.0–2.5% and 2.7–3.2%, respectively. The validated method was successfully applied for the analysis of inorganic selenium species in some water samples and satisfactory results were obtained. - Graphical abstract: An electrochemically controlled in-tube solid phase microextraction followed by hydride generation atomic absorption spectrometry was developed for extraction and determination ultra-trace amounts of Se in aqueous solutions. - Highlights: • A nanostructured composite coating consisting of PPy doped with EGDMA was prepared. • The coating was

Investigation of the electrochemically active surface area and lithium diffusion in graphite anodes by a novel OsO4 staining method

Science.gov (United States)

Pfaffmann, Lukas; Birkenmaier, Claudia; Müller, Marcus; Bauer, Werner; Mitsch, Tim; Feinauer, Julian; Krämer, Yvonne; Scheiba, Frieder; Hintennach, Andreas; Schleid, Thomas; Schmidt, Volker; Ehrenberg, Helmut

2016-03-01

Negative electrodes of lithium-ion batteries generally consist of graphite-based active materials. In order to realize batteries with a high current density and therefore accelerated charging processes, the intercalation of lithium and the diffusion processes of these carbonaceous materials must be understood. In this paper, we visualized the electrochemical active surface area for three different anode materials using a novel OsO4 staining method in combination with scanning electron microscopy techniques. The diffusion behavior of these three anode materials is investigated by potentiostatic intermittent titration technique measurements. From those we determine the diffusion coefficient with and without consideration of the electrochemical active surface area.

In situ generation of diazonium cations in organic electrolyte for electrochemical modification of electrode surface

International Nuclear Information System (INIS)

Baranton, Steve; Belanger, Daniel

2008-01-01

The modification of glassy carbon electrode was achieved by electrochemical reduction of in situ generated diazonium cations in acetonitrile. The in situ generation of 4-nitrophenyl diazonium cations in acetonitrile was investigated by spectroscopic methods. UV-visible spectroscopy revealed slow kinetics for the reaction of 4-nitroaniline with tert-butylnitrite in acetonitrile to form the corresponding diazonium cation. As a result, a coupling reaction, which implies a consumption of the amine and loss of the already formed diazonium cations, was evidenced by 1 H NMR spectroscopy. This spectroscopic study allowed the optimization of the in situ diazonium cations generation prior to the modification step. The electrochemical modification of the carbon electrodes with 4-nitrophenyl, 4-bromophenyl and anthraquinone groups was characterized by cyclic voltammetry and the resulting grafted layer were characterized by electrochemical techniques. The cyclic voltammetric behaviour during the electrochemical grafting was very similar to the one observed for an isolated diazonium salt dissolved in acetonitrile. In the case of the anthraquinone-modified electrode, the use of acetonitrile, into which the corresponding amine is soluble but not in aqueous media, allowed for its grafting by the in situ approach. The barrier properties of these grafted layers are similar to those obtained from isolated diazonium salts. Finally, the chemical composition of the grafted layers was determined by X-ray photoelectron spectroscopy and surface coverage in the range 5-7 x 10 -10 mol cm -2 was estimated for films grown in our experimental conditions

In situ generation of diazonium cations in organic electrolyte for electrochemical modification of electrode surface

Energy Technology Data Exchange (ETDEWEB)

Baranton, Steve [Departement de Chimie, Universite du Quebec a Montreal, Case Postale 8888, succursale Centre-Ville, Montreal (Quebec), H3C 3P8 (Canada); Belanger, Daniel [Departement de Chimie, Universite du Quebec a Montreal, Case Postale 8888, succursale Centre-Ville, Montreal (Quebec), H3C 3P8 (Canada)], E-mail: belanger.daniel@uqam.ca

2008-10-01

The modification of glassy carbon electrode was achieved by electrochemical reduction of in situ generated diazonium cations in acetonitrile. The in situ generation of 4-nitrophenyl diazonium cations in acetonitrile was investigated by spectroscopic methods. UV-visible spectroscopy revealed slow kinetics for the reaction of 4-nitroaniline with tert-butylnitrite in acetonitrile to form the corresponding diazonium cation. As a result, a coupling reaction, which implies a consumption of the amine and loss of the already formed diazonium cations, was evidenced by {sup 1}H NMR spectroscopy. This spectroscopic study allowed the optimization of the in situ diazonium cations generation prior to the modification step. The electrochemical modification of the carbon electrodes with 4-nitrophenyl, 4-bromophenyl and anthraquinone groups was characterized by cyclic voltammetry and the resulting grafted layer were characterized by electrochemical techniques. The cyclic voltammetric behaviour during the electrochemical grafting was very similar to the one observed for an isolated diazonium salt dissolved in acetonitrile. In the case of the anthraquinone-modified electrode, the use of acetonitrile, into which the corresponding amine is soluble but not in aqueous media, allowed for its grafting by the in situ approach. The barrier properties of these grafted layers are similar to those obtained from isolated diazonium salts. Finally, the chemical composition of the grafted layers was determined by X-ray photoelectron spectroscopy and surface coverage in the range 5-7 x 10{sup -10} mol cm{sup -2} was estimated for films grown in our experimental conditions.

Influence of Oxidation Treatments and Surface Finishing on the Electrochemical Behavior of Ni-20Cr HVOF Coatings

Science.gov (United States)

Ruiz-Luna, H.; Porcayo-Calderon, J.; Alvarado-Orozco, J. M.; Mora-García, A. G.; Martinez-Gomez, L.; Trápaga-Martínez, L. G.; Muñoz-Saldaña, J.

2017-12-01

The low-temperature electrochemical behavior of HVOF Ni-20Cr coatings was assessed. The coatings were evaluated in different conditions including as-sprayed, as-ground, and heat-treated in air and argon atmospheres. A detailed analysis of the coatings was carried out by means of XRD, SEM, and EPMA, prior and after the corrosion test. The corrosion rate was analyzed in a NaCl solution saturated with CO2. Results demonstrate that the use of a low-oxygen partial pressure favors the formation of a Cr2O3 layer on the surface of the coatings. According to the electrochemical results, the lower corrosion rates were obtained for the heat-treated coatings irrespective of the surface finishing, being the ground and argon heat-treated condition that shows the best corrosion performance. This behavior is due to the synergistic effect of the low-pressure heat treatment and the grinding processes. The grinding promotes a more homogeneous reaction area without surface heterogeneities such as voids, and the pre-oxidation treatment decreases the porosity content of the coating and also allows the growing of a Cr-rich oxide scale which acts as a barrier against the ions of the aqueous solution.

Use of cyclic voltammetry and electrochemical impedance spectroscopy for determination of active surface area of modified carbon-based electrodes

International Nuclear Information System (INIS)

Souza, Leticia Lopes de

2011-01-01

Carbon-based electrodes as well the ion exchange electrodes among others have been applied mainly in the treatment of industrial effluents and radioactive wastes. Carbon is also used in fuel cells as substrate for the electrocatalysts, having high surface area which surpasses its geometric area. The knowledge of the total active area is important for the determination of operating conditions of an electrochemical cell with respect to the currents to be applied (current density). In this study it was used two techniques to determine the electrochemical active surface area of glassy carbon, electrodes and ion exchange electrodes: cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The experiments were carried out with KNO 3 0.1 mol.L -1 solutions in a three-electrode electrochemical cell: carbon-based working electrode, platinum auxiliary electrode and Ag/AgCl reference electrode. The glassy carbon and porous carbon electrodes with geometric areas of 3.14 x 10 -2 and 2.83 X 10 -1 cm 2 , respectively, were used. The ion exchange electrode was prepared by mixing graphite, carbon, ion exchange resin and a binder, and this mixture was applied in three layers on carbon felt, using a geometric area of 1.0 cm 2 during the experiments. The capacitance (Cd) of the materials was determined by EIS using Bode diagrams. The value of 172 μF.cm -2 found for the glassy carbon is consistent with the literature data (∼ 200 μF.cm'- 2 ). By VC, varying the scan rate from 0.2 to 2.0 mV.s-1, the capacitance CdS (S = active surface area) in the region of the electric double layer (EDL) of each material was determined. By EIS, the values of C d , 3.0 x 10 -5 μF.cm'- 2 and 11 x 10 3 μF.cm-2, were found for the porous carbon and ion exchange electrodes, respectively, which allowed the determination of active surface areas as 3.73 x 106 cm 2 and 4.72 cm 2 . To sum up, the combined use of EIS and CV techniques is a valuable tool for the calculation of active surface

Recent Progress in Electrochemical HbA1c Sensors: A Review

Directory of Open Access Journals (Sweden)

Baozhen Wang

2015-03-01

Full Text Available This article reviews recent progress made in the development of electrochemical glycated hemoglobin (HbA1c sensors for the diagnosis and management of diabetes mellitus. Electrochemical HbA1c sensors are divided into two categories based on the detection protocol of the sensors. The first type of sensor directly detects HbA1c by binding HbA1c on the surface of an electrode through bio-affinity of antibody and boronic acids, followed by an appropriate mode of signal transduction. In the second type of sensor, HbA1c is indirectly determined by detecting a digestion product of HbA1c, fructosyl valine (FV. Thus, the former sensors rely on the selective binding of HbA1c to the surface of the electrodes followed by electrochemical signaling in amperometric, voltammetric, impedometric, or potentiometric mode. Redox active markers, such as ferrocene derivatives and ferricyanide/ferrocyanide ions, are often used for electrochemical signaling. For the latter sensors, HbA1c must be digested in advance by proteolytic enzymes to produce the FV fragment. FV is electrochemically detected through catalytic oxidation by fructosyl amine oxidase or by selective binding to imprinted polymers. The performance characteristics of HbA1c sensors are discussed in relation to their use in the diagnosis and control of diabetic mellitus.

Combination of Electrochemical Processes with Membrane Bioreactors for Wastewater Treatment and Fouling Control: A Review

OpenAIRE

Ensano, Benny M. B.; Borea, Laura; Naddeo, Vincenzo; Belgiorno, Vincenzo; de Luna, Mark D. G.; Ballesteros, Florencio C.

2016-01-01

This paper provides a critical review about the integration of electrochemical processes into membrane bioreactors (MBR) in order to understand the influence of these processes on wastewater treatment performance and membrane fouling control. The integration can be realized either in an internal or an external configuration. Electrically enhanced membrane bioreactors or electro membrane bioreactors (eMBRs) combine biodegradation, electrochemical and membrane filtration processes into one syst...

Combination of electrochemical processes with membrane bioreactors for wastewater treatment and fouling control: A review

OpenAIRE

Benny Marie B. Ensano; Laura Borea; Vincenzo Naddeo; Vincenzo Belgiorno; Mark Daniel G. de Luna; Mark Daniel G. de Luna; Florencio C. Ballesteros, Jr.; Florencio C. Ballesteros, Jr.

2016-01-01

This paper provides a critical review about the integration of electrochemical processes into membrane bioreactors (MBR) in order to understand the influence of these processes on wastewater treatment performance and membrane fouling control. The integration can be realized either in an internal or an external configuration. Electrically enhanced membrane bioreactors or electro membrane bioreactors (eMBRs) combine biodegradation, electrochemical and membrane filtration processes into one syst...

Effect of ammonium-salt solutions on the surface properties of carbon fibers in electrochemical anodic oxidation

Energy Technology Data Exchange (ETDEWEB)

Qian Xin, E-mail: qx3023@nimte.ac.cn [National Engineering Laboratory of Carbon Fiber Preparation Technology, Ningbo Institute of Material Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201 (China); Wang Xuefei; Ouyang Qin; Chen Yousi; Yan Qing [National Engineering Laboratory of Carbon Fiber Preparation Technology, Ningbo Institute of Material Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201 (China)

2012-10-15

Highlights: Black-Right-Pointing-Pointer Longitudinal grooves on the fiber surface became more well-defined and much deeper after surface treatment. Black-Right-Pointing-Pointer The concentration of oxygen and nitrogen on the fiber surface increased after surface treatment. Black-Right-Pointing-Pointer The intensity of oxidative reaction varied with the change of ammonium-salt solutions. Black-Right-Pointing-Pointer The higher the concentration of OH{sup -} ions in the electrolytes, the violent the oxidative reaction happened. - Abstract: The surfaces of polyacrylonitrile-based carbon fibers were treated by an electrochemical anodic method. Three different kinds of ammonium-salt solutions namely NH{sub 4}HCO{sub 3}, (NH{sub 4}){sub 2}CO{sub 3} and (NH{sub 4}){sub 3}PO{sub 4} were respectively chosen as the electrolytes. The effect of these electrolytes on the surface structure was studied by scanning electron microscopy (SEM), atomic force microscopy (AFM), and X-ray photoelectron spectroscopy (XPS). The results showed that longitudinal grooves on the fiber surface became more well-defined and much deeper after surface treatment, and the root mean square roughness (RMS) of carbon fiber surface increased from 4.6 nm for untreated fibers to 13.5 nm for treated fibers in (NH{sub 4}){sub 3}PO{sub 4} electrolytes. The concentration of oxygen and nitrogen atomic on the fiber surface increased after surface treatment. The tensile strength of oxidized fibers had an obvious decrease, whereas the interlaminar shear strength (ILSS) value of corresponding carbon fiber reinforced polymers (CFRPs) increased in a large extent. The intensity of oxidative reaction varied with the change of ammonium-salt solutions and electrochemical oxidation in (NH{sub 4}){sub 3}PO{sub 4} electrolyte was of the most violence. The corresponding mechanism was also discussed and the result showed that the higher the concentration of OH{sup -} ions in the electrolytes, the violent the oxidative

Design of characteristic parameters for controlling tungsten tip profile during electrochemical etching

Energy Technology Data Exchange (ETDEWEB)

Le Duy Cuong; Duong, Thanh Hung; Kim, Huyn Chul [Inje University, Gimhae (Korea, Republic of)

2014-05-15

Micro/nano-scale tungsten tips fabricated by electrochemical etching have many diverse industrial applications. The characteristic parameters of the tungsten tip profile include apex radius, taper angle, and aspect ratio. These parameters are governed by many factors including applied voltage, concentration of the electrolyte (potassium hydroxide) solution, and diameter of the inner gold ring. However, a systematic investigation with the aim of determining the best conditions for fabricating micro/nano-scale tips with desired profiles has not been carried out yet. This study is aimed at obtaining controllable tungsten tip -particularly with respect to the radius of curvature and aspect ratio of tips (taper angle)-by altering the experimental conditions. A series of experiments were executed and the results were aggregated and analyzed using response surface methodology in order to identify the relationships between the tungsten tip characteristics and input parameters. The method proposed herein would prove to be suitable for a variety of applications in industries that require tungsten tips with a specific profile.

Design of characteristic parameters for controlling tungsten tip profile during electrochemical etching

International Nuclear Information System (INIS)

Le Duy Cuong; Duong, Thanh Hung; Kim, Huyn Chul

2014-01-01

Micro/nano-scale tungsten tips fabricated by electrochemical etching have many diverse industrial applications. The characteristic parameters of the tungsten tip profile include apex radius, taper angle, and aspect ratio. These parameters are governed by many factors including applied voltage, concentration of the electrolyte (potassium hydroxide) solution, and diameter of the inner gold ring. However, a systematic investigation with the aim of determining the best conditions for fabricating micro/nano-scale tips with desired profiles has not been carried out yet. This study is aimed at obtaining controllable tungsten tip -particularly with respect to the radius of curvature and aspect ratio of tips (taper angle)-by altering the experimental conditions. A series of experiments were executed and the results were aggregated and analyzed using response surface methodology in order to identify the relationships between the tungsten tip characteristics and input parameters. The method proposed herein would prove to be suitable for a variety of applications in industries that require tungsten tips with a specific profile

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

Science.gov (United States)

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

2010-07-28

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

Real space mapping of ionic diffusion and electrochemical activity in energy storage and conversion materials

Science.gov (United States)

Kalinin, Sergei V; Balke, Nina; Kumar, Amit; Dudney, Nancy J; Jesse, Stephen

2014-05-06

A method and system for probing mobile ion diffusivity and electrochemical reactivity on a nanometer length scale of a free electrochemically active surface includes a control module that biases the surface of the material. An electrical excitation signal is applied to the material and induces the movement of mobile ions. An SPM probe in contact with the surface of the material detects the displacement of mobile ions at the surface of the material. A detector measures an electromechanical strain response at the surface of the material based on the movement and reactions of the mobile ions. The use of an SPM tip to detect local deformations allows highly reproducible measurements in an ambient environment without visible changes in surface structure. The measurements illustrate effective spatial resolution comparable with defect spacing and well below characteristic grain sizes of the material.

Electrochemical behavior and voltammetric determination of acetaminophen based on glassy carbon electrodes modified with poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite films

International Nuclear Information System (INIS)

Zhu, Wencai; Huang, Hui; Gao, Xiaochun; Ma, Houyi

2014-01-01

Poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite film modified glassy carbon electrodes (4-ABA/ERGO/GCEs) were fabricated by a two-step electrochemical method. The electrochemical behavior of acetaminophen at the modified electrode was investigated by means of cyclic voltammetry. The results indicated that 4-ABA/ERGO composite films possessed excellent electrocatalytic activity towards the oxidation of acetaminophen. The electrochemical reaction of acetaminophen at 4-ABA/ERGO/GCE is proved to be a surface-controlled process involving the same number of protons and electrons. The voltammetric determination of acetaminophen performed with the 4-ABA/ERGO modified electrode presents a good linearity in the range of 0.1–65 μM with a low detection limit of 0.01 μM (S/N = 3). In the case of using the 4-ABA/ERGO/GCE, acetaminophen and dopamine can be simultaneously determined without mutual interference. Furthermore, the 4-ABA/ERGO/GCE has good reproducibility and stability, and can be used to determine acetaminophen in tablets. - Highlights: • The 4-ABA/ERGO/GCE was fabricated by a two-step electrochemical method. • Electrochemical behavior of acetaminophen at the 4-ABA/ERGO/GCE was investigated. • The electrochemical sensor exhibited a low detection limit and good selectivity. • This sensor was applied to the detection of acetaminophen in commercial tablets

Electrochemical behavior and voltammetric determination of acetaminophen based on glassy carbon electrodes modified with poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite films

Energy Technology Data Exchange (ETDEWEB)

Zhu, Wencai [Key Laboratory for Colloid and Interface Chemistry of State Education Ministry, School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China); School of Chemistry and Chemical Engineering, Qilu Normal University, Jinan 250013 (China); Huang, Hui; Gao, Xiaochun [Key Laboratory for Colloid and Interface Chemistry of State Education Ministry, School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China); Ma, Houyi, E-mail: hyma@sdu.edu.cn [Key Laboratory for Colloid and Interface Chemistry of State Education Ministry, School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China)

2014-12-01

Poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite film modified glassy carbon electrodes (4-ABA/ERGO/GCEs) were fabricated by a two-step electrochemical method. The electrochemical behavior of acetaminophen at the modified electrode was investigated by means of cyclic voltammetry. The results indicated that 4-ABA/ERGO composite films possessed excellent electrocatalytic activity towards the oxidation of acetaminophen. The electrochemical reaction of acetaminophen at 4-ABA/ERGO/GCE is proved to be a surface-controlled process involving the same number of protons and electrons. The voltammetric determination of acetaminophen performed with the 4-ABA/ERGO modified electrode presents a good linearity in the range of 0.1–65 μM with a low detection limit of 0.01 μM (S/N = 3). In the case of using the 4-ABA/ERGO/GCE, acetaminophen and dopamine can be simultaneously determined without mutual interference. Furthermore, the 4-ABA/ERGO/GCE has good reproducibility and stability, and can be used to determine acetaminophen in tablets. - Highlights: • The 4-ABA/ERGO/GCE was fabricated by a two-step electrochemical method. • Electrochemical behavior of acetaminophen at the 4-ABA/ERGO/GCE was investigated. • The electrochemical sensor exhibited a low detection limit and good selectivity. • This sensor was applied to the detection of acetaminophen in commercial tablets.

Aggregation of Individual Sensing Units for Signal Accumulation: Conversion of Liquid-Phase Colorimetric Assay into Enhanced Surface-Tethered Electrochemical Analysis.

Science.gov (United States)

Wei, Tianxiang; Dong, Tingting; Wang, Zhaoyin; Bao, Jianchun; Tu, Wenwen; Dai, Zhihui

2015-07-22

A novel concept is proposed for converting liquid-phase colorimetric assay into enhanced surface-tethered electrochemical analysis, which is based on the analyte-induced formation of a network architecture of metal nanoparticles (MNs). In a proof-of-concept trial, thymine-functionalized silver nanoparticle (Ag-T) is designed as the sensing unit for Hg(2+) determination. Through a specific T-Hg(2+)-T coordination, the validation system based on functionalized sensing units not only can perform well in a colorimetric Hg(2+) assay, but also can be developed into a more sensitive and stable electrochemical Hg(2+) sensor. In electrochemical analysis, the simple principle of analyte-induced aggregation of MNs can be used as a dual signal amplification strategy for significantly improving the detection sensitivity. More importantly, those numerous and diverse colorimetric assays that rely on the target-induced aggregation of MNs can be augmented to satisfy the ambitious demands of sensitive analysis by converting them into electrochemical assays via this approach.

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.

Electrochemically assisted deposition of strontium modified magnesium phosphate on titanium surfaces

Energy Technology Data Exchange (ETDEWEB)

Meininger, M. [Department for Functional Materials in Medicine and Dentistry, University of Würzburg, Pleicherwall 2, D-97070 Würzburg (Germany); Wolf-Brandstetter, C. [Max Bergmann Center for Biomaterials, Technical University of Dresden, Budapester Straße 27, D-01069 Dresden (Germany); Zerweck, J.; Wenninger, F.; Gbureck, U.; Groll, J. [Department for Functional Materials in Medicine and Dentistry, University of Würzburg, Pleicherwall 2, D-97070 Würzburg (Germany); Moseke, C., E-mail: claus.moseke@fmz.uni-wuerzburg.de [Department for Functional Materials in Medicine and Dentistry, University of Würzburg, Pleicherwall 2, D-97070 Würzburg (Germany)

2016-10-01

Electrochemically assisted deposition was utilized to produce ceramic coatings on the basis of magnesium ammonium phosphate (struvite) on corundum-blasted titanium surfaces. By the addition of defined concentrations of strontium nitrate to the coating electrolyte Sr{sup 2+} ions were successfully incorporated into the struvite matrix. By variation of deposition parameters it was possible to fabricate coatings with different kinetics of Sr{sup 2+} into physiological media, whereas the release of therapeutically relevant strontium doses could be sustained over several weeks. Morphological and crystallographic examinations of the immersed coatings revealed that the degradation of struvite and the release of Sr{sup 2+} ions were accompanied by a transformation of the coating to a calcium phosphate based phase similar to low-crystalline hydroxyapatite. These findings showed that strontium doped struvite coatings may provide a promising degradable coating system for the local application of strontium or other biologically active metal ions in the implant–bone interface. - Highlights: • Sr-doped struvite coatings have been deposited on titanium by electrochemically assisted deposition. • Sr content can be adjusted by means of process time, current density and pulse mode. • Sr-doped coatings release therapeutically relevant Sr doses in physiological media for several weeks. • During immersion in physiological media Sr-doped struvite coatings transform into a low crystalline calcium phosphate phase.

Stress distributions due to hydrogen concentrations in electrochemically charged and aged austenitic stainless steel

International Nuclear Information System (INIS)

Rozenak, P.; Loew, A.

2008-01-01

As a result of hydrogen concentration gradients in type austenitic stainless steels, formed during electrochemical charging and followed by hydrogen loss during aging, at room temperature, surface stresses were developed. These stresses were measured by X-ray technique and the crack formation thus induced could be studied using equilibrium stress equations. After various electrochemical charging and aging times, X-ray diffraction patterns obtained from samples indicated that the reflected and broadened diffraction peaks are the result of the formation of a non-uniform but continuous solid solution in the austenitic matrix. Since both hydrogen penetrations during charging and hydrogen release during aging are diffusion controlled processes and huge hydrogen concentration gradients in the thin surface layer, at depths comparable with the depth of X-ray penetration, are observed. The non-uniform hydrogen concentration in the austenitic matrix, results to the non-uniform expansion of the atomic microstructure and latter inevitably leads to the development of internal stresses. The internal stresses development formulae's are very similar to those relating to non-uniform heating of the materials, where thermal stresses appear due to non-uniform expansion or contraction. The relevant well developed theory is applicable in our case of non-uniform hydrogen concentrations in a solid solution of electrochemically charged and aged austenitic matrix. A few cracks were present on the surface after some minutes of electrochemical charging and the severity of cracking increased as hydrogen was lost during subsequent aging. This is consistent with the expectation of high compressive stresses in the bulk of the specimen during charging and high tensile surface stresses (at the level of 1 x 10 11 Pa) during the aging process. These stresses can induce the formation of surface cracks during the aging process after electrochemical charging in the AISI 316 stainless steel

Nanometer-scale mapping of irreversible electrochemical nucleation processes on solid Li-ion electrolytes

Science.gov (United States)

Kumar, Amit; Arruda, Thomas M.; Tselev, Alexander; Ivanov, Ilia N.; Lawton, Jamie S.; Zawodzinski, Thomas A.; Butyaev, Oleg; Zayats, Sergey; Jesse, Stephen; Kalinin, Sergei V.

2013-01-01

Electrochemical processes associated with changes in structure, connectivity or composition typically proceed via new phase nucleation with subsequent growth of nuclei. Understanding and controlling reactions requires the elucidation and control of nucleation mechanisms. However, factors controlling nucleation kinetics, including the interplay between local mechanical conditions, microstructure and local ionic profile remain inaccessible. Furthermore, the tendency of current probing techniques to interfere with the original microstructure prevents a systematic evaluation of the correlation between the microstructure and local electrochemical reactivity. In this work, the spatial variability of irreversible nucleation processes of Li on a Li-ion conductive glass-ceramics surface is studied with ~30 nm resolution. An increased nucleation rate at the boundaries between the crystalline AlPO4 phase and amorphous matrix is observed and attributed to Li segregation. This study opens a pathway for probing mechanisms at the level of single structural defects and elucidation of electrochemical activities in nanoscale volumes. PMID:23563856

Converting biomass waste into microporous carbon with simultaneously high surface area and carbon purity as advanced electrochemical energy storage materials

Science.gov (United States)

Sun, Fei; Wang, Lijie; Peng, Yiting; Gao, Jihui; Pi, Xinxin; Qu, Zhibin; Zhao, Guangbo; Qin, Yukun

2018-04-01

Developing carbon materials featuring both high accessible surface area and high structure stability are desirable to boost the performance of constructed electrochemical electrodes and devices. Herein, we report a new type of microporous carbon (MPC) derived from biomass waste based on a simple high-temperature chemical activation procedure. The optimized MPC-900 possesses microporous structure, high surface area, partially graphitic structure, and particularly low impurity content, which are critical features for enhancing carbon-based electrochemical process. The constructed MPC-900 symmetric supercapacitor exhibits high performances in commercial organic electrolyte such as widened voltage window up to 3 V and thereby high energy/power densities (50.95 Wh kg-1 at 0.44 kW kg-1; 25.3 Wh kg-1 at 21.5 kW kg-1). Furthermore, a simple melt infiltration method has been employed to enclose SnO2 nanocrystals onto the carbon matrix of MPC-900 as a high-performance lithium storage material. The obtained SnO2-MPC composite with ultrafine SnO2 nanocrystals delivers high capacities (1115 mAh g-1 at 0.2 A g-1; 402 mAh g-1 at 10 A g-1) and high-rate cycling lifespan of over 2000 cycles. This work not only develops a microporous carbon with high carbon purity and high surface area, but also provides a general platform for combining electrochemically active materials.

Control of electrochemical signals from quantum dots conjugated to organic materials by using DNA structure in an analog logic gate.

Science.gov (United States)

Chen, Qi; Yoo, Si-Youl; Chung, Yong-Ho; Lee, Ji-Young; Min, Junhong; Choi, Jeong-Woo

2016-10-01

Various bio-logic gates have been studied intensively to overcome the rigidity of single-function silicon-based logic devices arising from combinations of various gates. Here, a simple control tool using electrochemical signals from quantum dots (QDs) was constructed using DNA and organic materials for multiple logic functions. The electrochemical redox current generated from QDs was controlled by the DNA structure. DNA structure, in turn, was dependent on the components (organic materials) and the input signal (pH). Independent electrochemical signals from two different logic units containing QDs were merged into a single analog-type logic gate, which was controlled by two inputs. We applied this electrochemical biodevice to a simple logic system and achieved various logic functions from the controlled pH input sets. This could be further improved by choosing QDs, ionic conditions, or DNA sequences. This research provides a feasible method for fabricating an artificial intelligence system. Copyright © 2016 Elsevier B.V. All rights reserved.

The Effects of Different Electrode Types for Obtaining Surface Machining Shape on Shape Memory Alloy Using Electrochemical Machining

Science.gov (United States)

Choi, S. G.; Kim, S. H.; Choi, W. K.; Moon, G. C.; Lee, E. S.

2017-06-01

Shape memory alloy (SMA) is important material used for the medicine and aerospace industry due to its characteristics called the shape memory effect, which involves the recovery of deformed alloy to its original state through the application of temperature or stress. Consumers in modern society demand stability in parts. Electrochemical machining is one of the methods for obtained these stabilities in parts requirements. These parts of shape memory alloy require fine patterns in some applications. In order to machine a fine pattern, the electrochemical machining method is suitable. For precision electrochemical machining using different shape electrodes, the current density should be controlled precisely. And electrode shape is required for precise electrochemical machining. It is possible to obtain precise square holes on the SMA if the insulation layer controlled the unnecessary current between electrode and workpiece. If it is adjusting the unnecessary current to obtain the desired shape, it will be a great contribution to the medical industry and the aerospace industry. It is possible to process a desired shape to the shape memory alloy by micro controlling the unnecessary current. In case of the square electrode without insulation layer, it derives inexact square holes due to the unnecessary current. The results using the insulated electrode in only side show precise square holes. The removal rate improved in case of insulated electrode than others because insulation layer concentrate the applied current to the machining zone.

Effect of Etching Parameter on Pore Size and Porosity of Electrochemically Formed Nanoporous Silicon

Directory of Open Access Journals (Sweden)

Pushpendra Kumar

2007-01-01

Full Text Available The most common fabrication technique of porous silicon (PS is electrochemical etching of a crystalline silicon wafer in a hydrofluoric (HF acid-based solution. The electrochemical process allows for precise control of the properties of PS such as thickness of the porous layer, porosity, and average pore diameter. The control of these properties of PS was shown to depend on the HF concentration in the used electrolyte, the applied current density, and the thickness of PS. The change in pore diameter, porosity, and specific surface area of PS was investigated by measuring nitrogen sorption isotherms.

An electrochemical engineering technique to improve the corrosion resistance of some structural materials in lead-alloy coolants

International Nuclear Information System (INIS)

Tacica, M.; Andrei, V.; Rusu, O.; Coaca, E.; Minca, M.; Florea, S.; Oncioiu, G.

2013-01-01

The goal of this paper is to present some conclusions resulted from the literature studies referring to the materials potential to be used in Lead Fast Reactors (LFR), and the results obtained in the surface engineering field which can be used in our institute in order to obtain materials with appropriate properties for their use in LFR. In this context, the paper presents some preliminary results obtained in Surface Analysis Laboratory of INR Pitesti and research works in progress referring to: controlled modification of AISI 316 L surface by electrochemical plasma treatment (carburization, nitrocarburizings); electrodeposition of some protective thin-films based on Ni and Al obtained from ionic liquids; development of some procedures related to the activities involved in the behaviour evaluation, in LFR specific conditions, for material samples subjected to treatments by surface engineering techniques using the LEad COrrosion TEsting LOop (LECOTELO) test bench. The superficial structures obtained have been characterized by metallographic microscopy, X-Ray Photoemission Spectroscopy (XPS), Electrochemical Impedance Spectroscopy (EIS); the electrochemical techniques were used to evaluate the corrosion behaviour. The preliminary results have shown that the used electrochemical surface engineering techniques are appropriate in order to improve the mechanical properties and corrosion behaviour of AISI 316 L steel. (authors)

Towards an Electrochemical Immunosensor System with Temperature Control for Cytokine Detection.

Science.gov (United States)

Metzner, Julia; Luckert, Katrin; Lemuth, Karin; Hämmerle, Martin; Moos, Ralf

2018-04-24

The cytokine interleukin-13 (IL-13) plays a major role in airway inflammation and is a target of new anti-asthmatic drugs. Hence, IL-13 determination could be interesting in assessing therapy success. Thus, in this work an electrochemical immunosensor for IL-13 was developed and integrated into a fluidic system with temperature control for read-out. Therefore, two sets of results are presented. First, the sensor was set up in sandwich format on single-walled carbon nanotube electrodes and was read out by applying the hydrogen peroxide⁻hydroquinone⁻horseradish peroxidase (HRP) system. Second, a fluidic system was built up with an integrated heating function realized by Peltier elements that allowed a temperature-controlled read-out of the immunosensor in order to study the influence of temperature on the amperometric read-out. The sensor was characterized at the temperature optimum of HRP at 30 °C and at 12 °C as a reference for lower performance. These results were compared to a measurement without temperature control. At the optimum operation temperature of 30 °C, the highest sensitivity (slope) was obtained compared to lower temperatures and a limit of detection of 5.4 ng/mL of IL-13 was calculated. Taken together, this approach is a first step towards an automated electrochemical immunosensor platform and shows the potential of a temperature-controlled read-out.

Screen-printed carbon electrode modified on its surface with amorphous carbon nitride thin film: Electrochemical and morphological study

Energy Technology Data Exchange (ETDEWEB)

Ghamouss, F. [Universite de Nantes, UMR 6006-CNRS, FR-2465-CNRS, Laboratoire d' Analyse isotopique et Electrochimique de Metabolismes (LAIEM) (France); Tessier, P.-Y. [Universite de Nantes, UMR CNRS 6502, Institut des Materiaux Jean Rouxel - IMN Faculte des Sciences and des Techniques de Nantes, 2 rue de la Houssiniere, 44322 Nantes Cedex 3 (France); Djouadi, A. [Universite de Nantes, UMR CNRS 6502, Institut des Materiaux Jean Rouxel - IMN Faculte des Sciences and des Techniques de Nantes, 2 rue de la Houssiniere, 44322 Nantes Cedex 3 (France); Besland, M.-P. [Universite de Nantes, UMR CNRS 6502, Institut des Materiaux Jean Rouxel - IMN Faculte des Sciences and des Techniques de Nantes, 2 rue de la Houssiniere, 44322 Nantes Cedex 3 (France); Boujtita, M. [Universite de Nantes, UMR 6006-CNRS, FR-2465-CNRS, Laboratoire d' Analyse isotopique et Electrochimique de Metabolismes (LAIEM) (France)]. E-mail: mohammed.boujtita@univ-nantes.fr

2007-04-20

The surface of a screen-printed carbon electrode (SPCE) was modified by using amorphous carbon nitride (a-CN {sub x}) thin film deposited by reactive magnetron sputtering. Scanning electron microscopy and photoelectron spectroscopy measurements were used to characterise respectively the morphology and the chemical structure of the a-CN {sub x} modified electrodes. The incorporation of nitrogen in the amorphous carbon network was demonstrated by X ray photoelectron spectroscopy. The a-CN {sub x} layers were deposited on both carbon screen-printed electrode (SPCE) and silicon (Si) substrates. A comparative study showed that the nature of substrate, i.e. SPCE and Si, has a significant effect on both the surface morphology of deposited a-CN {sub x} film and their electrochemical properties. The improvement of the electrochemical reactivity of SPCE after a-CN {sub x} film deposition was highlighted both by comparing the shapes of voltammograms and calculating the apparent heterogeneous electron transfer rate constant.

Electrochemical hydrogen storage of Ti-V-based body-centered-cubic phase alloy surface-modified with AB5 nanoparticles

International Nuclear Information System (INIS)

Yu, X.B.; Walker, G.S.; Grant, D.M.; Wu, Z.; Xia, B.J.; Shen, J.

2005-01-01

A composite of Ti-V-based bcc phase alloy surface-modified with AB 5 nanoparticles was prepared by ball milling. The composite showed significantly improved electrochemical hydrogen release capacities. For example, the 30 min ball milled Ti-30V-15Mn-15Cr+10 wt %AB 5 showed a discharge capacity in the first cycle, at 353 K, of 886 mA h g -1 , corresponding to 3.38 wt % of hydrogen, with a 45 mA g -1 discharge current. It is thought that this high capacity is due to the enhanced electrochemical-catalytic activity from the alloy surface covered with AB 5 nanoparticles, which not only have better charge-discharge capacity themselves, acting as both an electrocatalyst and a microcurrent collector, but also result in the greatly enhanced hydrogen atomic diffusivities in the nanocrystalline relative to their conventional coarse-grained counterparts. These results provide new insight for use of Ti-V-based bcc phase alloy for high-energy batteries

Electrochemical modification of carbon electrode with benzylphosphonic groups

International Nuclear Information System (INIS)

Benjamin, Ossonon Diby; Weissmann, Martin; Bélanger, Daniel

2014-01-01

Electrochemical modification of carbon electrodes by aryl groups bearing a phosphonate terminal functionality was carried out by both electrochemical reduction of diazonium ions (diazobenzylphosphonic acid) and electrochemical oxidation of an amine (aminobenzylphosphonic acid). The grafting by electrochemical reduction of aryl diazonium ions was found to be more efficient. The surface concentration of phosphonate groups, estimated by electrochemical reduction of electrostatically bound Pb(II) ions, was found to be about 25% higher for the layer formed by electrochemical reduction of diazonium ions than for the layer formed by oxidation of the amine. The acid–base properties of the grafted films were slightly influenced by the grafting procedure and the difference in the apparent pK a was most likely related to the presence of the substrate –NH-aryl linkage for the film generated by amine oxidation. X-ray photoelectron spectroscopy was used to get some insight on the chemical species present at the carbon electrode surface. For both procedures, the films consist in mixture of at least two different covalently grafted species

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 control of a DNA Holliday Junction nanoswitch by Mg2+ ions.

Science.gov (United States)

Ferapontova, E E; Mountford, C P; Crain, J; Buck, A H; Dickinson, P; Beattie, J S; Ghazal, P; Terry, J G; Walton, A J; Mount, A R

2008-11-15

The molecular conformation of a synthetic branched, 4-way DNA Holliday junction (HJ) was electrochemically switched between the open and closed (stacked) conformers. Switching was achieved by electrochemically induced quantitative release of Mg(2+) ions from the oxidised poly(N-methylpyrrole) film (PPy), which contained polyacrylate as an immobile counter anion and Mg(2+) ions as charge compensating mobile cations. This increase in the Mg(2+) concentration screened the electrostatic repulsion between the widely separated arms in the open HJ configuration, inducing switching to the closed conformation. Upon electrochemical reduction of PPy, entrapment of Mg(2+) ions back into the PPy film induced the reverse HJ switching from the closed to open state. The conformational transition was monitored using fluorescence resonance energy transfer (FRET) between donor and acceptor dyes each located at the terminus of one of the arms. The demonstrated electrochemical control of the conformation of the used probe-target HJ complex, previously reported as a highly sequence specific nanodevice for detecting of unlabelled target [Buck, A.H., Campbell, C.J., Dickinson, P., Mountford, C.P., Stoquert, H.C., Terry, J.G., Evans, S.A.G., Keane, L., Su, T.J., Mount, A.R., Walton, A.J., Beattie, J.S., Crain, J., Ghazal, P., 2007. Anal. Chem., 79, 4724-4728], allows the development of electronically addressable DNA nanodevices and label-free gene detection assays.

Constructing superhydrophobic WO3@TiO2 nanoflake surface beyond amorphous alloy against electrochemical corrosion on iron steel

Science.gov (United States)

Yu, S. Q.; Ling, Y. H.; Wang, R. G.; Zhang, J.; Qin, F.; Zhang, Z. J.

2018-04-01

To eliminate harmful localized corrosion, a new approach by constructing superhydrophobic WO3@TiO2 hierarchical nanoflake surface beyond FeW amorphous alloy formed on stainless steel was proposed. Facile dealloying and liquid deposition was employed at low temperature to form a nanostructured layer composing inner WO3 nanoflakes coated with TiO2 nanoparticles (NPs) layer. After further deposition of PFDS on nanoflakes, the contact angle reached 162° while the corrosion potential showed a negative shift of 230 mV under illumination, resulting in high corrosion resistance in 3.5 wt% NaCl solution. The tradeoff between superhydrophobic surface and photo-electro response was investigated. It was found that this surface feature makes 316 SS be immune to localized corrosion and a pronounced photo-induced process of electron storage/release as well as the stability of the functional layer were detected with or without illumination, and the mechanism behind this may be related to the increase of surface potential due to water repellence and the delayed cathodic protection of semiconducting coating derived mainly from the valence state changes of WO3. This study demonstrates a simple and low-cost electrochemical approach for protection of steel and novel means to produce superhydrophobic surface and cathodic protection with controllable electron storage/release on engineering scale.

Materials for electrochemical capacitors

Science.gov (United States)

Simon, Patrice; Gogotsi, Yury

2008-11-01

Electrochemical capacitors, also called supercapacitors, store energy using either ion adsorption (electrochemical double layer capacitors) or fast surface redox reactions (pseudo-capacitors). They can complement or replace batteries in electrical energy storage and harvesting applications, when high power delivery or uptake is needed. A notable improvement in performance has been achieved through recent advances in understanding charge storage mechanisms and the development of advanced nanostructured materials. The discovery that ion desolvation occurs in pores smaller than the solvated ions has led to higher capacitance for electrochemical double layer capacitors using carbon electrodes with subnanometre pores, and opened the door to designing high-energy density devices using a variety of electrolytes. Combination of pseudo-capacitive nanomaterials, including oxides, nitrides and polymers, with the latest generation of nanostructured lithium electrodes has brought the energy density of electrochemical capacitors closer to that of batteries. The use of carbon nanotubes has further advanced micro-electrochemical capacitors, enabling flexible and adaptable devices to be made. Mathematical modelling and simulation will be the key to success in designing tomorrow's high-energy and high-power devices.

Influence of the Surface Layer on the Electrochemical Deposition of Metals and Semiconductors into Mesoporous Silicon

Energy Technology Data Exchange (ETDEWEB)

Chubenko, E. B., E-mail: eugene.chubenko@gmail.com; Redko, S. V.; Sherstnyov, A. I.; Petrovich, V. A.; Kotov, D. A.; Bondarenko, V. P. [Belarusian State University of Information and RadioElectronics (Belarus)

2016-03-15

The influence of the surface layer on the process of the electrochemical deposition of metals and semiconductors into porous silicon is studied. It is shown that the surface layer differs in structure and electrical characteristics from the host porous silicon bulk. It is established that a decrease in the conductivity of silicon crystallites that form the surface layer of porous silicon has a positive effect on the process of the filling of porous silicon with metals and semiconductors. This is demonstrated by the example of nickel and zinc oxide. The effect can be used for the formation of nanocomposite materials on the basis of porous silicon and nanostructures with a high aspect ratio.

Influence of the Surface Layer on the Electrochemical Deposition of Metals and Semiconductors into Mesoporous Silicon

International Nuclear Information System (INIS)

Chubenko, E. B.; Redko, S. V.; Sherstnyov, A. I.; Petrovich, V. A.; Kotov, D. A.; Bondarenko, V. P.

2016-01-01

The influence of the surface layer on the process of the electrochemical deposition of metals and semiconductors into porous silicon is studied. It is shown that the surface layer differs in structure and electrical characteristics from the host porous silicon bulk. It is established that a decrease in the conductivity of silicon crystallites that form the surface layer of porous silicon has a positive effect on the process of the filling of porous silicon with metals and semiconductors. This is demonstrated by the example of nickel and zinc oxide. The effect can be used for the formation of nanocomposite materials on the basis of porous silicon and nanostructures with a high aspect ratio.

Advanced Electrochemical Machining (ECM) for tungsten surface micro-structuring in blanket applications

International Nuclear Information System (INIS)

Holstein, Nils; Krauss, Wolfgang; Konys, Jürgen; Heuer, Simon; Weber, Thomas

2016-01-01

Highlights: • Electrochemical Machining is an appropriate tool for tungsten shaping. • Progress in shaping achieved by combination of ECM with advanced micro-lithography. • Application in First Wall for connection of plasma facing material to breeder blanket. • Successful development of adhesion promotors by ECM for plasma spraying interlayers. • Microstructure electrochemical manufacturing of tungsten in sizes of 100 μm achieved. - Abstract: Plasma facing components for fusion applications must have to exhibit long-term stability under extreme physical conditions, and therefore any material imperfections caused by mechanical and/or thermal stresses in the shaping processes cannot be tolerated due to a high risk of possible technical failures under fusion conditions. To avoid such defects, the method of Electrochemical Machining (ECM) enables a complete defect-free processing of removal of tungsten material during the desired shaping, also for high penetration depths. Furthermore, supported by lithographic mask pretreatment, three-dimensional distinct geometric structures can be positive-imaged via the directional galvanic dissolution applying M-ECM process into the tungsten bulk material. New required applications for tungsten components, e.g. as adhesion promotors in W-surfaces to enable sure grip and bonding of thick plasma-spraying layers for blanket components, will define the way of further miniaturization of well-established millimeter dimensioned M-ECM shaping processes to dimensions of 100 μm and furthermore down to 50 μm. Besides current M-ECM limits the article describes inevitable needs of further developments for mask resists, mask materials and the resulting ECM parameters, to reach the needed accuracy in tungsten microstructure. The achieved progress and observed correlations of processing parameters will be manifested by produced demonstrators made by the new “μM”-ECM process.

Advanced Electrochemical Machining (ECM) for tungsten surface micro-structuring in blanket applications

Energy Technology Data Exchange (ETDEWEB)

Holstein, Nils, E-mail: nils.holstein@kit.edu [Karlsruhe Institute of Technology, Hermann-von-Helmholtz-Platz 1, D-76344 Eggenstein-Leopoldshafen, Baden-Württemberg (Germany); Krauss, Wolfgang; Konys, Jürgen [Karlsruhe Institute of Technology, Hermann-von-Helmholtz-Platz 1, D-76344 Eggenstein-Leopoldshafen, Baden-Württemberg (Germany); Heuer, Simon; Weber, Thomas [Research Center Jülich, Institute of Energy- and Climate Research – Plasma Physics (IEK-4), D-52425 Jülich (Germany)

2016-11-01

Highlights: • Electrochemical Machining is an appropriate tool for tungsten shaping. • Progress in shaping achieved by combination of ECM with advanced micro-lithography. • Application in First Wall for connection of plasma facing material to breeder blanket. • Successful development of adhesion promotors by ECM for plasma spraying interlayers. • Microstructure electrochemical manufacturing of tungsten in sizes of 100 μm achieved. - Abstract: Plasma facing components for fusion applications must have to exhibit long-term stability under extreme physical conditions, and therefore any material imperfections caused by mechanical and/or thermal stresses in the shaping processes cannot be tolerated due to a high risk of possible technical failures under fusion conditions. To avoid such defects, the method of Electrochemical Machining (ECM) enables a complete defect-free processing of removal of tungsten material during the desired shaping, also for high penetration depths. Furthermore, supported by lithographic mask pretreatment, three-dimensional distinct geometric structures can be positive-imaged via the directional galvanic dissolution applying M-ECM process into the tungsten bulk material. New required applications for tungsten components, e.g. as adhesion promotors in W-surfaces to enable sure grip and bonding of thick plasma-spraying layers for blanket components, will define the way of further miniaturization of well-established millimeter dimensioned M-ECM shaping processes to dimensions of 100 μm and furthermore down to 50 μm. Besides current M-ECM limits the article describes inevitable needs of further developments for mask resists, mask materials and the resulting ECM parameters, to reach the needed accuracy in tungsten microstructure. The achieved progress and observed correlations of processing parameters will be manifested by produced demonstrators made by the new “μM”-ECM process.

Electrochemical behavior and voltammetric determination of acetaminophen based on glassy carbon electrodes modified with poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite films.

Science.gov (United States)

Zhu, Wencai; Huang, Hui; Gao, Xiaochun; Ma, Houyi

2014-12-01

Poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite film modified glassy carbon electrodes (4-ABA/ERGO/GCEs) were fabricated by a two-step electrochemical method. The electrochemical behavior of acetaminophen at the modified electrode was investigated by means of cyclic voltammetry. The results indicated that 4-ABA/ERGO composite films possessed excellent electrocatalytic activity towards the oxidation of acetaminophen. The electrochemical reaction of acetaminophen at 4-ABA/ERGO/GCE is proved to be a surface-controlled process involving the same number of protons and electrons. The voltammetric determination of acetaminophen performed with the 4-ABA/ERGO modified electrode presents a good linearity in the range of 0.1-65 μM with a low detection limit of 0.01 μM (S/N=3). In the case of using the 4-ABA/ERGO/GCE, acetaminophen and dopamine can be simultaneously determined without mutual interference. Furthermore, the 4-ABA/ERGO/GCE has good reproducibility and stability, and can be used to determine acetaminophen in tablets. Copyright © 2014 Elsevier B.V. All rights reserved.

Recent Development of Advanced Electrode Materials by Atomic Layer Deposition for Electrochemical Energy Storage.

Science.gov (United States)

Guan, Cao; Wang, John

2016-10-01

Electrode materials play a decisive role in almost all electrochemical energy storage devices, determining their overall performance. Proper selection, design and fabrication of electrode materials have thus been regarded as one of the most critical steps in achieving high electrochemical energy storage performance. As an advanced nanotechnology for thin films and surfaces with conformal interfacial features and well controllable deposition thickness, atomic layer deposition (ALD) has been successfully developed for deposition and surface modification of electrode materials, where there are considerable issues of interfacial and surface chemistry at atomic and nanometer scale. In addition, ALD has shown great potential in construction of novel nanostructured active materials that otherwise can be hardly obtained by other processing techniques, such as those solution-based processing and chemical vapor deposition (CVD) techniques. This review focuses on the recent development of ALD for the design and delivery of advanced electrode materials in electrochemical energy storage devices, where typical examples will be highlighted and analyzed, and the merits and challenges of ALD for applications in energy storage will also be discussed.

Control of surface quality of sub-millimeter cylindrical gold targets

International Nuclear Information System (INIS)

Zhang Yunwang; Du Kai; Wan Xiaobo; Xiao Jiang; Zheng Wei; Zhang Lin; Sun Jingyuan; Chen Jing

2010-01-01

The morphology, composition and causes of defects are analyzed to reduce defects on the gold layer prepared by electrochemical deposition from sulfite solution, and to improve the surface quality of sub-millimeter cylindrical gold targets, by means of SEM and EDS. The effects of current density, metallic impurity, organic pollution, pre-deposition parameters and mandrel quality on the quality of the gold plating are discussed, along with their mechanisms. The result indicates that the current density must be controlled strictly. The optimal current density ranges from 2.4 to 3.2 mA/cm 2 when the concentration of gold ranges from 13 to 22 g/L, and from 2.0 to 2.6 mA/ cm 2 when the concentration of gold ranges from 5 to 13 g/L. The parameters of predeposition must be optimized and the predeposition time should be no longer than 1 minute to improve the surface quality. In addition, organic pollution should be removed from the bath, and the mandrels should be of good quality without oxide on their surfaces. (authors)

Superhydrophilic graphite surfaces and water-dispersible graphite colloids by electrochemical exfoliation

Energy Technology Data Exchange (ETDEWEB)

Li, Yueh-Feng [Department of Chemical and Materials Engineering, National Central University, Jhongli, 320 Taiwan (China); Chen, Shih-Ming; Lai, Wei-Hao [Materials and Chemical Research Laboratories, Industrial Technology Research Institute, Chutung, Hsinchu, 31040 Taiwan (China); Sheng, Yu-Jane [Department of Chemical Engineering, National Taiwan University, Taipei, 106 Taiwan (China); Tsao, Heng-Kwong [Department of Chemical and Materials Engineering, Department of Physics, National Central University, Jhongli, 320 Taiwan (China)

2013-08-14

Superhydrophilic graphite surfaces and water-dispersible graphite colloids are obtained by electrochemical exfoliation with hydrophobic graphite electrodes. Such counterintuitive characteristics are caused by partial oxidation and investigated by examining both graphite electrodes and exfoliated particles after electrolysis. The extent of surface oxidation can be explored through contact angle measurement, scanning electron microscope, electrical sheet resistance, x-ray photoelectron spectroscopy, zeta-potential analyzer, thermogravimetric analysis, UV-visible, and Raman spectroscopy. The degree of wettability of the graphite anode can be altered by the electrolytic current and time. The water contact angle declines generally with increasing the electrolytic current or time. After a sufficient time, the graphite anode becomes superhydrophilic and its hydrophobicity can be recovered by peeling with adhesive tape. This consequence reveals that the anodic graphite is oxidized by oxygen bubbles but the oxidation just occurs at the outer layers of the graphite sheet. Moreover, the characteristics of oxidation revealed by UV peak shift, peak ratio between D and G bands, and negative zeta-potential indicate the presence of graphite oxide on the outer shell of the exfoliated colloids. However, thermogravimetric analysis for the extent of decomposition of oxygen functional groups verifies that the amount of oxygen groups is significantly less than that of graphite oxide prepared via Hummer method. The structure of this partially oxidized graphite may consist of a graphite core covered with an oxidized shell. The properties of the exfoliated colloids are also influenced by pH of the electrolytic solution. As pH is increased, the extent of oxidation descends and the thickness of oxidized shell decreases. Those results reveal that the degree of oxidation of exfoliated nanoparticles can be manipulated simply by controlling pH.

Surface modification of β-Type titanium alloy by electrochemical potential pulse polarization

International Nuclear Information System (INIS)

Fujimoto, Shinji; Raman, Vedarajan; Tsuchiya, Hiroaki

2009-01-01

In the present work, we report the formation of a porous oxide/hydroxide surface layer on the Ti-29Nb-13Ta-4.6Zr (TNTZ) alloy achieved by the combination of an alkali immersion and a potential pulse polarisation process. The alkali treatment has been employed for pure titanium to produce amorphous and porous layer prior to hydroxyapatite (HAp) growth. But, in the case of TNTZ, immersion in 5M NaOH at the open circuit potential (OCP) at 60 deg. C for 24 hours, did not yield any uniform layer, instead a thick deposited layer with highly cracked one. The cracks were attributed to the growth of a tantalum enriched particulate. In order to avoid the crack formation, the electrochemical behaviour of the alloy and the pure alloying elements (Ti, Nb, Ta and Zr) was investigated to produce a uniform surface with the application of a square wave modulated potential pulse polarization, leading to the formation of a relatively uniform porous layer on the alloy.

Surface modification of {beta}-Type titanium alloy by electrochemical potential pulse polarization

Energy Technology Data Exchange (ETDEWEB)

Fujimoto, Shinji; Raman, Vedarajan; Tsuchiya, Hiroaki [Division of Materials and Manufacturing Science, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-0871 (Japan)], E-mail: fujimoto@mat.eng.osaka-u.ac.jp

2009-05-01

In the present work, we report the formation of a porous oxide/hydroxide surface layer on the Ti-29Nb-13Ta-4.6Zr (TNTZ) alloy achieved by the combination of an alkali immersion and a potential pulse polarisation process. The alkali treatment has been employed for pure titanium to produce amorphous and porous layer prior to hydroxyapatite (HAp) growth. But, in the case of TNTZ, immersion in 5M NaOH at the open circuit potential (OCP) at 60 deg. C for 24 hours, did not yield any uniform layer, instead a thick deposited layer with highly cracked one. The cracks were attributed to the growth of a tantalum enriched particulate. In order to avoid the crack formation, the electrochemical behaviour of the alloy and the pure alloying elements (Ti, Nb, Ta and Zr) was investigated to produce a uniform surface with the application of a square wave modulated potential pulse polarization, leading to the formation of a relatively uniform porous layer on the alloy.

Preparation of Atomically Flat Si(111)-H Surfaces in Aqueous Ammonium Fluoride Solutions Investigated by Using Electrochemical, In Situ EC-STM and ATR-FTIR Spectroscopic Methods

International Nuclear Information System (INIS)

Bae, Sang Eun; Oh, Mi Kyung; Min, Nam Ki; Paek, Se Hwan; Hong, Suk In; Lee, Chi-Woo J.

2004-01-01

Electrochemical, in situ electrochemical scanning tunneling microscope (EC-STM), and attenuated total reflectance-FTIR (ATR-FTIR) spectroscopic methods were employed to investigate the preparation of atomically flat Si(111)-H surface in ammonium fluoride solutions. Electrochemical properties of atomically flat Si(111)-H surface were characterized by anodic oxidation and cathodic hydrogen evolution with the open circuit potential (OCP) of ca. .0.4 V in concentrated ammonium fluoride solutions. As soon as the natural oxide-covered Si(111) electrode was immersed in fluoride solutions, OCP quickly shifted to near .1 V, which was more negative than the flat band potential of silicon surface, indicating that the surface silicon oxide had to be dissolved into the solution. OCP changed to become less negative as the oxide layer was being removed from the silicon surface. In situ EC-STM data showed that the surface was changed from the initial oxide covered silicon to atomically rough hydrogen-terminated surface and then to atomically flat hydrogen terminated surface as the OCP moved toward less negative potentials. The atomically flat Si(111)-H structure was confirmed by in situ EC-STM and ATR-FTIR data. The dependence of atomically flat Si(111)-H terrace on mis-cut angle was investigated by STM, and the results agreed with those anticipated by calculation. Further, the stability of Si(111)-H was checked by STM in ambient laboratory conditions

Multilevel electrochemical signal detections of metalloprotein heterolayers for bioelectronic device

Energy Technology Data Exchange (ETDEWEB)

Chung, Yong-Ho; Yoo, Si-Youl; Lee, Taek [Department of Chemical and Biomolecular Engineering, Sogang University, 35 Baekbeom-ro(Sinsu-dong), Mapo-gu, Seoul 121-742 (Korea, Republic of); Lee, Hun Joo [Interdisciplinary Program of Integrated Biotechnology, Sogang University, 35 Baekbeomro(Sinsu-dong), Mapo-gu, Seoul 121-742 (Korea, Republic of); Min, Junhong [School of Integrative Engineering, Chung-Ang University, Heukseok-dong, Dongjak-gu, Seoul 156-756 (Korea, Republic of); Choi, Jeong-Woo, E-mail: jwchoi@sogang.ac.kr [Department of Chemical and Biomolecular Engineering, Sogang University, 35 Baekbeom-ro(Sinsu-dong), Mapo-gu, Seoul 121-742 (Korea, Republic of); Interdisciplinary Program of Integrated Biotechnology, Sogang University, 35 Baekbeomro(Sinsu-dong), Mapo-gu, Seoul 121-742 (Korea, Republic of)

2014-01-31

In the present study, we investigated the simultaneous detection of multilevel electrochemical signals from various metalloprotein heterolayers for the bioelectronic devices. A layer-by-layer assembly method based on simple electrostatic interaction was introduced to form protein bilayers. The gold substrate was modified with poly (ethylene glycol) thiol acid as the precursor, which introduced negative charges to the surface. Based on the isoelectric point, net-charge controlled metalloproteins by pH adjustment were sequentially immobilized on this negatively charged substrate. The degree of protein immobilization on the gold substrate was confirmed by surface plasmon resonance spectroscopy, and the surface topology changes due to the protein immobilization were confirmed by atomic force microscopy. Redox signals in the protein layers were measured by cyclic voltammetry. As a result, various redox signals generated from different metalloproteins on a single electrode were monitored. This proposed method for the detection of multi-level electrochemical signals can be directly applied to bioelectronic devices that store multi-information in a single electrode. - Highlights: • We fabricated heterolayers composed of various metalloproteins. • Metalloproteins were immobilized by layer-by-layer assembly. • The degree of immobilization was controlled by the net charge of metalloproteins. • Various redox signals generated from heterolayers were well monitored.

Electrochemical oxidation of organic waste

International Nuclear Information System (INIS)

Almon, A.C.; Buchanan, B.R.

1990-01-01

Both silver catalyzed and direct electrochemical oxidation of organic species are examined in analytical detail. This paper describes the mechanisms, reaction rates, products, intermediates, capabilities, limitations, and optimal reaction conditions of the electrochemical destruction of organic waste. A small bench-top electrocell being tested for the treatment of small quantities of laboratory waste is described. The 200-mL electrochemical cell used has a processing capacity of 50 mL per day, and can treat both radioactive and nonradioactive waste. In the silver catalyzed process, Ag(I) is electrochemically oxidized to Ag(II), which attacks organic species such as tributylphosphate (TBP), tetraphenylborate (TPB), and benzene. In direct electrochemical oxidation, the organic species are destroyed at the surface of the working electrode without the use of silver as an electron transfer agent. This paper focuses on the destruction of tributylphosphate (TBP), although several organic species have been destroyed using this process. The organic species are converted to carbon dioxide, water, and inorganic acids

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.

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

Organic Electrochemical Transistors for the Detection of Cell Surface Glycans.

Science.gov (United States)

Chen, Lizhen; Fu, Ying; Wang, Naixiang; Yang, Anneng; Li, Yuanzhe; Wu, Jie; Ju, Huangxian; Yan, Feng

2018-05-23

Cell surface glycans play critical roles in diverse biological processes, such as cell-cell communication, immunity, infection, development, and differentiation. Their expressions are closely related to cancer growth and metastasis. This work demonstrates an organic electrochemical transistor (OECT)-based biosensor for the detection of glycan expression on living cancer cells. Herein, mannose on human breast cancer cells (MCF-7) as the target glycan model, poly dimethyl diallyl ammonium chloride-multiwall carbon nanotubes (PDDA-MWCNTs) as the loading interface, concanavalin A (Con A) with active mannose binding sites, aptamer and horseradish peroxidase co-immobilized gold nanoparticles (HRP-aptamer-Au NPs) as specific nanoprobes are used to fabricate the OECT biosensor. In this strategy, PDDA-MWCNT interfaces can enhance the loading of Con A, and the target cells can be captured through Con A via active mannose binding sites. Thus, the expression of cell surface can be reflected by the amount of cells captured on the gate. Specific nanoprobes are introduced to the captured cells to produce an OECT signal because of the reduction of hydrogen peroxide catalyzed by HRP conjugated on Au nanoparticles, while the aptamer on nanoprobes can selectively recognize the MCF-7 cells. It is reasonable that more target cells are captured on the gate electrode, more HRP-nanoprobes are loaded thus a larger signal response. The device shows an obvious response to MCF-7 cells down to 10 cells/μL and can be used to selectively monitor the change of mannose expression on cell surfaces upon a treatment with the N-glycan inhibitor. The OECT-based biosensor is promising for the analysis of glycan expressions on the surfaces of different types of cells.

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.

Measurement of the Ru surface content of electrodeposited PtRu electrodes with the electrochemical quartz crystal microbalance: implications for methanol and CO electrooxidation

NARCIS (Netherlands)

Frelink, T.; Visscher, W.; Veen, van J.A.R.

1996-01-01

To obtain the surface content of Ru in rough electrocodeposited PtRu electrodes, the mass change of a Pt electrode during Ru deposition was measured with the electrochemical quartz crystal microbalance (EQCMB). It is shown that there is a correlation between the potential of the surface oxide

The nanostructure of microbially-reduced graphene oxide fosters thick and highly-performing electrochemically-active biofilms

Science.gov (United States)

Virdis, Bernardino; Dennis, Paul G.

2017-07-01

Biofilms of electrochemically-active organisms are used in microbial electrochemical technologies (METs) to catalyze bioreactions otherwise not possible at bare electrodes. At present, however, achievable current outputs are still below levels considered sufficient for economic viability of large-scale METs implementations. Here, we report three-dimensional, self-aggregating biofilm composites comprising of microbial cells embedded with microbially-reduced graphene oxide (rGO) nanoparticles to form a thick macro-porous network with superior electrochemical properties. In the presence of metabolic substrate, these hybrid biofilms are capable of producing up to five times more catalytic current than the control biofilms. Cyclic voltammetry, linear sweep voltammetry, and electrochemical impedance spectroscopy, show that in spite of the increased thickness, the biofilms amended with GO display lower polarization/charge transfer resistance compared to the controls, which we ascribe to the incorporation of rGO into the biofilms, which (1) promotes fast electron transfer, yet conserving a macroporous structure that allows free diffusion of reactants and products, and (2) enhances the interfacial dynamics by allowing a higher load of microbial cells per electrode surface area. These results suggest an easy-to-apply and cost-effective method to produce high-performing electrochemically-active biofilms in situ.

Modulation of nitrogen vacancy charge state and fluorescence in nanodiamonds using electrochemical potential.

Science.gov (United States)

Karaveli, Sinan; Gaathon, Ophir; Wolcott, Abraham; Sakakibara, Reyu; Shemesh, Or A; Peterka, Darcy S; Boyden, Edward S; Owen, Jonathan S; Yuste, Rafael; Englund, Dirk

2016-04-12

The negatively charged nitrogen vacancy (NV(-)) center in diamond has attracted strong interest for a wide range of sensing and quantum information processing applications. To this end, recent work has focused on controlling the NV charge state, whose stability strongly depends on its electrostatic environment. Here, we demonstrate that the charge state and fluorescence dynamics of single NV centers in nanodiamonds with different surface terminations can be controlled by an externally applied potential difference in an electrochemical cell. The voltage dependence of the NV charge state can be used to stabilize the NV(-) state for spin-based sensing protocols and provides a method of charge state-dependent fluorescence sensing of electrochemical potentials. We detect clear NV fluorescence modulation for voltage changes down to 100 mV, with a single NV and down to 20 mV with multiple NV centers in a wide-field imaging mode. These results suggest that NV centers in nanodiamonds could enable parallel optical detection of biologically relevant electrochemical potentials.

Modulation of nitrogen vacancy charge state and fluorescence in nanodiamonds using electrochemical potential

Science.gov (United States)

Karaveli, Sinan; Gaathon, Ophir; Wolcott, Abraham; Sakakibara, Reyu; Shemesh, Or A.; Peterka, Darcy S.; Boyden, Edward S.; Owen, Jonathan S.; Yuste, Rafael; Englund, Dirk

2016-04-01

The negatively charged nitrogen vacancy (NV-) center in diamond has attracted strong interest for a wide range of sensing and quantum information processing applications. To this end, recent work has focused on controlling the NV charge state, whose stability strongly depends on its electrostatic environment. Here, we demonstrate that the charge state and fluorescence dynamics of single NV centers in nanodiamonds with different surface terminations can be controlled by an externally applied potential difference in an electrochemical cell. The voltage dependence of the NV charge state can be used to stabilize the NV- state for spin-based sensing protocols and provides a method of charge state-dependent fluorescence sensing of electrochemical potentials. We detect clear NV fluorescence modulation for voltage changes down to 100 mV, with a single NV and down to 20 mV with multiple NV centers in a wide-field imaging mode. These results suggest that NV centers in nanodiamonds could enable parallel optical detection of biologically relevant electrochemical potentials.

Controlling formation of single-molecule junctions by electrochemical reduction of diazonium terminal groups.

Science.gov (United States)

Hines, Thomas; Díez-Pérez, Ismael; Nakamura, Hisao; Shimazaki, Tomomi; Asai, Yoshihiro; Tao, Nongjian

2013-03-06

We report controlling the formation of single-molecule junctions by means of electrochemically reducing two axialdiazonium terminal groups on a molecule, thereby producing direct Au-C covalent bonds in situ between the molecule and gold electrodes. We report a yield enhancement in molecular junction formation as the electrochemical potential of both junction electrodes approach the reduction potential of the diazonium terminal groups. Step length analysis shows that the molecular junction is significantly more stable, and can be pulled over a longer distance than a comparable junction created with amine anchoring bonds. The stability of the junction is explained by the calculated lower binding energy associated with the direct Au-C bond compared with the Au-N bond.

Novel Graphene-Gold Hybrid Nanostructures Constructed via Sulfur Modified Graphene: Preparation and Characterization by Surface and Electrochemical Techniques

International Nuclear Information System (INIS)

Shervedani, Reza Karimi; Amini, Akbar

2014-01-01

Graphical abstract: Graphene nanosheet-gold nanoparticles (GNs-AuNPs) hybrid has been fabricated from sulfur-modified graphene nanosheets (S-GNs) impregnated with HAuCl4 as Au precursor. Application of the GNs-AuNPs hybrid in electrochemical biosensing was demonstrated by immobilization of glucose oxidase as a model on the surface of GCE-ATP-GNs-AuNPs, and then, using it for sensing of glucose. - Highlights: • A new hybrid of GNs-AuNPs is synthesized by using sulfur-modified graphene. • Stability of the hybrid is exceptionally improved in comparison with previous works. • Aminothiophenol mediated fabrication and stabilization of GNs-AuNPs on GCE electrode. • High electrocatalytic activity was observed for O 2 reduction by hybrid. • Activity of the hybrid was originated from synergistic effect and surface roughness. - Abstract: A novel and uniform graphene nanosheet-gold nanoparticles (GNs-AuNPs) hybrid has been fabricated from sulfur-modified graphene nanosheets (S-GNs) impregnated with HAuCl 4 as Au precursor. Physicochemical and morphological characteristics of the GNs-AuNPs hybrids were investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), surface Raman spectroscopy (SRS), and high resolution transmission electron microscopy (HRTEM). The results of the XRD and HRTEM demonstrated well dispersed Au nanoparticles on GNs with an average particle size of less than 10 nm and a narrow size distribution of 6 to 8 nm. A film of GNs-AuNPs hybrid was constructed on a glassy carbon electrode (GCE) through layer-by-layer (LBL) assembly of 4-aminothiphenol (ATP) on GCE, and then, transferring the hybrid to the sulfur function of ATP to form GCE-ATP-GNs-AuNPs modified surface. Application of the GNs-AuNPs hybrid in electrochemical biosensing was demonstrated by immobilization of glucose oxidase (GOx) as a model on the surface of GCE-ATP-GNs-AuNPs, and then, using it for sensing of glucose. The biosensor exhibited a wide linear response

Electrochemical Machining – Special Equipment and Applications in Aircraft Industry

Directory of Open Access Journals (Sweden)

Ruszaj Adam

2016-06-01

Full Text Available Electrochemical machining is an unique method of shaping in which, for optimal parameters tool has no wear, surface layer properties after machining are similar to the core material and surface quality and accuracy increase together with material removal rate increase. Such advantages of electrochemical machining, besides of some ecological problems, create industry interest in the range of manufacturing elements made of materials with special properties (i.e. turbine blades of flow aircrafts engines. In the paper the nowadays possibilities and recent practical application of electrochemical machining in aircraft have been presented.

Evaluation of chemically modified Ti–5Mo–3Fe alloy surface: Electrochemical aspects and in vitro bioactivity on MG63 cells

Energy Technology Data Exchange (ETDEWEB)

Kumar, A. Madhan [Center of Research Excellence in Corrosion, King Fahd University of Petroleum and Minerals, Dhahran 31261 (Saudi Arabia); Sudhagar, P. [Energy Materials Laboratory, WCU Program Department of Energy Engineering, Hanyang University, Seoul 133-791 (Korea, Republic of); Ramakrishna, Suresh [Graduate School of Biomedical Science and Engineering/College of Medicine, Hanyang University, Sungdong-gu, Seoul (Korea, Republic of); Kang, Yong Soo [Energy Materials Laboratory, WCU Program Department of Energy Engineering, Hanyang University, Seoul 133-791 (Korea, Republic of); Kim, Hyongbum [Graduate School of Biomedical Science and Engineering/College of Medicine, Hanyang University, Sungdong-gu, Seoul (Korea, Republic of); Gasem, Zuhair M. [Center of Research Excellence in Corrosion, King Fahd University of Petroleum and Minerals, Dhahran 31261 (Saudi Arabia); Rajendran, N., E-mail: nrajendran@annauniv.edu [Department of Chemistry, Anna University, Chennai (India)

2014-07-01

Ti–5Mo–3Fe (TMF) alloy is a newly developed β-titanium alloy with low modulus, and it has been deemed as suitable material for dental or orthopaedic implant. The aim of the present study is to evaluate the effect of alkali and hydrogen peroxide treatment on the corrosion and biological performance of TMF surface. The phases, morphology with chemical composition and topography of the treated surface were examined by X-ray diffraction, scanning electron microscopy (SEM) coupled with energy dispersive X-ray (EDAX) analysis and atomic force microscopy (AFM), respectively. Micro hardness of treated substrates was measured using Vicker's micro hardness method. The electrochemical studies were carried out using potentiodynamic polarisation and electrochemical impedance spectroscopy (EIS) measurements. In order to describe the bio-activity, contact angle measurements, in vitro characterisation and cell culture studies were performed for treated TMF surfaces in simulated body fluid (SBF) and MG63 cells. All these observations showed that the NaOH treatment is the most appropriate method for TMF alloy which exhibited superior biocompatibility and enhanced corrosion protection performance due to their hydrophilic, smooth, compact porous surface morphology than that of other substrates.

Electrochemical and corrosion behaviour of ion and laser-beam modified metal surfaces

International Nuclear Information System (INIS)

Bonora, P.L.

1989-01-01

Ion implantation may improve the resistance of metals to wear and corrosion both: by the formation of stable or metastable chemical compounds localized in a thin external layer; or by the so-called 'radiation damage' which is mainly active in lowering the potential gradients between different grains and between grain and grain boundaries as an effect of subdivision into substructures, up to a quasi-amorphous inert surface. The changes in the corrosion fatigue behaviour of iron as well as in its catalytic properties as a consequence of ion implantation are considered. The electrochemical behaviour of laser irradiated and ion mixed metals in terms of changed corrosion rate, corrosion morphology, passivability or breakdown of passivity is also explained. 27 refs.; 12 figs.; 5 tabs

Effect of oxide ion concentration on the electrochemical oxidation of carbon in molten LiCl

International Nuclear Information System (INIS)

Yun, J. W.; Choi, I. K.; Park, Y. S.; Kim, W. H.

2001-01-01

The continuous measurement of lithium oxide concentration was required in DOR (Direct Oxide Reduction) process, which converts spent nuclear fuel to metal form, for the reactivity monitor and effective control of the process. The concentration of lithium oxide was measured by the electrochemical method, which was based on the phenomenon that carbon atoms of glassy carbon electrode electrochemically react with oxygen ions of lithium oxide in molten LiCl medium. From the results of electrode polarization experiments, the trend of oxidation rate of carbon atoms was classified into two different regions, which were proportional and non-proportional ones, dependent on the amount of lithium oxide. Below about 2.5 wt % Li 2 O, as the carbon atom ionization rate was fast enough for reacting with diffusing lithium oxide to the surface of carbon electrode. In this concentration range, the oxidation rate of carbon atoms was controlled by the diffusion of lithium oxide, and the concentration of lithium oxide could be measured by electrochemical method. But, above 2.5 wt % Li 2 O, the oxidation rate of carbon atoms was controlled by the applied electrochemical potential, because the carbon atom ionization rate was suppressed by the huge amounts of diffusing Li 2 O. Above this concentration, the electrochemical method was not applicable to determine the concentration of lithium oxide

Recent Advances in Porous Carbon Materials for Electrochemical Energy Storage.

Science.gov (United States)

Wang, Libin; Hu, Xianluo

2018-06-18

Climate change and the energy crisis have promoted the rapid development of electrochemical energy-storage devices. Owing to many intriguing physicochemical properties, such as excellent chemical stability, high electronic conductivity, and a large specific surface area, porous carbon materials have always been considering as a promising candidate for electrochemical energy storage. To date, a wide variety of porous carbon materials based upon molecular design, pore control, and compositional tailoring have been proposed for energy-storage applications. This focus review summarizes recent advances in the synthesis of various porous carbon materials from the view of energy storage, particularly in the past three years. Their applications in representative electrochemical energy-storage devices, such as lithium-ion batteries, supercapacitors, and lithium-ion hybrid capacitors, are discussed in this review, with a look forward to offer some inspiration and guidelines for the exploitation of advanced carbon-based energy-storage materials. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Electrochemical Study of Modified Glassy Carbon Electrode with Carboxyphenyl Diazonium Salt in Aqueous Solutions

Directory of Open Access Journals (Sweden)

Mariem BOUROUROU

2014-05-01

Full Text Available The covalent grafting of carboxyphenyl functionalities to planar carbon substrates by reaction with 2-carboxybenezenediazonium salt has been studied in aqueous acid solution. The surface was characterized, before and after the functionnalization process, by cyclic voltammetry, electrochemical impedance spectroscopy and linear sweep voltammetry (LSV in order to control and to prove the formation of a coating on the carbon surface. The results indicate the presence of substituted phenyl groups on the investigated surface. Electrochemical impedance measurements show that the slowing down of the electron transfer kinetics was more evident by increasing the number of cycles resulting to higher DEp and RCT parameters. Besides, the effect of the pH on the electron transfer processes of the Fe(CN63-/4- at the modified electrode is studied. By changing the solution pH the terminal group’s charge state would vary, based on which the surface pKa value is estimated.

The Influence of Electrolytic Concentration on the Electrochemical Deposition of Calcium Phosphate Coating on a Direct Laser Metal Forming Surface

Directory of Open Access Journals (Sweden)

Qianyue Sun

2017-01-01

Full Text Available A calcium phosphate (CaP coating on titanium surface enhances its biocompatibility, thus facilitating osteoconduction and osteoinduction with the inorganic phase of the human bone. Electrochemical deposition has been suggested as an effective means of fabricating CaP coatings on porous surface. The purpose of this study was to develop CaP coatings on a direct laser metal forming implant using electrochemical deposition and to investigate the effect of electrolytic concentration on the coating’s morphology and structure by X-ray diffraction, scanning electron microscopy, water contact angle analysis, and Fourier transform infrared spectroscopy. In group 10−2, coatings were rich in dicalcium phosphate, characterized to be thick, layered, and disordered plates. In contrast, in groups 10−3 and 10−4, the relatively thin and well-ordered coatings predominantly consisted of granular hydroxyapatite. Further, the hydrophilicity and cell affinity were improved as electrolytic concentration increased. In particular, the cells cultured in group 10−3 appeared to have spindle morphology with thick pseudopodia on CaP coatings; these spindles and pseudopodia strongly adhered to the rough and porous surface. By analyzing and evaluating the surface properties, we provided further knowledge on the electrolytic concentration effect, which will be critical for improving CaP coated Ti implants in the future.

Electrochemical carbon dioxide reduction on rough copper surfaces

NARCIS (Netherlands)

Kas, Recep

2016-01-01

Sustainable development and climate change is considered to be one of the top challenges of humanity. Electrochemical carbon dioxide (CO2) reduction to fuels or fuel precursor using renewable electricity is a very promising way to recycle CO2 and store the electricity. This would also provide

Electrochemical sensors and biosensors based on less aggregated graphene.

Science.gov (United States)

Bo, Xiangjie; Zhou, Ming; Guo, Liping

2017-03-15

As a novel single-atom-thick sheet of sp 2 hybridized carbon atoms, graphene (GR) has attracted extensive attention in recent years because of its unique and remarkable properties, such as excellent electrical conductivity, large theoretical specific surface area, and strong mechanical strength. However, due to the π-π interaction, GR sheets are inclined to stack together, which may seriously degrade the performance of GR with the unique single-atom layer. In recent years, an increasing number of GR-based electrochemical sensors and biosensors are reported, which may reflect that GR has been considered as a kind of hot and promising electrode material for electrochemical sensor and biosensor construction. However, the active sites on GR surface induced by the irreversible GR aggregations would be deeply secluded inside the stacked GR sheets and therefore are not available for the electrocatalysis. So the alleviation or the minimization of the aggregation level for GR sheets would facilitate the exposure of active sites on GR and effectively upgrade the performance of GR-based electrochemical sensors and biosensors. Less aggregated GR with low aggregation and high dispersed structure can be used in improving the electrochemical activity of GR-based electrochemical sensors or biosensors. In this review, we summarize recent advances and new progress for the development of electrochemical sensors based on less aggregated GR. To achieve such goal, many strategies (such as the intercalation of carbon materials, surface modification, and structural engineering) have been applied to alleviate the aggregation level of GR in order to enhance the performance of GR-based electrochemical sensors and biosensors. Finally, the challenges associated with less aggregated GR-based electrochemical sensors and biosensors as well as related future research directions are discussed. Copyright © 2016 Elsevier B.V. All rights reserved.

A new simulation model for electrochemical metal deposition

International Nuclear Information System (INIS)

Schmickler, W.; Poetting, K.; Mariscal, M.

2006-01-01

A new atomistic simulation model for electrochemical systems is presented. It combines microcanonical molecular dynamics for the electrode with stochastic dynamics for the solution, and allows the simulation of electrochemical deposition and dissolution for specific electrode potentials. As first applications the deposition of silver and platinum on Au(1 1 1) have been studied; both flat surfaces and surfaces with islands have been considered. The two systems behave quite differently: Ag on Au(1 1 1) grows layer by layer, while Pt forms a surface alloy on Au(1 1 1), which is followed by three-dimensional growth

Electrochemical capacity fading of polyaniline electrode in supercapacitor: An XPS analysis

Directory of Open Access Journals (Sweden)

Jinxing Deng

2017-04-01

Full Text Available To understand the electrochemical capacity fading of the polyaniline (PANI electrodes in supercapacitors, for the first time, their chemical structure change during electrochemical cycles was traced with XPS analysis after the HCl doped PANI electrodes were subjected to the cyclic voltammetry test in 1.0 M H2SO4 electrolyte for different cycle numbers. The results showed that the chlorine disappeared in the electrode surface, while the surface element contents of sulfur and oxygen increased with the electrochemical cycles increased. It demonstrated that the hydrolytic degradation of the PANI chains and exchange of dopant occurred during the electrochemical cycling, causing the fading in the mechanical and electrochemical performance of the PANI electrodes. This understanding should lead to better design of the conductive polymer-based energy storage devices.

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

Science.gov (United States)

2018-01-01

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

ELECTROCHEMICAL OXIDATION OF ETHANOL USING Ni-Co-PVC COMPOSITE ELECTRODE

Directory of Open Access Journals (Sweden)

Riyanto Riyanto

2011-07-01

Full Text Available The morphological characteristics and electrochemical behavior of nickel metal foil (Ni, nickel-polyvinyl chloride (Ni-PVC and nickel-cobalt-polyvinyl chloride (Ni-Co-PVC electrodes in alkaline solution has been investigated. The morphological characteristics of the electrode surface were studied using SEM and EDS, while the electrochemical behavior of the electrodes was studied using cyclic voltammetry (CV. It was found that composite electrodes (Ni-PVC and Ni-Co-PVC have a porous, irregular and rough surface. In situ studies using electrochemical technique using those three electrodes exhibited electrochemical activity for redox system, as well as selectivity in the electrooxidation of ethanol to acetic acid. The studies also found that an electrokinetics and electrocatalytic activity behaviors of the electrodes prepared were Ni metal foil

Resistive Switching Characteristics in Electrochemically Synthesized ZnO Films

Directory of Open Access Journals (Sweden)

Shuhan Jing

2015-04-01

Full Text Available The semiconductor industry has long been seeking a new kind of non-volatile memory technology with high-density, high-speed, and low-power consumption. This study demonstrated the electrochemical synthesis of ZnO films without adding any soft or hard templates. The effect of deposition temperatures on crystal structure, surface morphology and resistive switching characteristics were investigated. Our findings reveal that the crystallinity, surface morphology and resistive switching characteristics of ZnO thin films can be well tuned by controlling deposition temperature. A conducting filament based model is proposed to explain the switching mechanism in ZnO thin films.

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)

Preparation of porous lead from shape-controlled PbO bulk by in situ electrochemical reduction in ChCl-EG deep eutectic solvent

Science.gov (United States)

Ru, Juanjian; Hua, Yixin; Xu, Cunying; Li, Jian; Li, Yan; Wang, Ding; Zhou, Zhongren; Gong, Kai

2015-12-01

Porous lead with different shapes was firstly prepared from controlled geometries of solid PbO bulk by in situ electrochemical reduction in choline chloride-ethylene glycol deep eutectic solvents at cell voltage 2.5 V and 353 K. The electrochemical behavior of PbO powders on cavity microelectrode was investigated by cyclic voltammetry. It is indicated that solid PbO can be directly reduced to metal in the solvent and a nucleation loop is apparent. Constant voltage electrolysis demonstrates that PbO pellet can be completely converted to metal for 13 h, and the current efficiency and specific energy consumption are about 87.79% and 736.82 kWh t-1, respectively. With the electro-deoxidation progress on the pellet surface, the reduction rate reaches the fastest and decreases along the distance from surface to inner center. The morphologies of metallic products are porous and mainly consisted of uniform particles which connect with each other by finer strip-shaped grains to remain the geometry and macro size constant perfectly. In addition, an empirical model of the electro-deoxidation process from spherical PbO bulk to porous lead is also proposed. These findings provide a novel and simple route for the preparation of porous metals from oxide precursors in deep eutectic solvents at room temperature.

Insights into the Surface Transformation and Electrochemical Dissolution Process of Bornite in Bioleaching

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Hongbo Zhao

2018-04-01

Full Text Available In this work, density functional theory (DFT calculations, X-ray photoelectron spectroscopy (XPS and electrochemistry analysis were combined to analyze the electrochemical dissolution process of bornite during bioleaching. DFT calculations showed that bornite was a conductor with metallic conductivity. The formula of bornite may be (Cu+5Fe3+(S2−4 and the surface reconstruction of (111-S surface was discussed. Electrochemistry and XPS analysis showed that bornite tended to be directly oxidized with high conductivity when the potential was higher than 0.3 V vs. Ag/AgCl. Elemental sulfur (S0, FeOOH and CuS were the main intermediate species on the bornite surface during the oxidation process. The production of S0 and FeOOH on bornite surface can be significantly accelerated with increased redox potential, but no insoluble sulfate (SO42− formed on bornite surface in 0.3–0.65 V vs. Ag/AgCl. The oxidative dissolution of bornite was significantly accelerated with increasing redox potential, which was one important reason why mixed culture was more effective than single strains of A. caldus and L. ferriphilum in bornite bioleaching. The insoluble SO42− was formed mainly through the chemical reactions in solution and then covered the bornite surface in bioleaching. Based on the obtained results, a model for interpreting the dissolution process of bornite in bioleaching was proposed.

Development of remote electrochemical decontamination for hot cell applications

International Nuclear Information System (INIS)

Turner, A.D.; Pottinger, J.S.; Lain, M.J.; Dawson, R.K.; Neville, M.D.; Junkison, A.R.

1988-01-01

The paper concerns the development and evaluation of remote electrochemical decontamination systems for metal surfaces, in connection with the decommissioning of nuclear installations. Two types of technique based on the electrochemical dissolution of thin surface layers of the substrate were investigated: immersion of small items in tanks for electroetching and in situ electropolishing. A description is given of the work programme, the progress of work and the results obtained. (U.K.)

Quadrilateral Micro-Hole Array Machining on Invar Thin Film: Wet Etching and Electrochemical Fusion Machining

Directory of Open Access Journals (Sweden)

Woong-Kirl Choi

2018-01-01

Full Text Available Ultra-precision products which contain a micro-hole array have recently shown remarkable demand growth in many fields, especially in the semiconductor and display industries. Photoresist etching and electrochemical machining are widely known as precision methods for machining micro-holes with no residual stress and lower surface roughness on the fabricated products. The Invar shadow masks used for organic light-emitting diodes (OLEDs contain numerous micro-holes and are currently machined by a photoresist etching method. However, this method has several problems, such as uncontrollable hole machining accuracy, non-etched areas, and overcutting. To solve these problems, a machining method that combines photoresist etching and electrochemical machining can be applied. In this study, negative photoresist with a quadrilateral hole array pattern was dry coated onto 30-µm-thick Invar thin film, and then exposure and development were carried out. After that, photoresist single-side wet etching and a fusion method of wet etching-electrochemical machining were used to machine micro-holes on the Invar. The hole machining geometry, surface quality, and overcutting characteristics of the methods were studied. Wet etching and electrochemical fusion machining can improve the accuracy and surface quality. The overcutting phenomenon can also be controlled by the fusion machining. Experimental results show that the proposed method is promising for the fabrication of Invar film shadow masks.

3D, chemical and electrochemical characterization of blasted TI6Al4V surfaces: Its influence on the corrosion behaviour

International Nuclear Information System (INIS)

Barranco, V.; Escudero, M.L.; Garcia-Alonso, M.C.

2007-01-01

The blasting process to increase the roughness of the surface of metallic biomaterials is widely used. As a consequence, one can produce a renewed surface with different topography and chemical composition compared to the original one, which can alter the general corrosion behaviour of the samples. With this idea, the aim of this work is not only the topographical and compositional characterization of blasted surfaces of Ti6Al4V alloy but mainly its influence on the corrosion behaviour of these modified surfaces. The surfaces of Ti6Al4V alloys were blasted with SiO 2 /ZrO 2 and Al 2 O 3 particles of different size in order to obtain different roughnesses. To carry out the microstructural and topographical characterization of the blasted surfaces, the scanning electron microscopy (SEM) coupled with an energy dispersive X-ray (EDX), the contact profilometry method and the 3D characterization by means of stereo-Fe-SEM have been used. By means of stereo-Fe-SEM, the roughness and the real surface area of the rough surfaces have been calculated. The microstructural, topographical and compositional results have been correlated with the corrosion behaviour of the samples immersed in Hank's solution and studied by means of electrochemical impedance spectroscopy (EIS). The blasting process alters topographical and chemically the surface of the samples. These modifications induce to an increase in the capacitance values of the roughened samples due to the prevalence of the effect of electrochemically active areas of Ti6Al4V surface over the effect of the presence of Al 2 O 3 and ZrO 2 particles on the blasted surfaces. However, the general corrosion behaviour of the samples is not drastically changed

Electro-chemical deposition of nano hydroxyapatite-zinc coating on titanium metal substrate.

Science.gov (United States)

El-Wassefy, N A; Reicha, F M; Aref, N S

2017-08-13

Titanium is an inert metal that does not induce osteogenesis and has no antibacterial properties; it is proposed that hydroxyapatite coating can enhance its bioactivity, while zinc can contribute to antibacterial properties and improve osseointegration. A nano-sized hydroxyapatite-zinc coating was deposited on commercially pure titanium using an electro-chemical process, in order to increase its surface roughness and enhance adhesion properties. The hydroxyapatite-zinc coating was attained using an electro-chemical deposition in a solution composed of a naturally derived calcium carbonate, di-ammonium hydrogen phosphate, with a pure zinc metal as the anode and titanium as the cathode. The applied voltage was -2.5 for 2 h at a temperature of 85 °C. The resultant coating was characterized for its surface morphology and chemical composition using a scanning electron microscope (SEM), energy dispersive x-ray spectroscope (EDS), and Fourier transform infrared (FT-IR) spectrometer. The coated specimens were also evaluated for their surface roughness and adhesion quality. Hydroxyapatite-zinc coating had shown rosette-shaped, homogenous structure with nano-size distribution, as confirmed by SEM analysis. FT-IR and EDS proved that coatings are composed of hydroxyapatite (HA) and zinc. The surface roughness assessment revealed that the coating procedure had significantly increased average roughness (Ra) than the control, while the adhesive tape test demonstrated a high-quality adhesive coat with no laceration on tape removal. The developed in vitro electro-chemical method can be employed for the deposition of an even thickness of nano HA-Zn adhered coatings on titanium substrate and increases its surface roughness significantly.

Electrochemical cell structure including an ionomeric barrier

Science.gov (United States)

Lambert, Timothy N.; Hibbs, Michael

2017-06-20

An apparatus includes an electrochemical half-cell comprising: an electrolyte, an anode; and an ionomeric barrier positioned between the electrolyte and the anode. The anode may comprise a multi-electron vanadium phosphorous alloy, such as VP.sub.x, wherein x is 1-5. The electrochemical half-cell is configured to oxidize the vanadium and phosphorous alloy to release electrons. A method of mitigating corrosion in an electrochemical cell includes disposing an ionomeric barrier in a path of electrolyte or ion flow to an anode and mitigating anion accumulation on the surface of the anode.

Longitudinally Controlled Modification of Cylindrical and Conical Track-Etched Poly(ethylene terephthalate) Pores Using an Electrochemically Assisted Click Reaction

International Nuclear Information System (INIS)

Coceancigh, Herman; Tran-Ba, Khanh-Hoa; Columbia University, New York, NY; Siepser, Natasha; Baker, Lane A.; Ito, Takashi

2017-01-01

Here in this study, the longitudinally controlled modification of the inner surfaces of poly(ethylene terephthalate) (PET) track-etched pores was explored using an electrochemically assisted Cu(I)-catalyzed azide–alkyne cycloaddition (CuAAC) click reaction. Cylindrical or conical PET track-etched pores were first decorated with ethynyl groups via the amidation of surface -COOH groups, filled with a solution containing Cu(II) and azide-tagged fluorescent dye, and then sandwiched between comb-shaped and planar gold electrodes. Cu(I) was produced at the comb-shaped working electrode by the reduction of Cu(II); it diffused along the pores toward the other electrode and catalyzed CuAAC between an azide-tagged fluorescent dye and a pore-tethered ethynyl group. The modification efficiency of cylindrical pores (ca. 1 μm in diameter) was assessed from planar and cross-sectional fluorescence microscope images of modified membranes. Planar images showed that pore modification took place only above the teeth of the comb-shaped electrode with a higher reaction yield for longer Cu(II) reduction times. Cross-sectional images revealed micrometer-scale gradient modification along the pore axis, which reflected a Cu(I) concentration profile within the pores, as supported by finite-element computer simulations. The reported approach was applicable to the asymmetric modification of cylindrical pores with two different fluorescent dyes in the opposite directions and also for the selective visualization of the tip and base openings of conical pores (ca. 3.5 μm in base diameter and ca. 1 μm in tip diameter). Lastly, the method based on electrochemically assisted CuAAC provides a controlled means to fabricate asymmetrically modified nanoporous membranes and, in the future, will be applicable for chemical separations and the development of sequential catalytic reactors.

Functionalized Solid Electrodes for Electrochemical Biosensing of Purine Nucleobases and Their Analogues: A Review

Science.gov (United States)

Sharma, Vimal Kumar; Jelen, Frantisek; Trnkova, Libuse

2015-01-01

Interest in electrochemical analysis of purine nucleobases and few other important purine derivatives has been growing rapidly. Over the period of the past decade, the design of electrochemical biosensors has been focused on achieving high sensitivity and efficiency. The range of existing electrochemical methods with carbon electrode displays the highest rate in the development of biosensors. Moreover, modification of electrode surfaces based on nanomaterials is frequently used due to their extraordinary conductivity and surface to volume ratio. Different strategies for modifying electrode surfaces facilitate electron transport between the electrode surface and biomolecules, including DNA, oligonucleotides and their components. This review aims to summarize recent developments in the electrochemical analysis of purine derivatives, as well as discuss different applications. PMID:25594595

Functionalized Solid Electrodes for Electrochemical Biosensing of Purine Nucleobases and Their Analogues: A Review

Directory of Open Access Journals (Sweden)

Vimal Kumar Sharma

2015-01-01

Full Text Available Interest in electrochemical analysis of purine nucleobases and few other important purine derivatives has been growing rapidly. Over the period of the past decade, the design of electrochemical biosensors has been focused on achieving high sensitivity and efficiency. The range of existing electrochemical methods with carbon electrode displays the highest rate in the development of biosensors. Moreover, modification of electrode surfaces based on nanomaterials is frequently used due to their extraordinary conductivity and surface to volume ratio. Different strategies for modifying electrode surfaces facilitate electron transport between the electrode surface and biomolecules, including DNA, oligonucleotides and their components. This review aims to summarize recent developments in the electrochemical analysis of purine derivatives, as well as discuss different applications.

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.

Photo-induced electrochemical anodization of p-type silicon: achievement and demonstration of long term surface stability

International Nuclear Information System (INIS)

Dhanekar, Saakshi; Islam, S S; Harsh

2012-01-01

Surface stability is achieved and demonstrated by porous silicon (PS) fabricated using a wavelength-dependent photo-electrochemical (PEC) anodization technique. During anodization, the photon flux for all wavelengths was kept constant while only the effect of light wavelength on the surface morphology of PS was investigated. PS optical sensors were realized, characterized and tested using a photoluminescence (PL) quenching technique. An aliphatic chain of alcohols (methanol to n-octanol) was detected in the range of 10–200 ppm. Long term surface stability was observed from samples prepared under red (750–620 nm) and green illumination (570–495 nm), where the PL quenching cycles evoke the possibility of using PS for stable sensor device applications. This study provides a route for preparing highly sensitive organic vapour sensors with a precise selection of the fabrication parameters and demonstrating their prolonged performance. (paper)

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

Effect of the electrochemical passivation on the corrosion behaviour of austenitic stainless steel

International Nuclear Information System (INIS)

Barbucci, A.; Delucchi, M.; Panizza, M.; Farne, G.; Cerisola, G.

2004-01-01

Cold rolled SS is also fruitfully used in deep drawing however the presence of scales or oxides on the surface reduces the life of the tools and emphasises creep phenomena of the material. Then a cleaning of the SS surface from these impurities is necessary. Oxides can be formed during the hot rolling preceding the cold one, or during the annealing performed between the several steps of thickness reduction. The annealing helps to decrease the work hardening occurring during the process. Normally this heat treatment is performed in reducing atmosphere of pure hydrogen (bright annealing), but even in this conditions oxides are formed on the SS surface. To avoid this uncontrolled oxide growth one method recently applied is an electrochemical cleaning performed in an electrolytic solution containing chrome, generally called electrochemical passivation. The electrochemical passivation allows the dissolution of the contaminating hard particles on the strips. Few scientific contributions are available in literature, which explain in detail the process mechanism. The aim of this work is to investigate if the electrochemical passivated surface acts in a different way with regard to corrosion phenomena with respect to conventional SS. Electrochemical measurements like polarisation, chrono-amperometries and surface analysis were used to investigate the corrosion behaviour of electrochemically passivated AISI 304L and AISI 305. The effect of some process parameters were considered, too. (authors)

Effect of the electrochemical passivation on the corrosion behaviour of austenitic stainless steel

Energy Technology Data Exchange (ETDEWEB)

Barbucci, A.; Delucchi, M.; Panizza, M.; Farne, G.; Cerisola, G. [DICheP, University of Genova, P.le Kennedy 1, 16129 Genova (Italy)

2004-07-01

Cold rolled SS is also fruitfully used in deep drawing however the presence of scales or oxides on the surface reduces the life of the tools and emphasises creep phenomena of the material. Then a cleaning of the SS surface from these impurities is necessary. Oxides can be formed during the hot rolling preceding the cold one, or during the annealing performed between the several steps of thickness reduction. The annealing helps to decrease the work hardening occurring during the process. Normally this heat treatment is performed in reducing atmosphere of pure hydrogen (bright annealing), but even in this conditions oxides are formed on the SS surface. To avoid this uncontrolled oxide growth one method recently applied is an electrochemical cleaning performed in an electrolytic solution containing chrome, generally called electrochemical passivation. The electrochemical passivation allows the dissolution of the contaminating hard particles on the strips. Few scientific contributions are available in literature, which explain in detail the process mechanism. The aim of this work is to investigate if the electrochemical passivated surface acts in a different way with regard to corrosion phenomena with respect to conventional SS. Electrochemical measurements like polarisation, chrono-amperometries and surface analysis were used to investigate the corrosion behaviour of electrochemically passivated AISI 304L and AISI 305. The effect of some process parameters were considered, too. (authors)

Gold nanoparticle-based electrochemical biosensors

International Nuclear Information System (INIS)

Pingarron, Jose M.; Yanez-Sedeno, Paloma; Gonzalez-Cortes, Araceli

2008-01-01

The unique properties of gold nanoparticles to provide a suitable microenvironment for biomolecules immobilization retaining their biological activity, and to facilitate electron transfer between the immobilized proteins and electrode surfaces, have led to an intensive use of this nanomaterial for the construction of electrochemical biosensors with enhanced analytical performance with respect to other biosensor designs. Recent advances in this field are reviewed in this article. The advantageous operational characteristics of the biosensing devices designed making use of gold nanoparticles are highlighted with respect to non-nanostructured biosensors and some illustrative examples are commented. Electrochemical enzyme biosensors including those using hybrid materials with carbon nanotubes and polymers, sol-gel matrices, and layer-by-layer architectures are considered. Moreover, electrochemical immunosensors in which gold nanoparticles play a crucial role in the electrode transduction enhancement of the affinity reaction as well as in the efficiency of immunoreagents immobilization in a stable mode are reviewed. Similarly, recent advances in the development of DNA biosensors using gold nanoparticles to improve DNA immobilization on electrode surfaces and as suitable labels to improve detection of hybridization events are considered. Finally, other biosensors designed with gold nanoparticles oriented to electrically contact redox enzymes to electrodes by a reconstitution process and to the study of direct electron transfer between redox proteins and electrode surfaces have also been treated

Gold nanoparticle-based electrochemical biosensors

Energy Technology Data Exchange (ETDEWEB)

Pingarron, Jose M.; Yanez-Sedeno, Paloma; Gonzalez-Cortes, Araceli [Department of Analytical Chemistry, Faculty of Chemistry, University Complutense of Madrid, 28040 Madrid (Spain)

2008-08-01

The unique properties of gold nanoparticles to provide a suitable microenvironment for biomolecules immobilization retaining their biological activity, and to facilitate electron transfer between the immobilized proteins and electrode surfaces, have led to an intensive use of this nanomaterial for the construction of electrochemical biosensors with enhanced analytical performance with respect to other biosensor designs. Recent advances in this field are reviewed in this article. The advantageous operational characteristics of the biosensing devices designed making use of gold nanoparticles are highlighted with respect to non-nanostructured biosensors and some illustrative examples are commented. Electrochemical enzyme biosensors including those using hybrid materials with carbon nanotubes and polymers, sol-gel matrices, and layer-by-layer architectures are considered. Moreover, electrochemical immunosensors in which gold nanoparticles play a crucial role in the electrode transduction enhancement of the affinity reaction as well as in the efficiency of immunoreagents immobilization in a stable mode are reviewed. Similarly, recent advances in the development of DNA biosensors using gold nanoparticles to improve DNA immobilization on electrode surfaces and as suitable labels to improve detection of hybridization events are considered. Finally, other biosensors designed with gold nanoparticles oriented to electrically contact redox enzymes to electrodes by a reconstitution process and to the study of direct electron transfer between redox proteins and electrode surfaces have also been treated. (author)

On-line electrochemical monitoring of microbially influenced corrosion

International Nuclear Information System (INIS)

Dowling, N.J.E.; Stansbury, E.E.; White, D.C.; Borenstein, S.W.; Danko, J.C.

1989-01-01

Newly emerging electrochemical measurement techniques can provide on-line, non-destructive monitoring of the average corrosion rate and indications of localized pitting corrosion together with insight into fundamental electrochemical mechanisms responsible for the corrosion process. This information is relevant to evaluating, monitoring, understanding and controlling microbially influenced corrosion (MIC). MIC of coupons exposed in sidestream devices on site or in laboratory-based experiments, where the corrosion response is accelerated by exposure to active consortia of microbes recovered from specific sites, can be utilized to evaluate mitigation strategies. The average corrosion rates can be determined by small amplitude cyclic voltametry (SACV), and AC impedance spectroscopy (EIS). EIS can also give insight into the mechanisms of the MIC and indications of localized corrosion. Pitting corrosion can be detected non-destructively with open circuit potential monitoring (OCP). OCP also responds to bacterial biofilm activities such as oxygen depletion and other electrochemical activities. Utilizing these methods, accelerated tests can be designed to direct the selection of materials, surface treatments of materials, and welding filler materials, as well as the optimization of chemical and mechanical countermeasures with the microbial consortia recovered and characterized from the specific sites of interest

Neural Cell Chip Based Electrochemical Detection of Nanotoxicity.

Science.gov (United States)

Kafi, Md Abdul; Cho, Hyeon-Yeol; Choi, Jeong Woo

2015-07-02

Development of a rapid, sensitive and cost-effective method for toxicity assessment of commonly used nanoparticles is urgently needed for the sustainable development of nanotechnology. A neural cell with high sensitivity and conductivity has become a potential candidate for a cell chip to investigate toxicity of environmental influences. A neural cell immobilized on a conductive surface has become a potential tool for the assessment of nanotoxicity based on electrochemical methods. The effective electrochemical monitoring largely depends on the adequate attachment of a neural cell on the chip surfaces. Recently, establishment of integrin receptor specific ligand molecules arginine-glycine-aspartic acid (RGD) or its several modifications RGD-Multi Armed Peptide terminated with cysteine (RGD-MAP-C), C(RGD)₄ ensure farm attachment of neural cell on the electrode surfaces either in their two dimensional (dot) or three dimensional (rod or pillar) like nano-scale arrangement. A three dimensional RGD modified electrode surface has been proven to be more suitable for cell adhesion, proliferation, differentiation as well as electrochemical measurement. This review discusses fabrication as well as electrochemical measurements of neural cell chip with particular emphasis on their use for nanotoxicity assessments sequentially since inception to date. Successful monitoring of quantum dot (QD), graphene oxide (GO) and cosmetic compound toxicity using the newly developed neural cell chip were discussed here as a case study. This review recommended that a neural cell chip established on a nanostructured ligand modified conductive surface can be a potential tool for the toxicity assessments of newly developed nanomaterials prior to their use on biology or biomedical technologies.

Neural Cell Chip Based Electrochemical Detection of Nanotoxicity

Directory of Open Access Journals (Sweden)

Md. Abdul Kafi

2015-07-01

Full Text Available Development of a rapid, sensitive and cost-effective method for toxicity assessment of commonly used nanoparticles is urgently needed for the sustainable development of nanotechnology. A neural cell with high sensitivity and conductivity has become a potential candidate for a cell chip to investigate toxicity of environmental influences. A neural cell immobilized on a conductive surface has become a potential tool for the assessment of nanotoxicity based on electrochemical methods. The effective electrochemical monitoring largely depends on the adequate attachment of a neural cell on the chip surfaces. Recently, establishment of integrin receptor specific ligand molecules arginine-glycine-aspartic acid (RGD or its several modifications RGD-Multi Armed Peptide terminated with cysteine (RGD-MAP-C, C(RGD4 ensure farm attachment of neural cell on the electrode surfaces either in their two dimensional (dot or three dimensional (rod or pillar like nano-scale arrangement. A three dimensional RGD modified electrode surface has been proven to be more suitable for cell adhesion, proliferation, differentiation as well as electrochemical measurement. This review discusses fabrication as well as electrochemical measurements of neural cell chip with particular emphasis on their use for nanotoxicity assessments sequentially since inception to date. Successful monitoring of quantum dot (QD, graphene oxide (GO and cosmetic compound toxicity using the newly developed neural cell chip were discussed here as a case study. This review recommended that a neural cell chip established on a nanostructured ligand modified conductive surface can be a potential tool for the toxicity assessments of newly developed nanomaterials prior to their use on biology or biomedical technologies.

Effect of surface modification by nitrogen ion implantation on the electrochemical and cellular behaviors of super-elastic NiTi shape memory alloy.

Science.gov (United States)

Maleki-Ghaleh, H; Khalil-Allafi, J; Sadeghpour-Motlagh, M; Shakeri, M S; Masoudfar, S; Farrokhi, A; Beygi Khosrowshahi, Y; Nadernezhad, A; Siadati, M H; Javidi, M; Shakiba, M; Aghaie, E

2014-12-01

The aim of this investigation was to enhance the biological behavior of NiTi shape memory alloy while preserving its super-elastic behavior in order to facilitate its compatibility for application in human body. The surfaces of NiTi samples were bombarded by three different nitrogen doses. Small-angle X-ray diffraction was employed for evaluating the generated phases on the bombarded surfaces. The electrochemical behaviors of the bare and surface-modified NiTi samples were studied in simulated body fluid (SBF) using electrochemical impedance and potentio-dynamic polarization tests. Ni ion release during a 2-month period of service in the SBF environment was evaluated using atomic absorption spectrometry. The cellular behavior of nitrogen-modified samples was studied using fibroblast cells. Furthermore, the effect of surface modification on super-elasticity was investigated by tensile test. The results showed the improvement of both corrosion and biological behaviors of the modified NiTi samples. However, no significant change in the super-elasticity was observed. Samples modified at 1.4E18 ion cm(-2) showed the highest corrosion resistance and the lowest Ni ion release.

Electrochemical Sensors Based on Carbon Nanotubes

Directory of Open Access Journals (Sweden)

Md. Aminur Rahman

2009-03-01

Full Text Available This review focuses on recent contributions in the development of the electrochemical sensors based on carbon nanotubes (CNTs. CNTs have unique mechanical and electronic properties, combined with chemical stability, and behave electrically as a metal or semiconductor, depending on their structure. For sensing applications, CNTs have many advantages such as small size with larger surface area, excellent electron transfer promoting ability when used as electrodes modifier in electrochemical reactions, and easy protein immobilization with retention of its activity for potential biosensors. CNTs play an important role in the performance of electrochemical biosensors, immunosensors, and DNA biosensors. Various methods have been developed for the design of sensors using CNTs in recent years. Herein we summarize the applications of CNTs in the construction of electrochemical sensors and biosensors along with other nanomaterials and conducting polymers.

Gold Nanoparticles with Externally Controlled, Reversible Shifts of Local Surface Plasmon Resonance Bands

Science.gov (United States)

Yavuz, Mustafa S.; Jensen, Gary C.; Penaloza, David P.; Seery, Thomas A. P.; Pendergraph, Samuel A.; Rusling, James F.; Sotzing, Gregory A.

2010-01-01

We have achieved reversible tunability of local surface plasmon resonance in conjugated polymer functionalized gold nanoparticles. This property was facilitated by the preparation of 3,4-ethylenedioxythiophene (EDOT) containing polynorbornene brushes on gold nanoparticles via surface-initiated ring-opening metathesis polymerization. Reversible tuning of the surface plasmon band was achieved by electrochemically switching the EDOT polymer between its reduced and oxidized states. PMID:19839619

Effect of morphology and defect density on electron transfer of electrochemically reduced graphene oxide

Energy Technology Data Exchange (ETDEWEB)

Zhang, Yan, E-mail: yanzhang@sues.edu.cn [School of Material Engineering, Shanghai University of Engineering Science, Shanghai 201620 (China); Hao, Huilian, E-mail: huilian.hao@sues.edu.cn [School of Material Engineering, Shanghai University of Engineering Science, Shanghai 201620 (China); Wang, Linlin, E-mail: wlinlin@mail.ustc.edu.cn [College of Chemistry and Chemical Engineering, Shanghai University of Engineering Science, Shanghai 201620 (China)

2016-12-30

Highlights: • Different morphologies of ERGO on the surface of GCE were prepared via different methods. • The defect densities of ERGO were controlled by tuning the mass or concentration of GO. • A higher defect density of ERGO accelerates electron transfer rate. • ERGO with more exposed edge planes shows significantly higher electron transfer kinetics. • Both edge planes and defect density contribute to electron transfer of ERGO. - Abstract: Electrochemically reduced graphene oxide (ERGO) is widely used to construct electrochemical sensors. Understanding the electron transfer behavior of ERGO is essential for its electrode material applications. In this paper, different morphologies of ERGO were prepared via two different methods. Compared to ERGO/GCEs prepared by electrochemical reduction of pre-deposited GO, more exposed edge planes of ERGO are observed on the surface of ERGO-GCE that was constructed by electrophoretic deposition of GO. The defect densities of ERGO were controlled by tuning the mass or concentration of GO. The electron transfer kinetics (k{sup 0}) of GCE with different ERGOs was comparatively investigated. Owing to increased surface areas and decreased defect density, the k{sup 0} values of ERGO/GCE initially increase and then decrease with incrementing of GO mass. When the morphology and surface real areas of ERGO-GCE are the same, an increased defect density induces an accelerated electron transfer rate. k{sup 0} valuesof ERGO-GCEs are about 1 order of magnitude higher than those of ERGO/GCEs due to the difference in the amount of edge planes. This work demonstrates that both defect densities and edge planes of ERGO play crucial roles in electron transfer kinetics.

Effect of morphology and defect density on electron transfer of electrochemically reduced graphene oxide

International Nuclear Information System (INIS)

Zhang, Yan; Hao, Huilian; Wang, Linlin

2016-01-01

Highlights: • Different morphologies of ERGO on the surface of GCE were prepared via different methods. • The defect densities of ERGO were controlled by tuning the mass or concentration of GO. • A higher defect density of ERGO accelerates electron transfer rate. • ERGO with more exposed edge planes shows significantly higher electron transfer kinetics. • Both edge planes and defect density contribute to electron transfer of ERGO. - Abstract: Electrochemically reduced graphene oxide (ERGO) is widely used to construct electrochemical sensors. Understanding the electron transfer behavior of ERGO is essential for its electrode material applications. In this paper, different morphologies of ERGO were prepared via two different methods. Compared to ERGO/GCEs prepared by electrochemical reduction of pre-deposited GO, more exposed edge planes of ERGO are observed on the surface of ERGO-GCE that was constructed by electrophoretic deposition of GO. The defect densities of ERGO were controlled by tuning the mass or concentration of GO. The electron transfer kinetics (k"0) of GCE with different ERGOs was comparatively investigated. Owing to increased surface areas and decreased defect density, the k"0 values of ERGO/GCE initially increase and then decrease with incrementing of GO mass. When the morphology and surface real areas of ERGO-GCE are the same, an increased defect density induces an accelerated electron transfer rate. k"0 valuesof ERGO-GCEs are about 1 order of magnitude higher than those of ERGO/GCEs due to the difference in the amount of edge planes. This work demonstrates that both defect densities and edge planes of ERGO play crucial roles in electron transfer kinetics.

Hybrid electronic tongue based on optical and electrochemical microsensors for quality control of wine.

Science.gov (United States)

Gutiérrez, Manuel; Llobera, Andreu; Vila-Planas, Jordi; Capdevila, Fina; Demming, Stefanie; Büttgenbach, Stephanus; Mínguez, Santiago; Jiménez-Jorquera, Cecilia

2010-07-01

A multiparametric system able to classify red and white wines according to the grape varieties and for analysing some specific parameters is presented. The system, known as hybrid electronic tongue, consists of an array of electrochemical microsensors and a colorimetric optofluidic system. The array of electrochemical sensors is composed of six ISFETs based sensors, a conductivity sensor, a redox potential sensor and two amperometric electrodes, an Au microelectrode and a microelectrode for sensing electrochemical oxygen demand. The optofluidic system is entirely fabricated in polymer technology and comprises a hollow structure, air mirrors, microlenses and self-alignment structures. The data obtained from these sensors has been treated with multivariate advanced tools; Principal Component Analysis (PCA), for the patterning recognition and classification of wine samples, and Partial-Least Squares (PLS) regression, for quantification of several chemical and optical parameters of interest in wine quality. The results have demonstrated the utility of this system for distinguishing the samples according to the grape variety and year vintage and for quantifying several sample parameters of interest in wine quality control.

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.

Effect of covalently bonded polysiloxane multilayers on the electrochemical behavior of graphite electrode in lithium ion batteries

Energy Technology Data Exchange (ETDEWEB)

Pan, Qinmin; Jiang, Yinghua [Department of Applied Chemistry, Harbin Institute of Technology, Harbin 150001 (China)

2008-03-15

Polysiloxane multilayers were covalently bonded to the surface of natural graphite particles via diazonium chemistry and silylation reaction. The as-prepared graphite exhibited excellent discharge-charge behavior as negative electrode materials in lithium ion batteries. The improvement in the electrochemical performance of the graphite electrodes was attributed to the formation of a stable and flexible passive film on their surfaces. It was also revealed that the chemical compositions of the multilayers exerted influence on the electrochemical behavior of the graphite electrodes. The result of this study presents a new strategy to the formation of elastic and strong passive film on the graphite electrode via molecular design. Owing to the diversity of polysilxoane multilayers, this method also enables researchers to control the surface chemistries of carbonaceous materials with flexibility. (author)

Electrochemical studies of Pu on prussian blue (PB)-gold nanoparticles (AuNPs) functionalized glassy carbon (GC) electrode

International Nuclear Information System (INIS)

Sharma, Manoj K.; Ambolikar, Arvind S.; Aggarwal, Suresh K.

2011-01-01

In electrochemical processes, electron transfer across the solid-liquid interface is the elementary step and electron transfer kinetics is significantly influenced by the interfacial properties. Therefore, preparation of well-defined electrochemical interface with highly controllable properties - larger effective surface area, increased mass transport, and better electronic interaction between the analyte and electrode - is significant for both fundamental and applied studies in electrochemistry. In the present work electrochemistry of Pu(IV)/Pu(III) is studied on multilayered AuNPs-PB-AuNPs functionalized electrode

An Overview of Pesticide Monitoring at Environmental Samples Using Carbon Nanotubes-Based Electrochemical Sensors

Directory of Open Access Journals (Sweden)

Ademar Wong

2017-03-01

Full Text Available Carbon nanotubes have received enormous attention in the development of electrochemical sensors by promoting electron transfer reactions, decreasing the work overpotential within great surface areas. The growing concerns about environmental health emphasized the necessity of continuous monitoring of pollutants. Pesticides have been successfully used to control agricultural and public health pests; however, intense use can cause a number of damages for biodiversity and human health. In this sense, carbon nanotubes-based electrochemical sensors have been proposed for pesticide monitoring combining different electrode modification strategies and electroanalytical techniques. In this paper, we provide a review of the recent advances in the use of carbon nanotubes for the construction of electrochemical sensors dedicated to the environmental monitoring of pesticides. Future directions, perspectives, and challenges are also commented.

Method for controlling power flow between an electrochemical cell and a power grid

International Nuclear Information System (INIS)

Coleman, A. K.

1981-01-01

A method is disclosed for controlling a force-commutated inverter coupled between an electrochemical cell and a power grid for adjusting the magnitude and direction of the electrical energy flowing therebetween. Both the real power component and the reactive power component of ac electrical energy flow can be independently VARied through the switching waveform presented to the intermediately coupled inverter. A VAR error signal is derived from a comparison of a var command signal with a signal proportional to the actual reactive power circulating between the inverter and the power grid. This signal is presented to a voltage controller which essentially varies only the effective magnitude of the fundamental voltage waveform out of the inverter , thereby leaving the real power component substantially unaffected. In a similar manner, a power error signal is derived by a comparison of a power command signal with a signal proportional to the actual real power flowing between the electrochemical cell and the power grid. This signal is presented to a phase controller which varies only the phase of the fundamental component of the voltage waveform out of the inverter relative to that of the power grid and changes only the real power in proportion thereto, thus leaving the reactive power component substantially unaffected

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)

Fabrication of a miniaturized cell using microsystem technologies for electrochemical applications

International Nuclear Information System (INIS)

Lakard, Boris; Jeannot, Jean-Claude; Spajer, Michel; Herlem, Guillaume; Labachelerie, Michel de; Blind, Pascal; Fahys, Bernard

2005-01-01

A new type of electrochemical cell has been developed for use in electrochemical, chemical and biological applications. Using a platinum microelectrode as working electrode, this cell incorporates a silver microelectrode as reference electrode. These microelectrodes, whose area is equal to 1 μm 2 , were fabricated using photolithography, sputtering, and focused ion beam (FIB) technologies since these micro-fabrication techniques allow us to develop miniaturized electrochemical cells useful either for nanoelectrochemistry or biosensors applications. In this study, we show it is possible to coat a surface by chemical or biological compounds by immersing the microelectrodes in a solution, then setting a difference of potential between the two microelectrodes of the cell. For example, we used this miniaturized cell to realize the electrochemical polymerization of aniline into polyaniline to show that this electrochemical cell is efficient to coat a surface with a thin film of polymer

Surface analytical and electrochemical characterization of oxide films formed on Incoloy-800 and carbon steel in simulated secondary water chemistry conditions of PHWRs

International Nuclear Information System (INIS)

Rangarajan, S.; Sinu, C.; Balaji, V.; Narasimhan, S.V.

2010-01-01

The water chemistry in the Steam Generator (SG) Circuits of Indian Pressurized Heavy Water Reactors (PHWRs) is controlled by the all volatile treatment (AVT) procedure, wherein volatile amines are used to maintain the alkaline pH required for minimizing the corrosion of the structural materials. Earlier, Monel and morpholine were used as the Steam Generator material and the alkalizing agent respectively. However, currently they are replaced by Incoloy-800 and Ethanolamine (ETA). ETA was chosen because of its beneficial effects due to low pK b and K d values, loading behaviour on condensate polishing unit (CPU) and also on cost comparison with other amines. Since we have Incoloy-800 on the tube side and Carbon steel(CS) on the shell side in the SG circuits, efforts were taken to study the nature of the oxide films formed on these surfaces and to evaluate the corrosion resistance and electrochemical properties of the same, under simulated secondary water chemistry conditions of PHWRs containing different dissolved oxygen (DO) concentration. In this context, experiments were carried out by exposing finely polished CS and Incoloy -800 coupons to ETA based medium in the presence and absence of Hydrazine (pH: 9.2) at 240 o C under two different DO conditions (< 10 ppb and 200 ppb) for 24 hours. Oxide films formed under these conditions were characterized using SEM, Raman spectroscopy, electrochemical impedance, polarization and Mott-Schottky techniques. Further, studies at a controlled DO level ( < 10 ppb) were carried out for different time durations viz., 7- and 30- days. The composition, surface morphology, oxide thickness, resistance, type of semi-conductivity and defect density of the oxide films were evaluated and correlated with the DO levels and discussed elaborately in this paper. (author)

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

Service water electrochemical monitoring development at Ontario Hydro

International Nuclear Information System (INIS)

Brennenstuhl, A.M.

1994-01-01

Ontario Hydro (OH) is currently investigating the feasibility of using electrochemical techniques for the corrosion monitoring of service water systems. To date all evaluations have been carried out in a field simulator. The studies include examining the effects of; system startup after periods of stagnation, sodium hypochlorite injection, and zebra mussel settlement on metallic surfaces. Carbon steel and Type 304L stainless steel have been evaluated. Electrochemical potential noise (EPN), electrochemical current noise (ECN) potential and coupling current were semi-continuously monitored over a period of up to one year. Data obtained from the electrochemical noise monitoring has given OH valuable insights into the mechanisms of degradation in service water systems. The high sensitivity of the electrochemical noise technique, particularly to localized corrosion has proved to be the major attraction of the system

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.

Ordered mesoporous carbon for electrochemical sensing: A review

Energy Technology Data Exchange (ETDEWEB)

Ndamanisha, Jean Chrysostome [Faculty of Chemistry, Northeast Normal University, Changchun 130024 (China); Universite du Burundi, Institut de pedagogie appliquee, B.P. 5223, Bujumbura (Burundi); Guo Liping, E-mail: guolp078@nenu.edu.cn [Faculty of Chemistry, Northeast Normal University, Changchun 130024 (China)

2012-10-17

Highlights: Black-Right-Pointing-Pointer The preparation and functionalization of ordered mesoporous carbon. Black-Right-Pointing-Pointer Their applications as electrochemical sensors with high electrocatalytic activity. Black-Right-Pointing-Pointer A promising electrode material based on its interesting properties. - Abstract: With its well-ordered pore structure, high specific surface area and tunable pore diameters in the mesopore range, ordered mesoporous carbon (OMC) is suitable for applications in catalysis and sensing. We report recent applications of OMC in electrochemical sensors and biosensors. After a brief description of the electrochemical properties, the functionalization of the OMC for improvement of the electrocatalytic properties is then presented. We show how the ordered mesostructure of OMC is very important in those applications. The high density of edge plane-like defective sites (EDSs), oxygen-containing groups and a large surface area on OMC may provide many favorable sites for electron transfer to compounds, which makes OMC a potential novel material for an investigation of the electrochemical behavior of substances. Moreover, the structural capabilities of OMC at the scale of a few nanometers agree with immobilization of other electrocataytic substances. Interesting properties of this material may open up a new approach to study the electrochemical determination of other biomolecules.

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

Electrochemical performance of 3D porous Ni-Co oxide with electrochemically exfoliated graphene for asymmetric supercapacitor applications

International Nuclear Information System (INIS)

Kim, Dae Kyom; Hwang, Minsik; Ko, Dongjin; Kang, Jeongmin; Seong, Kwang-dong; Piao, Yuanzhe

2017-01-01

Graphical abstract: The paper reported the Ni-Co oxide/electrochemically exfoliated graphene nanocomposites with 3D porous nano-architectures (NC-EEG) using a simple low temperature solution method combined with a thermal annealing treatment. 3D porous architectures provide large surface areas and shorten electron diffusion pathways for high performance asymmetric supercapacitors. Display Omitted -- Highlights: •A simple low temperature solution method was used for preparing NC-EEG. •Graphene sheets were obtained by electrochemically exfoliation process. •A high capacity of NC-EEG in a three-electrode system, as high as 649 C g −1 , was recorded. •Asymmetric supercapacitor based on NC-EEG exhibited excellent energy density and power density. -- Abstract: Ni-Co oxide, one of the binary metal oxides, has many advantages for use in high-performance supercapacitor electrode materials due to its relatively high electronic conductivity and improved electrochemical performance. In this work, Ni-Co oxide/electrochemically exfoliated graphene nanocomposites (NC-EEG) are successfully synthesized using a simple low temperature solution method combined with a thermal annealing treatment. Graphene sheets are directly obtained by an electrochemical exfoliation process with graphite foil, which is very simple, environmentally friendly, and has a relatively short reaction time. This electrochemically exfoliated graphene (EEG) can improve the electrical conductivity of the Ni-Co oxide nanostructures. The as-prepared NC-EEG nanocomposites have 3D porous architectures that can provide large surface areas and shorten electron diffusion pathways. Electrochemical properties were performed by cyclic voltammetry and galvanostatic charge/discharge in a 6 M KOH electrolyte. The NC-EEG nanocomposites exhibited a high capacity value of 649 C g −1 at a current density of 1.0 A g −1 . The asymmetric supercapacitors, manufactured on the basis of NC-EEG nanocomposites as a positive

Electrochemical properties of porous carbon black layer as an electron injector into iodide redox couple

International Nuclear Information System (INIS)

Kim, Jung-Min; Rhee, Shi-Woo

2012-01-01

Highlights: ► Carbon black (CB) porous layer for triiodide (I 3 − ) ion reduction is coated with spray coating method at 120 °C on the fluorine-doped tin oxide glass. ► The electrochemical impedance spectroscopy is analyzed for a symmetric cell and a new circuit model is applied to identify electrochemical parameters. ► Decreased particle size and increased thickness improve the catalytic activity because of the increase in the surface area and the conductivity of the CB layer. - Abstract: Electrochemical properties of carbon black (CB) porous layer as a counter electrode in dye-sensitized solar cells (DSC) are studied. CB electrode for triiodide (I 3 − ) ion reduction is coated with spray coating method on the fluorine-doped tin oxide glass at 120 °C. The CB particle size is varied from 20 nm to 90 nm and the CB electrode thickness is controlled from 1 μm to 9 μm by controlling the spraying time. The electrochemical impedance spectroscopy is analyzed for a symmetric cell and a new circuit model is applied to identify electrochemical parameters. As the CB particle size is decreased, the catalytic activity is improved because of the increase in the surface area and the conductivity of the CB layer. Increased CB electrode thickness also improves the catalytic activity and leads to the low charge transfer resistance at the electrolyte/CB electrode interface. The CB counter electrode with the particle size of 20 nm and the thickness of 9 μm for DSC shows the energy conversion efficiency of 7.2% with the highest fill factor (FF) of 65.6%, which is similar to the Pt counter electrode with FF of 65.8% and the efficiency of 7.6%.

Controlling the Sn-C bonds content in SnO2@CNTs composite to form in situ pulverized structure for enhanced electrochemical kinetics.

Science.gov (United States)

Cheng, Yayi; Huang, Jianfeng; Qi, Hui; Cao, Liyun; Luo, Xiaomin; Li, Jiayin; Xu, Zhanwei; Yang, Jun

2017-12-07

The Sn-C bonding content between the SnO 2 and CNTs interface was controlled by the hydrothermal method and subsequent heat treatment. Electrochemical analysis found that the SnO 2 @CNTs with high Sn-C bonding content exhibited much higher capacity contribution from alloying and conversion reaction compared with the low content of Sn-C bonding even after 200 cycles. The high Sn-C bonding content enabled the SnO 2 nanoparticles to stabilize on the CNTs surface, realizing an in situ pulverization process of SnO 2 . The in situ pulverized structure was beneficial to maintain the close electrochemical contact of the working electrode during the long-term cycling and provide ultrafast transfer paths for lithium ions and electrons, which promoted the alloying and conversion reaction kinetics greatly. Therefore, the SnO 2 @CNTs composite with high Sn-C bonding content displayed highly reversible alloying and conversion reaction. It is believed that the composite could be used as a reference for design chemically bonded metal oxide/carbon composite anode materials in lithium-ion batteries.

Sol-gel Technology and Advanced Electrochemical Energy Storage Materials

Science.gov (United States)

Chu, Chung-tse; Zheng, Haixing

1996-01-01

Advanced materials play an important role in the development of electrochemical energy devices such as batteries, fuel cells, and electrochemical capacitors. The sol-gel process is a versatile solution for use in the fabrication of ceramic materials with tailored stoichiometry, microstructure, and properties. This processing technique is particularly useful in producing porous materials with high surface area and low density, two of the most desirable characteristics for electrode materials. In addition,the porous surface of gels can be modified chemically to create tailored surface properties, and inorganic/organic micro-composites can be prepared for improved material performance device fabrication. Applications of several sol-gel derived electrode materials in different energy storage devices are illustrated in this paper. V2O5 gels are shown to be a promising cathode material for solid state lithium batteries. Carbon aerogels, amorphous RuO2 gels and sol-gel derived hafnium compounds have been studied as electrode materials for high energy density and high power density electrochemical capacitors.

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...

Combination of electrochemical processes with membrane bioreactors for wastewater treatment and fouling control: A review

Directory of Open Access Journals (Sweden)

Benny Marie B. Ensano

2016-08-01

Full Text Available This paper provides a critical review about the integration of electrochemical processes into membrane bioreactors (MBR in order to understand the influence of these processes on wastewater treatment performance and membrane fouling control. The integration can be realized either in an internal or an external configuration. Electrically enhanced membrane bioreactors or electro membrane bioreactors (eMBRs combine biodegradation, electrochemical and membrane filtration processes into one system providing higher effluent quality as compared to conventional MBRs and activated sludge plants. Furthermore, electrochemical processes, such as electrocoagulation, electrophoresis and electroosmosis, help to mitigate deposition of foulants into the membrane and enhance sludge dewaterability by controlling the morphological properties and mobility of the colloidal particles and bulk liquid. Intermittent application of minute electric field has proven to reduce energy consumption and operational cost as well as minimize the negative effect of direct current field on microbial activity which are some of the main concerns in eMBR technology. The present review discusses important design considerations of eMBR, its advantages as well as its applications to different types of wastewater. It also presents several challenges that need to be addressed for future development of this hybrid technology which include treatment of high strength industrial wastewater and removal of emerging contaminants, optimization study, cost benefit analysis and the possible combination with microbial electrolysis cell for biohydrogen production.

Controlled synthesis of MnSn(OH)6/graphene nanocomposites and their electrochemical properties as capacitive materials

International Nuclear Information System (INIS)

Wang Gongkai; Sun Xiang; Lu Fengyuan; Yu Qingkai; Liu Changsheng; Lian Jie

2012-01-01

We report the synthesis of novel MnSn(OH) 6 /graphene nanocomposites produced by a co-precipitation method and their potential application for electrochemical energy storage. The hydroxide decorated graphene nanocomposites display better performance over pure MnSn(OH) 6 nanoparticles because the graphene sheets act as conductive bridges improving the ionic and electronic transport. The crystallinity of MnSn(OH) 6 nanoparticles deposited on the surface of graphene sheets also impacts the capacitive properties as electrodes. The maximum capacitance of 31.2 F/g (59.4 F/g based on the mass of MnSn(OH) 6 nanoparticles) was achieved for the sample with a low degree of crystallinity. No significant degradation of capacitance occurred after 500 cycles at a current density of 1.5 A/g in 1 M Na 2 SO 4 aqueous solution, indicating an excellent electrochemical stability. The results serve as an example demonstrating the potential of integrating highly conductive graphene networks into binary metal hydroxide in improving the performance of active electrode materials for electrochemical energy storage applications. - Graphical abstract: Graphite oxide (GO) can be synthesized by oxidizing graphite using Hummers method. Graphene was reduced from GO by thermal exfoliation. In this work, MnSn(OH) 6 /graphene nano-composites were synthesized by a simple co-precipitation method and their electrochemical performances have been explored. Highlights: ► Noval MnSn(OH) 6 /graphene nano-composites were synthesized. ► Microstructure can be tailored by changing the reaction temperature and time. ► Crystallinity of MnSn(OH) 6 nanoparticles impacts capacitive properties as electrode. ► Nano-composites display improved electrochemical performance over MnSn(OH) 6 alone. ► Results serve as an example demonstrating the potential for energy storage.

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.

Rapid and sensitive detection of malachite green in aquaculture water by electrochemical preconcentration and surface-enhanced Raman scattering.

Science.gov (United States)

Xu, Kai-Xuan; Guo, Mei-Hong; Huang, Yu-Ping; Li, Xiao-Dong; Sun, Jian-Jun

2018-04-01

A highly sensitive and rapid method of in-situ surface-enhanced Raman spectroscopy (SERS) combining with electrochemical preconcentration (EP) in detecting malachite green (MG) in aquaculture water was established. Ag nanoparticles (AgNPs) were synthesized and spread onto the surface of gold electrodes after centrifuging to produce SERS-active substrates. After optimizing the pH values, preconcentration potentials and times, in-situ EP-SERS detection was carried out. A sensitive and rapid analysis of the low-concentration MG was accomplished within 200s and the limit of detection was 2.4 × 10 -16 M. Copyright © 2017 Elsevier B.V. All rights reserved.

Chemical modification of graphene aerogels for electrochemical capacitor applications.

Science.gov (United States)

Hong, Jin-Yong; Wie, Jeong Jae; Xu, Yu; Park, Ho Seok

2015-12-14

Graphene aerogel is a relatively new type of aerogel that is ideal for energy storage applications because of its large surface area, high electrical conductivity and good chemical stability. Also, three dimensional interconnected macropores offer many advantages such as low density, fast ion and mass transfer, and easy access to storage sites. Such features allow graphene aerogels to be intensively applied for electrochemical capacitor applications. Despite the growing interest in graphene aerogel-based electrochemical capacitors, however, the graphene aerogels still suffer from their low capacitive performances and high fragility. Both relatively low capacitance and brittleness of physically crosslinked graphene aerogels remain a critical challenge. Until now, a number of alternative attempts have been devoted to overcome these shortcomings. In this perspective, we summarize the recent research progress towards the development of advanced graphene aerogel-based electrochemical capacitors according to the different approaches (e.g. porosity, composition and structure controls). Then, the recently proposed chemical strategies to improve the capacitive performances and mechanical durability of graphene aerogels for practical applications are highlighted. Finally, the current challenges and perspectives in this emerging material are also discussed.

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.

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.

Chip cleaning and regeneration for electrochemical sensor arrays

Energy Technology Data Exchange (ETDEWEB)

Bhalla, Vijayender [Biochemistry Department ' G.Moruzzi' , University of Bologna, Via Irnerio 48, 40126 Bologna (Italy); Carrara, Sandro, E-mail: sandro.carrara@epfl.c [Biochemistry Department ' G.Moruzzi' , University of Bologna, Via Irnerio 48, 40126 Bologna (Italy); Stagni, Claudio [Department DEIS, University of Bologna, viale Risorgimento 2, 40136 Bologna (Italy); Samori, Bruno [Biochemistry Department ' G.Moruzzi' , University of Bologna, Via Irnerio 48, 40126 Bologna (Italy)

2010-04-02

Sensing systems based on electrochemical detection have generated great interest because electronic readout may replace conventional optical readout in microarray. Moreover, they offer the possibility to avoid labelling for target molecules. A typical electrochemical array consists of many sensing sites. An ideal micro-fabricated sensor-chip should have the same measured values for all the equivalent sensing sites (or spots). To achieve high reliability in electrochemical measurements, high quality in functionalization of the electrodes surface is essential. Molecular probes are often immobilized by using alkanethiols onto gold electrodes. Applying effective cleaning methods on the chip is a fundamental requirement for the formation of densely-packed and stable self-assembly monolayers. However, the available well-known techniques for chip cleaning may not be so reliable. Furthermore, it could be necessary to recycle the chip for reuse. Also in this case, an effective recycling technique is required to re-obtain well cleaned sensing surfaces on the chip. This paper presents experimental results on the efficacy and efficiency of the available techniques for initial cleaning and further recycling of micro-fabricated chips. Piranha, plasma, reductive and oxidative cleaning methods were applied and the obtained results were critically compared. Some interesting results were attained by using commonly considered cleaning methodologies. This study outlines oxidative electrochemical cleaning and recycling as the more efficient cleaning procedure for electrochemical based sensor arrays.

Electrochemical mass-flow control of hydrogen using a fullerene-based proton conductor

International Nuclear Information System (INIS)

Maruyama, Ryuichiro

2002-01-01

A membrane electrode assembly (MEA) was fabricated using proton conductive hydrogensulfated fullerenol (C 60 (OSO 3 H) n (OH) n ). Rate-controlled mass flow of hydrogen was performed by applying voltage to both electrodes of the MEA without humidification. The amount of the electrochemically transported hydrogen through the MEA increased as the applied current increased, obeying Faraday's law. Residual gas analysis of the transported hydrogen showed that the transported hydrogen contains trace amounts of water less than 1%

Electrochemical monitoring of biointeraction by graphene-based material modified pencil graphite electrode.

Science.gov (United States)

Eksin, Ece; Zor, Erhan; Erdem, Arzum; Bingol, Haluk

2017-06-15

Recently, the low-cost effective biosensing systems based on advanced nanomaterials have received a key attention for development of novel assays for rapid and sequence-specific nucleic acid detection. The electrochemical biosensor based on reduced graphene oxide (rGO) modified disposable pencil graphite electrodes (PGEs) were developed herein for electrochemical monitoring of DNA, and also for monitoring of biointeraction occurred between anticancer drug, Daunorubicin (DNR), and DNA. First, rGO was synthesized chemically and characterized by using UV-Vis, TGA, FT-IR, Raman Spectroscopy and SEM techniques. Then, the quantity of rGO assembling onto the surface of PGE by passive adsorption was optimized. The electrochemical behavior of rGO-PGEs was examined by cyclic voltammetry (CV). rGO-PGEs were then utilized for electrochemical monitoring of surface-confined interaction between DNR and DNA using differential pulse voltammetry (DPV) technique. Additionally, voltammetric results were complemented with electrochemical impedance spectroscopy (EIS) technique. Electrochemical monitoring of DNR and DNA was resulted with satisfying detection limits 0.55µM and 2.71µg/mL, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

Electrochemical analysis of gold-coated magnetic nanoparticles for detecting immunological interaction

International Nuclear Information System (INIS)

Pham, Thao Thi-Hien; Sim, Sang Jun

2010-01-01

An electrochemical impedance immunosensor was developed for detecting the immunological interaction between human immunoglobulin (IgG) and protein A from Staphylococcus aureus based on the immobilization of human IgG on the surface of modified gold-coated magnetic nanoparticles. The nanoparticles with an Au shell and Fe oxide cores were functionalized by a self-assembled monolayer of 11-mercaptoundecanoic acid. The electrochemical analysis was conducted on the modified magnetic carbon paste electrodes with the nanoparticles. The magnetic nanoparticles were attached to the surface of the magnetic carbon paste electrodes via magnetic force. The cyclic voltammetry technique and electrochemical impedance spectroscopy measurements of the magnetic carbon paste electrodes coated with magnetic nanoparticles-human IgG complex showed changes in its alternating current (AC) response both after the modification of the surface of the electrode and the addition of protein A. The immunological interaction between human IgG on the surface of the modified magnetic carbon paste electrodes and protein A in the solution could be successfully monitored.

Local deposition of anisotropic nanoparticles using scanning electrochemical microscopy (SECM).

Science.gov (United States)

Fedorov, Roman G; Mandler, Daniel

2013-02-28

We demonstrate localized electrodeposition of anisotropic metal nanoobjects, namely Au nanorods (GNR), on indium tin oxide (ITO) using scanning electrochemical microscopy (SECM). A gold microelectrode was the source of the gold ions whereby double pulse chronoamperometry was employed to generate initially Au seeds which were further grown under controlled conditions. The distance between the microelectrode and the ITO surface as well as the different experimental parameters (electrodeposition regime, solution composition and temperature) were optimized to produce faceted gold seeds with the required characteristics (size and distribution). Colloidal chemical synthesis was successfully exploited for better understanding the role of the surfactant and different additives in breaking the crystallographic symmetry and anisotropic growth of GNR. Experiments performed in a conventional three-electrode cell revealed the most appropriate electrochemical conditions allowing high yield synthesis of nanorods with well-defined shape as well as nanocubes and bipyramids.

Electrochemical Energy Storage Applications of CVD Grown Niobium Oxide Thin Films.

Science.gov (United States)

Fiz, Raquel; Appel, Linus; Gutiérrez-Pardo, Antonio; Ramírez-Rico, Joaquín; Mathur, Sanjay

2016-08-24

We report here on the controlled synthesis, characterization, and electrochemical properties of different polymorphs of niobium pentoxide grown by CVD of new single-source precursors. Nb2O5 films deposited at different temperatures showed systematic phase evolution from low-temperature tetragonal (TT-Nb2O5, T-Nb2O5) to high temperature monoclinic modifications (H-Nb2O5). Optimization of the precursor flux and substrate temperature enabled phase-selective growth of Nb2O5 nanorods and films on conductive mesoporous biomorphic carbon matrices (BioC). Nb2O5 thin films deposited on monolithic BioC scaffolds produced composite materials integrating the high surface area and conductivity of the carbonaceous matrix with the intrinsically high capacitance of nanostructured niobium oxide. Heterojunctions in Nb2O5/BioC composites were found to be beneficial in electrochemical capacitance. Electrochemical characterization of Nb2O5/BioC composites showed that small amounts of Nb2O5 (as low as 5%) in conjunction with BioCarbon resulted in a 7-fold increase in the electrode capacitance, from 15 to 104 F g(-1), while imparting good cycling stability, making these materials ideally suited for electrochemical energy storage applications.

Dual responsive supramolecular hydrogel with electrochemical activity.

Science.gov (United States)

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

2011-08-02

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

Electro-oxidation of methanol on gold in alkaline media: Adsorption characteristics of reaction intermediates studied using time resolved electro-chemical impedance and surface plasmon resonance techniques

Science.gov (United States)

Assiongbon, K. A.; Roy, D.

2005-12-01

Electro-catalytic oxidation of methanol is the anode reaction in direct methanol fuel cells. We have studied the adsorption characteristics of the intermediate reactants of this multistep reaction on a gold film electrode in alkaline solutions by combining surface plasmon resonance (SPR) measurements with Fourier transform electro-chemical impedance spectroscopy (FT-EIS). Methanol oxidation in this system shows no significant effects of "site poisoning" by chemisorbed CO. Our results suggest that OH - chemisorbed onto Au acts as a stabilizing agent for the surface species of electro-active methanol. Double layer charging/discharging and adsorption/desorption of OH - show more pronounced effects than adsorption/oxidation of methanol in controlling the surface charge density of the Au substrate. These effects are manifested in both the EIS and the SPR data, and serve as key indicators of the surface reaction kinetics. The data presented here describe the important role of adsorbed OH - in electro-catalysis of methanol on Au, and demonstrate how SPR and FT-EIS can be combined for quantitative probing of catalytically active metal-solution interfaces.

The Surface Coating of Commercial LiFePO4 by Utilizing ZIF-8 for High Electrochemical Performance Lithium Ion Battery

Science.gov (United States)

Xu, XiaoLong; Qi, CongYu; Hao, ZhenDong; Wang, Hao; Jiu, JinTing; Liu, JingBing; Yan, Hui; Suganuma, Katsuaki

2018-03-01

The requirement of energy-storage equipment needs to develop the lithium ion battery (LIB) with high electrochemical performance. The surface modification of commercial LiFePO4 (LFP) by utilizing zeolitic imidazolate frameworks-8 (ZIF-8) offers new possibilities for commercial LFP with high electrochemical performances. In this work, the carbonized ZIF-8 (CZIF-8) was coated on the surface of LFP particles by the in situ growth and carbonization of ZIF-8. Transmission electron microscopy indicates that there is an approximate 10 nm coating layer with metal zinc and graphite-like carbon on the surface of LFP/CZIF-8 sample. The N2 adsorption and desorption isotherm suggests that the coating layer has uniform and simple connecting mesopores. As cathode material, LFP/CZIF-8 cathode-active material delivers a discharge specific capacity of 159.3 mAh g-1 at 0.1C and a discharge specific energy of 141.7 mWh g-1 after 200 cycles at 5.0C (the retention rate is approximate 99%). These results are attributed to the synergy improvement of the conductivity, the lithium ion diffusion coefficient, and the degree of freedom for volume change of LFP/CZIF-8 cathode. This work will contribute to the improvement of the cathode materials of commercial LIB.[Figure not available: see fulltext.

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.

Improved in vivo performance of amperometric oxygen (PO2) sensing catheters via electrochemical nitric oxide generation/release.

Science.gov (United States)

Ren, Hang; Coughlin, Megan A; Major, Terry C; Aiello, Salvatore; Rojas Pena, Alvaro; Bartlett, Robert H; Meyerhoff, Mark E

2015-08-18

A novel electrochemically controlled release method for nitric oxide (NO) (based on electrochemical reduction of nitrite ions) is combined with an amperometric oxygen sensor within a dual lumen catheter configuration for the continuous in vivo sensing of the partial pressure of oxygen (PO2) in blood. The on-demand electrochemical NO generation/release method is shown to be fully compatible with amperometric PO2 sensing. The performance of the sensors is evaluated in rabbit veins and pig arteries for 7 and 21 h, respectively. Overall, the NO releasing sensors measure both venous and arterial PO2 values more accurately with an average deviation of -2 ± 11% and good correlation (R(2) = 0.97) with in vitro blood measurements, whereas the corresponding control sensors without NO release show an average deviation of -31 ± 28% and poor correlation (R(2) = 0.43) at time points >4 h after implantation in veins and >6 h in arteries. The NO releasing sensors induce less thrombus formation on the catheter surface in both veins and arteries (p < 0.05). This electrochemical NO generation/release method could offer a new and attractive means to improve the biocompatibility and performance of implantable chemical sensors.

In situ electrochemical impedance spectroscopy/synchrotron radiation grazing incidence X-ray diffraction-A powerful new technique for the characterization of electrochemical surfaces and interfaces

Energy Technology Data Exchange (ETDEWEB)

De Marco, Roland [Nanochemistry Research Institute, Department of Applied Chemistry, Curtin University of Technology, GPO Box U 1987, Perth, WA 6845 (Australia)]. E-mail: r.demarco@exchange.curtin.edu.au; Jiang, Z.-T. [Nanochemistry Research Institute, Department of Applied Chemistry, Curtin University of Technology, GPO Box U 1987, Perth, WA 6845 (Australia); Martizano, Jay [Nanochemistry Research Institute, Department of Applied Chemistry, Curtin University of Technology, GPO Box U 1987, Perth, WA 6845 (Australia); Lowe, Alex [Nanochemistry Research Institute, Department of Applied Chemistry, Curtin University of Technology, GPO Box U 1987, Perth, WA 6845 (Australia); Pejcic, Bobby [Nanochemistry Research Institute, Department of Applied Chemistry, Curtin University of Technology, GPO Box U 1987, Perth, WA 6845 (Australia); Riessen, Arie van [Materials Research Group, Department of Applied Physics, Curtin University of Technology, GPO Box U 1987, Perth, WA 6845 (Australia)

2006-08-15

A marriage of electrochemical impedance spectroscopy (EIS) and in situ synchrotron radiation grazing incidence X-ray diffraction (SR-GIXRD) has provided a powerful new technique for the elucidation of the mechanistic chemistry of electrochemical systems. In this study, EIS/SR-GIXRD has been used to investigate the influence of metal ion buffer calibration ligands, along with natural organic ligands in seawater, on the behaviour of the iron chalcogenide glass ion-selective electrode (ISE). The SR-GIXRD data demonstrated that citrate - a previously reported poor iron calibration ligand for the analysis of seawater - induced an instantaneous and total dissolution of crystalline GeSe and Sb{sub 2}Se{sub 3} in the modified surface layer (MSL) of the ISE, while natural organic ligands in seawater and a mixture of ligands in a mimetic seawater ligand system protected the MSL's crystalline inclusions of GeSe and Sb{sub 2}Se{sub 3} from oxidative attack. Expectedly, the EIS data showed that citrate induced a loss in the medium frequency time constant for the MSL of the ISE, while seawater's natural organic ligands and the mimetic ligand system preserved the medium frequency EIS response characteristics of the ISE's MSL. The new EIS/SR-GIXRD technique has provided insights into the suitability of iron calibration ligands for the analysis of iron in seawater.

Electrochemically Smart Bimetallic Materials Featuring Group 11 Metals: In-situ Conductive Network Generation and Its Impact on Cell Capacity

Energy Technology Data Exchange (ETDEWEB)

Takeuchi, Esther [Stony Brook Univ., NY (United States)

2016-11-30

Our results for this program “Electrochemically smart bimetallic materials featuring Group 11 metals: in-situ conductive matrix generation and its impact on battery capacity, power and reversibility” have been highly successful: 1) we demonstrated material structures which generated in-situ conductive networks through electrochemical activation with increases in conductivity up to 10,000 fold, 2) we pioneered in situ analytical methodology to map the cathodes at several stages of discharge through the use of Energy Dispersive X-ray Diffraction (EDXRD) to elucidate the kinetic dependence of the conductive network formation, and 3) we successfully designed synthetic methodology for direct control of material properties including crystallite size and surface area which showed significant impact on electrochemical behavior.

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

Science.gov (United States)

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

2016-09-01

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

Buffered Electrochemical Polishing of Niobium

Energy Technology Data Exchange (ETDEWEB)

Ciovati, Gianluigi [Thomas Jefferson National Accelerator Facility (TJNAF), Newport News, VA (United States); Tian, Hui [Thomas Jefferson National Accelerator Facility (TJNAF), Newport News, VA (United States); College of William and Mary, Williamsburg, VA (United States); Corcoran, Sean [Virginia Polytechnic Inst. and State Univ. (Virginia Tech), Blacksburg, VA (United States)

2011-03-01

The standard preparation of superconducting radio-frequency (SRF) cavities made of pure niobium include the removal of a 'damaged' surface layer, by buffered chemical polishing (BCP) or electropolishing (EP), after the cavities are formed. The performance of the cavities is characterized by a sharp degradation of the quality factor when the surface magnetic field exceeds about 90 mT, a phenomenon referred to as 'Q-drop.' In cavities made of polycrystalline fine grain (ASTM 5) niobium, the Q-drop can be significantly reduced by a low-temperature (? 120 °C) 'in-situ' baking of the cavity if the chemical treatment was EP rather than BCP. As part of the effort to understand this phenomenon, we investigated the effect of introducing a polarization potential during buffered chemical polishing, creating a process which is between the standard BCP and EP. While preliminary results on the application of this process to Nb cavities have been previously reported, in this contribution we focus on the characterization of this novel electrochemical process by measuring polarization curves, etching rates, surface finish, electrochemical impedance and the effects of temperature and electrolyte composition. In particular, it is shown that the anodic potential of Nb during BCP reduces the etching rate and improves the surface finish.

In situ monitoring magnetism and resistance of nanophase platinum upon electrochemical oxidation

Directory of Open Access Journals (Sweden)

Eva-Maria Steyskal

2013-06-01

Full Text Available Controlled tuning of material properties by external stimuli represents one of the major topics of current research in the field of functional materials. Electrochemically induced property tuning has recently emerged as a promising pathway in this direction making use of nanophase materials with a high fraction of electrode-electrolyte interfaces. The present letter reports on electrochemical property tuning of porous nanocrystalline Pt. Deeper insight into the underlying processes could be gained by means of a direct comparison of the charge-induced response of two different properties, namely electrical resistance and magnetic moment. For this purpose, four-point resistance measurements and SQUID magnetometry were performed under identical in situ electrochemical control focussing on the regime of electrooxidation. Fully reversible variations of the electrical resistance and the magnetic moment of 6% and 1% were observed upon the formation or dissolution of a subatomic chemisorbed oxygen surface layer, respectively. The increase of the resistance, which is directly correlated to the amount of deposited oxygen, is considered to be primarily caused by charge-carrier scattering processes at the metal–electrolyte interfaces. In comparison, the decrease of the magnetic moment upon positive charging appears to be governed by the electric field at the nanocrystallite–electrolyte interfaces due to spin–orbit coupling.

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.

Electrochemical Impedance Response of the surface treated FMS in Liquid Sodium Environment

International Nuclear Information System (INIS)

Lee, Jeong Hyeon; Shin, Sang Hun; Kim, Ji Hyun

2014-01-01

HT9 and Gr.92 are known as compatible in sodium environment because the usual refueling time of SFRs is designed about 54 months. It is very important to investigate the corrosion-related behavior such as surface corrosion rate, carburization, decarburization and mechanical properties for its operation time. SiC and Si 3 N 4 CVD coating for decarburization barrier on the surface of FMS is considered in this study. The decarburization process where dissolved carbon near the specimen surface disused in to the liquid sodium. This process can originate from the difference between dissolved carbon in the material and liquid sodium. A compatibility test the cladding tube revealed that a decrease of the mechanical property instigated by the aging proves governed the whole mechanical property. To monitor the corrosion behavior of these candidate materials in sodium environment, Electrochemical Impedance Spectroscopy (EIS) method is first introduced and investigated in this study. The compatibility of cladding and structural materials with sodium has to be carefully investigated, as sodium could promote corrosion of cladding and structural materials in two ways. One is produced by the dissolution of alloy constituents into the sodium, and the other is produced through a chemical reaction with impurities (especially oxygen and carbon) in the sodium environment. EIS test with pre-oxidized Gr. 92 specimen in 200 .deg. C liquid sodium environment was carried out in this study. A clear Nyquist and Bode plots were obtained in liquid metal environment and the resistance of sodium and the oxide, and the capacitance of the oxide were measured from this result

Optical and electrical properties of porous silicon layer formed on the textured surface by electrochemical etching

Science.gov (United States)

Weiying, Ou; Lei, Zhao; Hongwei, Diao; Jun, Zhang; Wenjing, Wang

2011-05-01

Porous silicon (PS) layers were formed on textured crystalline silicon by electrochemical etching in HF-based electrolyte. Optical and electrical properties of the TMAH textured surfaces with PS formation are studied. Moreover, the influences of the initial structures and the anodizing time on the optical and electrical properties of the surfaces after PS formation are investigated. The results show that the TMAH textured surfaces with PS formation present a dramatic decrease in reflectance. The longer the anodizing time is, the lower the reflectance. Moreover, an initial surface with bigger pyramids achieved lower reflectance in a short wavelength range. A minimum reflectance of 3.86% at 460 nm is achieved for a short anodizing time of 2 min. Furthermore, the reflectance spectrum of the sample, which was etched in 3 vol.% TMAH for 25 min and then anodized for 20 min, is extremely flat and lies between 3.67% and 6.15% in the wavelength range from 400 to 1040 nm. In addition, for a short anodizing time, a slight increase in the effective carrier lifetime is observed. Our results indicate that PS layers formed on a TMAH textured surface for a short anodization treatment can be used as both broadband antireflection coatings and passivation layers for the application in solar cells.

Optical and electrical properties of porous silicon layer formed on the textured surface by electrochemical etching

Energy Technology Data Exchange (ETDEWEB)

Ou Weiying; Zhao Lei; Diao Hongwei; Zhang Jun; Wang Wenjing, E-mail: wjwangwj@126.com [Key Laboratory of Solar Thermal Energy and Photovoltaic System, Institute of Electrical Engineering, Chinese Academy of Sciences, Beijing 100190 (China)

2011-05-15

Porous silicon (PS) layers were formed on textured crystalline silicon by electrochemical etching in HF-based electrolyte. Optical and electrical properties of the TMAH textured surfaces with PS formation are studied. Moreover, the influences of the initial structures and the anodizing time on the optical and electrical properties of the surfaces after PS formation are investigated. The results show that the TMAH textured surfaces with PS formation present a dramatic decrease in reflectance. The longer the anodizing time is, the lower the reflectance. Moreover, an initial surface with bigger pyramids achieved lower reflectance in a short wavelength range. A minimum reflectance of 3.86% at 460 nm is achieved for a short anodizing time of 2 min. Furthermore, the reflectance spectrum of the sample, which was etched in 3 vol.% TMAH for 25 min and then anodized for 20 min, is extremely flat and lies between 3.67% and 6.15% in the wavelength range from 400 to 1040 nm. In addition, for a short anodizing time, a slight increase in the effective carrier lifetime is observed. Our results indicate that PS layers formed on a TMAH textured surface for a short anodization treatment can be used as both broadband antireflection coatings and passivation layers for the application in solar cells. (semiconductor technology)

Morphology and Activity Tuning of Cu ₃ Pt/C Ordered Intermetallic Nanoparticles by Selective Electrochemical Dealloying

Energy Technology Data Exchange (ETDEWEB)

Wang, Deli; Yu, Yingchao; Zhu, Jing; Liu, Sufen; Muller, David A.; Abruña, Héctor D.

2015-02-11

Improving the catalytic activity of Pt-based bimetallic nanoparticles is a key challenge in the application of proton-exchange membrane fuel cells. Electrochemical dealloying represents a powerful approach for tuning the surface structure and morphology of these catalyst nanoparticles. We present a comprehensive study of using electrochemical dealloying methods to control the morphology of ordered Cu3Pt/C intermetallic nanoparticles, which could dramatically affect their electrocatalytic activity for the oxygen reduction reaction (ORR). Depending on the electrochemical dealloying conditions, the nanoparticles with Pt-rich core–shell or porous structures were formed. We further demonstrate that the core–shell and porous morphologies can be combined to achieve the highest ORR activity. This strategy provides new guidelines for optimizing nanoparticles synthesis and improving electrocatalytic activity.

Carbonate anion controlled growth of LiCoPO4/C nanorods and its improved electrochemical behavior

International Nuclear Information System (INIS)

Gangulibabu; Nallathamby, Kalaiselvi; Meyrick, Danielle; Minakshi, Manickam

2013-01-01

Highlights: ► Carbonate anion controlled growth of LiCoPO 4 nanorods has been prepared. ► Mixture of H 2 CO 3 + (NH 4 ) 2 CO 3 increases the CO 3 2− concentration and acts as an effective growth inhibitor. ► Heating the carbonate rich precursor in an inert atmosphere produces a Co 2 P phase that is conductive. ► Addition of super P carbon resulted in an amorphous carbon coating on LiCoPO 4 particles. ► LiCoPO 4 /C nanorods with a co-existence of Co 2 P exhibit excellent discharge capacity with retention on multiple cycling. -- Abstract: LiCoPO 4 /C nanocomposite with growth controlled by carbonate anions was synthesized via a unique solid-state fusion method. Carbonate anions in the form of H 2 CO 3 or a mixture of H 2 CO 3 + (NH 4 ) 2 CO 3 have been used as a growth inhibiting modifier to produce morphology controlled lithium cobalt phosphate. The presence of cobalt phosphide (Co 2 P) as a second phase improved the conductivity and electrochemical properties of the parent LiCoPO 4. The formation of Co 2 P is found to be achievable only in an inert atmosphere. Super P ® carbon (10 wt.%) provided an adherent carbon coating on pristine LiCoPO 4 resulting in the LiCoPO 4 /C composite cathode. This electrode exhibited enhanced electrochemical properties: capacity of 123 mAh g −1 with excellent capacity retention of 89% after 30 cycles, and reasonable rate capability of up to 5 C rate. The synergistic effect of carbonate anions and formation of Co 2 P under inert atmosphere has influenced the electrochemical behavior of LiCoPO 4 /C cathode through controlling the morphology and increasing the conductivity

The pharmacokinetic study of rutin in rat plasma based on an electrochemically reduced graphene oxide modified sensor

Directory of Open Access Journals (Sweden)

Pei Zhang

2016-04-01

Full Text Available An electrochemical method based on a directly electrochemically reduced graphene oxide (ERGO film coated on a glassy carbon electrode (GCE was developed for the rapid and convenient determination of rutin in plasma. ERGO was modified on the surface of GCE by one-step electro-deposition method. Electrochemical behavior of rutin on ERGO/GCE indicated that rutin underwent a surface-controlled quasi-reversible process and the electrochemical parameters such as charge transfer coefficient (α, electron transfer number (n and electrode reaction standard rate constant (ks were 0.53, 2 and 3.4 s−1, respectively. The electrochemical sensor for rutin in plasma provided a wide linear response range of 4.70×10−7−1.25×10−5 M with the detection limit (s/n=3 of 1.84×10−8 M. The assay was successfully used to the pharmacokinetic study of rutin. The pharmacokinetic parameters such as elimination rate half-life (t1/2, area under curve (AUC, and plasma clearance (CL were calculated to be 3.345±0.647 min, 5750±656.0 µg min/mL, and 5.891±0.458 mL/min/kg, respectively. The proposed method utilized a small sample volume of 10 μL and had no complicated sample pretreatment (without deproteinization, which was simple, eco-friendly, and time- and cost-efficient for rutin pharmacokinetic studies.

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

Reversible mechano-electrochemical writing of metallic nanostructures with the tip of an atomic force microscope

Directory of Open Access Journals (Sweden)

Christian Obermair

2012-12-01

Full Text Available We recently introduced a method that allows the controlled deposition of nanoscale metallic patterns at defined locations using the tip of an atomic force microscope (AFM as a “mechano-electrochemical pen”, locally activating a passivated substrate surface for site-selective electrochemical deposition. Here, we demonstrate the reversibility of this process and study the long-term stability of the resulting metallic structures. The remarkable stability for more than 1.5 years under ambient air without any observable changes can be attributed to self-passivation. After AFM-activated electrochemical deposition of copper nanostructures on a polycrystalline gold film and subsequent AFM imaging, the copper nanostructures could be dissolved by reversing the electrochemical potential. Subsequent AFM-tip-activated deposition of different copper nanostructures at the same location where the previous structures were deleted, shows that there is no observable memory effect, i.e., no effect of the previous writing process on the subsequent writing process. Thus, the four processes required for reversible information storage, “write”, “read”, “delete” and “re-write”, were successfully demonstrated on the nanometer scale.

Reversible mechano-electrochemical writing of metallic nanostructures with the tip of an atomic force microscope.

Science.gov (United States)

Obermair, Christian; Kress, Marina; Wagner, Andreas; Schimmel, Thomas

2012-01-01

We recently introduced a method that allows the controlled deposition of nanoscale metallic patterns at defined locations using the tip of an atomic force microscope (AFM) as a "mechano-electrochemical pen", locally activating a passivated substrate surface for site-selective electrochemical deposition. Here, we demonstrate the reversibility of this process and study the long-term stability of the resulting metallic structures. The remarkable stability for more than 1.5 years under ambient air without any observable changes can be attributed to self-passivation. After AFM-activated electrochemical deposition of copper nanostructures on a polycrystalline gold film and subsequent AFM imaging, the copper nanostructures could be dissolved by reversing the electrochemical potential. Subsequent AFM-tip-activated deposition of different copper nanostructures at the same location where the previous structures were deleted, shows that there is no observable memory effect, i.e., no effect of the previous writing process on the subsequent writing process. Thus, the four processes required for reversible information storage, "write", "read", "delete" and "re-write", were successfully demonstrated on the nanometer scale.

Electrochemical characterization of irreversibly adsorbed germanium on platinum stepped surfaces vicinal to Pt(1 0 0)

International Nuclear Information System (INIS)

Rodriguez, P.; Herrero, E.; Solla-Gullon, J.; Vidal-Iglesias, F.J.; Aldaz, A.; Feliu, J.M.

2005-01-01

The electrochemical behavior of germanium irreversibly adsorbed at stepped surfaces vicinal to the Pt(1 0 0) pole is reported. The process taking part on the (1 0 0) terraces is evaluated from charge density measurements and calibration lines versus the terrace dimension are plotted. On the series Pt(2n - 1,1,1) having (1 1 1) monoatomic steps, the charge involved in the redox process undergone by the irreversibly adsorbed germanium is able to account for (n - 0.5) terrace atoms, thus suggesting some steric difficulties in the growth of the adlayer on the (1 0 0) terraces. Conversely, no steric problems are apparent in the series Pt(n,1,0) in which more open (1 0 0) steps are present on the (1 0 0) terraces. In this latter case the charge density under the germanium redox peaks is proportional to the number of terrace atoms. Some comparison is made with other stepped surfaces to understand the behavior and stability of germanium irreversibly adsorbed on the different platinum surface sites

Influencing Mechanism of Electrochemical Treatment on Preparation of CNTs-grafted on Carbon Fibers

Directory of Open Access Journals (Sweden)

SONG Lei

2017-11-01

Full Text Available Based on electrochemical anodic oxidation, an innovative technique was developed to efficiently obtain the uniform catalyst coating on continuous carbon fibers. Through systematic investigation on the effect of electrochemical modified strength on the physical and chemical characteristics of carbon fiber surface, catalyst particles and the morphology of CNTs-grafted carbon fibers, tensile strength of multi-scale reinforcement and the interlaminar shear strength of its reinforced composites, the electrochemical modification process on carbon fibre surface was optimized. The results show that the morphology and distribution of catalyst particles not only affect the morphology of CNTs deposited on the surface of carbon fibres,but also affect the mechanical properties of multi-scale reinforcement and its reinforced composites of CNTs-grafted carbon fibers.

Deposition of a thin electro-polymerized organic film on iron surface

International Nuclear Information System (INIS)

Lecayon, Gerard

1980-01-01

We use an electrochemical method to prepare a polymerized thin film, obtained from acrylonitrile in a solution of acetonitrile and tetraethylammonium perchlorate. The films are deposited on oxidized iron electrodes, with a surface area varying from a few mm to several cm, their thickness ranges from ten A to thousand A. This result is obtained by controlling the evolution of reactions: duplication, hydrogenation, polymerization which occur during the electrochemical reduction of acrylonitrile. The choice of suitable experimental conditions enhances the polymerization and increases the adherence of the polymer on the electrode. The usual methods of surface studies: S.E.M., A.E.S., S.I.M.S., permit the characterization of the electrode surface and the chemical composition of the deposit films. The molecular structure of polymer, and its evolution under aging or heating was studied by infrared multi-reflection spectroscopy. Very good correlation exists between the electrochemical characteristic: I = f(t), the initial surface state of the electrodes, and the homogeneity of the electro-polymerized films. Diagrams corresponding to mechanisms of different stages of electro-polymerization are proposed. (author) [fr

Electrochemical properties of opal-V6O13 composites

International Nuclear Information System (INIS)

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

2014-01-01

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

Electrochemical remediation technologies for soil and groundwater

Energy Technology Data Exchange (ETDEWEB)

Doering, F. [Electrochemical Processes I.I. c. Valley Forge, PA (United States)]|[P2 Soil Remediation, Inc. Stuttgart (Germany); Doering, N. [P2 Soil Remediation, Inc. Stuttgart (Germany)

2001-07-01

In Direct Current Technologies (DCTs) a direct current electricity is passed between at least two subsurface electrodes in order to effect the remediation of the groundwater and/or the soil. DCTs in line with the U.S.-terminology comprise of the ElectroChemical Remediation Technologies (ECRTs), and GeoKinetics. The primary distinction between ECRTs and ElectroKinetics are the power input, and the mode of operation, which are electrochemical reactions vs. mass transport. ECRTs combine phenomena of colloid (surface) electrochemistry with the phenomena of Induced Polarization (IP). This report focuses on ECRTs, comprising of the ElectroChemical GeoOxidation (ECGO) for the mineralization of organic pollutants to finally carbon dioxide and water, and Induced Complexation (IC), related to the electrochemical conversion of metals enhancing the mobilization and precipitation of heavy metals on both electrodes. Both technologies are based on reduction-oxidation (redox) reactions at the scale of the individual soil particles. (orig.)

Electrochemical Chloride extraction using external electrodes?

DEFF Research Database (Denmark)

Ottosen, Lisbeth M.; Pedersen, Anne Juul

2006-01-01

Electrochemical methods for the removal of chloride from concrete have been developed and the methods are primarily designed for situations where corrosion has started due to an increased chloride concentration in the vicinity of the reinforcement. In these methods the reinforcement is used...... as the cathode. However, some unwanted side effects can occur, including alkali-silica reaction and in some cases hydrogen embrittlement. It is also suggested also to use electrochemical chloride extraction in a preventive way in constructions where chloride induced corrosion is likely to be a problem after...... a period of time, i.e. remove the chlorides before the chloride front reaches the reinforcement. If the chlorides are removed from outer few centimetres from the surface, the chloride will not reach the reinforcement and cause damage. By using the electrochemical chloride removal in this preventive way...

Electrochemical Sensor Coating Based on Electrophoretic Deposition of Au-Doped Self-Assembled Nanoparticles.

Science.gov (United States)

Zhang, Rongli; Zhu, Ye; Huang, Jing; Xu, Sheng; Luo, Jing; Liu, Xiaoya

2018-02-14

The electrophoretic deposition (EPD) of self-assembled nanoparticles (NPs) on the surface of an electrode is a new strategy for preparing sensor coating. By simply changing the deposition conditions, the electrochemical response for an analyte of deposited NPs-based coating can be controlled. This advantage can decrease the difference between different batches of sensor coating and ensure the reproducibility of each sensor. This work investigated the effects of deposition conditions (including deposition voltage, pH value of suspension, and deposition time) on the structure and the electrochemical response for l-tryptophan of sensor coating formed from Au-doped poly(sodium γ-glutamate) with pendant dopamine units nanohybrids (Au/γ-PGA-DA NBs) via the EPD method. The structure and thickness of the deposited sensor coating were measured by atomic force microscopy, which demonstrated that the structure and thickness of coating can be affected by the deposition voltage, the pH value of the suspension, and the deposition time. The responsive current for l-tryptophan of the deposited sensor coating were measured by differential pulse voltammetry, which showed that the responsive current value was affected by the structure and thickness of the deposited coating. These arguments suggested that a rich design-space for tuning the electrochemical response for analyte and a source of variability in the structure of sensor coating can be provided by the deposition conditions. When Au/γ-PGA-DA NBs were deposited on the electrode surface and formed a continuous coating with particle morphology and thinner thickness, the deposited sensor coating exhibited optimal electrochemical response for l-tryptophan.

Effects of low-pressure nitrogen plasma treatment on the surface properties and electrochemical performance of the polyethylene separator used lithium-ion batteries

Science.gov (United States)

Li, Chun; Li, Hsiao-Ling; Li, Chi-Heng; Liu, Yu-Shuan; Sung, Yu-Ching; Huang, Chun

2018-01-01

In this paper, we describe the surface transition of the polyethylene (PE) separator used in lithium-ion batteries treated by low-pressure nitrogen plasma discharge. The nitrogen-plasma-treated PE separator was characterized by contact angle measurement, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and scanning electron microscopy. The electrochemical performance of the lithium ion batteries fabricated with the nitrogen-plasma-treated separator was also evaluated. Results showed that polar functionalization groups were induced on the PE surface by the nitrogen plasma discharge, causing the surface to become hydrophilic. The increases in surface wettability and surface free energy result in electrolyte retention improvement. Moreover, the nitrogen plasma-treated PE separator leads to superior performance in lithium-ion battery assembly.

Binder-free carbon nanotube electrode for electrochemical removal of chromium.

Science.gov (United States)

Wang, Haitao; Na, Chongzheng

2014-11-26

Electrochemical treatment of chromium-containing wastewater has the advantage of simultaneously reducing hexavalent chromium (CrVI) and reversibly adsorbing the trivalent product (CrIII), thereby minimizing the generation of waste for disposal and providing an opportunity for resource reuse. The application of electrochemical treatment of chromium is often limited by the available electrochemical surface area (ESA) of conventional electrodes with flat surfaces. Here, we report the preparation and evaluation of carbon nanotube (CNT) electrodes consisting of vertically aligned CNT arrays directly grown on stainless steel mesh (SSM). We show that the 3-D organization of CNT arrays increases ESA up to 13 times compared to SSM. The increase of ESA is correlated with the length of CNTs, consistent with a mechanism of roughness-induced ESA enhancement. The increase of ESA directly benefits CrVI reduction by proportionally accelerating reduction without compromising the electrode's ability to adsorb CrIII. Our results suggest that the rational design of electrodes with hierarchical structures represents a feasible approach to improve the performance of electrochemical treatment of contaminated water.

A low cost computer-controlled electrochemical measurement system for education and research

International Nuclear Information System (INIS)

Cottis, R.A.

1989-01-01

With the advent of low cost computers of significant processing power, it has become economically attractive, as well as offering practical advantages, to replace conventional electrochemical instrumentation with computer-based equipment. For example, the equipment to be described can perform all of the functions required for the measurement of a potentiodynamic polarization curve, replacing the conventional arrangement of sweep generator, potentiostat and chart recorder at a cost (based on the purchase cost of parts) which is less than that of most chart recorders alone. Additionally the use of computer control at a relatively low level provides a versatility (assuming the development of suitable software) which cannot easily be matched by conventional instruments. As a result of these considerations a simple computer-controlled electrochemical measurement system has been developed, with a primary aim being its use in teaching an MSc class in corrosion science and engineering, with additional applications in MSc and PhD research. For education reasons the design of the user interface has tried to make the internal operation of the unit as obvious as possible, and thereby minimize the tendency for students to treat the unit as a 'black box' with incomprehensible inner workings. This has resulted in a unit in which the three main components of function generator, potentiostat and recorder are presented as independent areas on the front panel, and can be configured by the user in exactly the same way as conventional instruments. (author) 11 figs

A low cost computer-controlled electrochemical measurement system for education and research

Energy Technology Data Exchange (ETDEWEB)

Cottis, R A [Manchester Univ. (UK). Inst. of Science and Technology

1989-01-01

With the advent of low cost computers of significant processing power, it has become economically attractive, as well as offering practical advantages, to replace conventional electrochemical instrumentation with computer-based equipment. For example, the equipment to be described can perform all of the functions required for the measurement of a potentiodynamic polarization curve, replacing the conventional arrangement of sweep generator, potentiostat and chart recorder at a cost (based on the purchase cost of parts) which is less than that of most chart recorders alone. Additionally the use of computer control at a relatively low level provides a versatility (assuming the development of suitable software) which cannot easily be matched by conventional instruments. As a result of these considerations a simple computer-controlled electrochemical measurement system has been developed, with a primary aim being its use in teaching an MSc class in corrosion science and engineering, with additional applications in MSc and PhD research. For education reasons the design of the user interface has tried to make the internal operation of the unit as obvious as possible, and thereby minimize the tendency for students to treat the unit as a 'black box' with incomprehensible inner workings. This has resulted in a unit in which the three main components of function generator, potentiostat and recorder are presented as independent areas on the front panel, and can be configured by the user in exactly the same way as conventional instruments. (author) 11 figs.

Infrared spectroscopy of model electrochemical interfaces in ultrahigh vacuum: some implications for ionic and chemisorbate solvation at electrode surfaces

Science.gov (United States)

Villegas, Ignacio; Kizhakevariam, Naushad; Weaver, Michael J.

1995-07-01

The utility of infrared reflection-absorption spectroscopy (IRAS) for examining structure and bonding for model electrochemical interfaces in ultrahigh vacuum (UHV) is illustrated, focusing specifically on the solvation of cations and chemisorbed carbon monoxide on Pt(111). These systems were chosen partly in view of the availability of IRAS data (albeit limited to chemisorbate vibrations) for the corresponding in-situ metal-solution interfaces, enabling direct spectral comparisons to be made with the "UHV electrochemical model" systems. Kelvin probe measurements of the metal-UHV surface potential changes (ΔΦ) attending alterations in the interfacial composition are also described: these provide the required link to the in-situ electrode potentials as well as yielding additional insight into surface solvation. Variations in the negative electronic charge density and, correspondingly, in the cation surface concentration (thereby mimicking charge-induced alterations in the electrode potential below the potential of zero charge) are achieved by potassium atom dosage onto Pt(111). Of the solvents selected for discussion here — deuterated water, methanol, and acetonitrile — the first two exhibit readily detectable vibrational bands which provide information on the ionic solvation structure. Progressively dosing these solvents onto Pt(111) in the presence of low potassium coverages yields marked alterations in the solvent vibrational bands which can be understood in terms of sequential cation solvation. Comparison between these spectra for methanol with analogous data for sequential methanol solvation of gas-phase alkali cations enables the influence of the interfacial environment to be assessed. The effects of solvating chemisorbed CO are illustrated for acetonitrile; the markedly larger shifts in CO frequencies and binding sites for dilute CO adlayers can be accounted for in terms of short-range coadsorbate interactions in addition to longer-range Stark effects

Electrochemical study of stress corrosion cracking of copper alloys

International Nuclear Information System (INIS)

Malki, Brahim

1999-01-01

This work deals with the electrochemical study of stress corrosion of copper alloys in aqueous environment. Selective dissolution and electrochemical oxidation are two key-points of the stress corrosion of these alloys. The first part of this thesis treats of these aspects applied to Cu-Au alloys. Measurements have been performed using classical electrochemical techniques (in potentio-dynamic, potentio-static and galvano-static modes). The conditions of occurrence of an electrochemical noise is analysed using signal processing techniques. The impact on the behavior of Cu 3 Au are discussed. In the second part, the stress corrosion problem is addressed in the case of surface oxide film formation, in particular for Cu-Zn alloys. We have found useful to extend this study to mechanical stress oxidation mechanisms in the presence of an oscillating potential electrochemical system. The aim is to examine the influence of these new electrochemical conditions (galvano-static mode) on the behavior of stressed brass. Finally, the potential distribution at crack tip is calculated in order to compare the different observations [fr

The chemical and electrochemical anisotropic etching of silicon

International Nuclear Information System (INIS)

Dixon, E.

1997-06-01

The success of silicon IC technology in producing a wide variety of microstructures relies heavily on the orientation dependant etching observed for silicon in alkaline media. Despite the rapid growth of this industry, the chemical and electrochemical mechanisms by which anisotropic etching occurs remain poorly understood. The most common etchant systems in use are ethylenediamine-pyrocatechol-water (EPW) and potassium hydroxide-isopropanol-water (KOH-IPA), and whilst these systems are highly plane selective they each have distinct disadvantages. The occurrence of inhomogeneities such as micropyramids and pits on the surface of etched substrates is a particularly disadvantageous characteristic of many alkaline etching systems. A complete understanding of the chemical and electrochemical anisotropic etching mechanisms is essential in order to obtain more reproducible etching, improved etch rate ratios and the development of more reliable etching baths. Wet chemical etching experiments to evaluate the etching rates for the different alkali metal cations have shown that similar etch rates are observed for LiOH, NaOH and KOH but those of RbOH and CsOH are significantly lower. The presence of impurities was shown to worsen the etched wafer's surface finish obtained in these etching baths. Additives have been shown to dramatically improve the surface finish with the presence of IPA in conjunction with etchant oxygenation virtually eliminating all surface defects. Electrochemical experiments were used to assess the electrochemical behaviour of Si p-(100) in of a wide variety of etchants and variations were seen according to the etchant used. A.C impedance spectroscopy showed a variation in the flat-band potential (V FB ) according to alkali metal hydroxide etchant used. These trends were similarly observed in the presence of isopropanol. Oxygenation was observed to reproducibly alter the flat-band potentials. A.c impedance spectroscopic studies additionally confirmed the

Electrochemical investigations of the interaction of C-reactive protein (CRP) with a CRP antibody chemically immobilized on a gold surface

International Nuclear Information System (INIS)

Hennessey, Hooman; Afara, Nadia; Omanovic, Sasha; Padjen, Ante L.

2009-01-01

A possibility of using a range of dc and ac electrochemical techniques to probe associative interactions of C-reactive protein (CRP) with CRP antibody (aCRP) immobilized on a gold electrode surface was investigated. It was demonstrated that the investigated electrochemical techniques can be used efficiently to probe these interactions over a wide CRP concentration range, from 1.15 x 10 -5 to 1.15 mg L -1 . The measured sensitivity of the techniques is in the following decreasing order: differential pulse voltammetry, charge-transfer resistance obtained from electrochemical impedance spectroscopy (EIS), cyclic voltammetry, chronoamperometry, and double-layer capacitance deduced from EIS measurements which gave the poorest sensitivity. Measurements of kinetic parameters demonstrated that the associative interactions of CRP with the immobilized aCRP reached quasi-equilibrium after 20-30 min. The kinetics of these interactions was modeled successfully using a two-step kinetic model. In this model, the first step represents reversible CRP-aCRP associative-dissociative interactions, while the second step represents the irreversible transformation of the bound CRP into a thermodynamically stable configuration. It was demonstrated that the thermodynamically stable configuration of CRP starts prevailing after 7 min of interaction of CRP with the immobilized aCRP.

Evaluation and improvement of dynamic optimality in electrochemical reactors

International Nuclear Information System (INIS)

Vijayasekaran, B.; Basha, C. Ahmed

2005-01-01

A systematic approach for the dynamic optimization problem statement to improve the dynamic optimality in electrochemical reactors is presented in this paper. The formulation takes an account of the diffusion phenomenon in the electrode/electrolyte interface. To demonstrate the present methodology, the optimal time-varying electrode potential for a coupled chemical-electrochemical reaction scheme, that maximizes the production of the desired product in a batch electrochemical reactor with/without recirculation are determined. The dynamic optimization problem statement, based upon this approach, is a nonlinear differential algebraic system, and its solution provides information about the optimal policy. Optimal control policy at different conditions is evaluated using the best-known Pontryagin's maximum principle. The two-point boundary value problem resulting from the application of the maximum principle is then solved using the control vector iteration technique. These optimal time-varying profiles of electrode potential are then compared to the best uniform operation through the relative improvements of the performance index. The application of the proposed approach to two electrochemical systems, described by ordinary differential equations, shows that the existing electrochemical process control strategy could be improved considerably when the proposed method is incorporated

Identifying the Active Surfaces of Electrochemically Tuned LiCoO2 for Oxygen Evolution Reaction

International Nuclear Information System (INIS)

Lu, Zhiyi; Chen, Guangxu; Li, Yanbin; Wang, Haotian; Xie, Jin

2017-01-01

Identification of active sites for catalytic processes has both fundamental and technological implications for rational design of future catalysts. Herein, we study the active surfaces of layered lithium cobalt oxide (LCO) for the oxygen evolution reaction (OER) using the enhancement effect of electrochemical delithiation (De-LCO). Our theoretical results indicate that the most stable (0001) surface has a very large overpotential for OER independent of lithium content. In contrast, edge sites such as the nonpolar (1120) and polar (0112) surfaces are predicted to be highly active and dependent on (de)lithiation. The effect of lithium extraction from LCO on the surfaces and their OER activities can be understood by the increase of Co 4+ sites relative to Co 3+ and by the shift of active oxygen 2p states. Experimentally, it is demonstrated that LCO nanosheets, which dominantly expose the (0001) surface show negligible OER enhancement upon delithiation. However, a noticeable increase in OER activity (~0.1 V in overpotential shift at 10 mA cm –2 ) is observed for the LCO nanoparticles, where the basal plane is greatly diminished to expose the edge sites, consistent with the theoretical simulations. In addition, we find that the OER activity of De-LCO nanosheets can be improved if we adopt an acid etching method on LCO to create more active edge sites, which in turn provides a strong evidence for the theoretical indication.

Development of an electrochemical biosensor for vitamin B12 using D-phenylalanine nanotubes

Science.gov (United States)

Moazeni, Maryam; Karimzadeh, Fathallah; Kermanpur, Ahmad; Allafchian, Alireza

2018-01-01

In the past decades, biosensors are one of the most interesting topics among researchers and scientist. The biosensors are used in several applications such as determining food quality, control and diagnose clinical problems and metabolic control. Therefore, many efforts have been carried out to design and develop a new generation of these systems. On the other hand nanotechnology by improving the performance of sensors has created an excellent outlook. Using nanomaterials such as nanoparticles, nanotubes, nanowires, and nanorods in diagnostic tools has been significantly increased accuracy, sensitivity and improved detection limits in sensors. In this study, the one-dimensional morphology of the D-phenylalanine was assembled on the surface of the gold electrode. In the next step electrochemical performance of the modified electrode was investigated by Cyclic Voltammetry (CV), Electrochemical Impedance Spectroscopy (EIS) and Differential Pals Voltammograms (DPV). Finally, by measuring the different concentrations of vitamin B12, the detection limit of the biosensor was obtained 1.6 µM.

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.

Preparation and Electrochemical Properties of Silver Doped Hollow Carbon Nanofibers

Directory of Open Access Journals (Sweden)

LI Fu

2016-11-01

Full Text Available Silver doped PAN-based hollow carbon nanofibers were prepared combining co-electrospinning with in situ reduction technique subsequently heat treatment to improve the electrochemical performances of carbon based supercapacitor electrodes. The morphology, structure and electrochemical performances of the resulted nanofiber were studied. The results show that the silver nanoparticles can be doped on the surface of hollow carbon nanofibers and the addition of silver favors the improvement of the electrochemical performances, exhibiting the enhanced reversibility of electrode reaction and the capacitance and the reduced charge transfer impedance.

A miniaturized silicon based device for nucleic acids electrochemical detection

Directory of Open Access Journals (Sweden)

Salvatore Petralia

2015-12-01

Full Text Available In this paper we describe a novel portable system for nucleic acids electrochemical detection. The core of the system is a miniaturized silicon chip composed by planar microelectrodes. The chip is embedded on PCB board for the electrical driving and reading. The counter, reference and work microelectrodes are manufactured using the VLSI technology, the material is gold for reference and counter electrodes and platinum for working electrode. The device contains also a resistor to control and measuring the temperature for PCR thermal cycling. The reaction chamber has a total volume of 20 μL. It is made in hybrid silicon–plastic technology. Each device contains four independent electrochemical cells.Results show HBV Hepatitis-B virus detection using an unspecific DNA intercalating redox probe based on metal–organic compounds. The recognition event is sensitively detected by square wave voltammetry monitoring the redox signals of the intercalator that strongly binds to the double-stranded DNA. Two approaches were here evaluated: (a intercalation of electrochemical unspecific probe on ds-DNA on homogeneous solution (homogeneous phase; (b grafting of DNA probes on electrode surface (solid phase.The system and the method here reported offer better advantages in term of analytical performances compared to the standard commercial optical-based real-time PCR systems, with the additional incomes of being potentially cheaper and easier to integrate in a miniaturized device. Keywords: Electrochemical detection, Real time PCR, Unspecific DNA intercalator

The strategies of DNA immobilization and hybridization detection mechanism in the construction of electrochemical DNA sensor: A review

Directory of Open Access Journals (Sweden)

Jahwarhar Izuan Abdul Rashid

2017-11-01

Full Text Available In recent years, electrochemical deoxyribonucleic acid (DNA sensor has recently emerged as promising alternative clinical diagnostic devices especially for infectious disease by exploiting DNA recognition events and converting them into an electrochemical signal. This is because the existing DNA diagnostic method possesses certain drawbacks such as time-consuming, expensive, laborious, low selectivity and sensitivity. DNA immobilization strategies and mechanism of electrochemical detection are two the most important aspects that should be considered before developing highly selective and sensitive electrochemical DNA sensor. Here, we focus on some recent strategies for DNA probes immobilization on the surface of electrochemical transducer such as adsorption, covalent bonding and Avidin/Streptavidin-Biotin interaction on the electrode surface for specific interaction with its complementary DNA target. A numerous approach for DNA hybridization detection based electrochemical technique that frequently used including direct DNA electrochemical detection and label based electrochemical (redox-active indicator, enzyme label and nanoparticles were also discussed in aiming to provide general guide for the design of electrochemical DNA sensor. We also discussed the challenges and suggestions to improve the application of electrochemical DNA sensor at point-care setting. Keywords: Electrochemical DNA sensor, DNA immobilization, DNA hybridization, Electrochemical mechanism

A critical revisit of the key parameters used to describe microbial electrochemical systems

International Nuclear Information System (INIS)

Sharma, Mohita; Bajracharya, Suman; Gildemyn, Sylvia; Patil, Sunil A.; Alvarez-Gallego, Yolanda; Pant, Deepak; Rabaey, Korneel; Dominguez-Benetton, Xochitl

2014-01-01

Graphical abstract: - Abstract: Many microorganisms have the innate capability to discharge and/or receive electrons to and from solid state materials such as electrodes. This ability is now used towards innovative processes in wastewater treatment, power generation, production of fuels and biochemicals, bioremediation, desalination and resource recovery, among others. Despite being a dynamic field in science and technology, significant challenges remain towards industrial implementation which include representation of judicious performance indicators. This critical review outlines the progress in current density evaluated per projected surface area of electrodes, the most wide-spread performance indicator. It also proposes guidelines to correct current and exchange current per porous surface area, biofilm covered area, electrochemically- or bioelectrochemically- active surface area, of the electrodes. Recommendations for indicators to describe the environmental and electrochemical robustness of electrochemically-active biofilms are portrayed, including preservation of the predominant functionality as well as electrochemical mechanistic and phenomenological features. A few additional key elements for industrial processing are depicted. Whereas Microbial Fuel Cells (MFCs) are the main focus, some important parameters for reporting on cathodic bioproduction performance are also discussed. This critical revision aims to provide key parameters to compare the whole spectrum of microbial electrochemical systems in a consistent way

Current Progress of Nanomaterials in Molecularly Imprinted Electrochemical Sensing.

Science.gov (United States)

Zhong, Chunju; Yang, Bin; Jiang, Xinxin; Li, Jianping

2018-01-02

Nanomaterials have received much attention during the past decade because of their excellent optical, electronic, and catalytic properties. Nanomaterials possess high chemical reactivity, also high surface energy. Thus, provide a stable immobilization platform for biomolecules, while preserving their reactivity. Due to the conductive and catalytic properties, nanomaterials can also enhance the sensitivity of molecularly imprinted electrochemical sensors by amplifying the electrode surface, increasing the electron transfer, and catalyzing the electrochemical reactions. Molecularly imprinted polymers that contain specific molecular recognition sites can be designed for a particular target analyte. Incorporating nanomaterials into molecularly imprinted polymers is important because nanomaterials can improve the response signal, increase the sensitivity, and decrease the detection limit of the sensors. This study describes the classification of nanomaterials in molecularly imprinted polymers, their analytical properties, and their applications in the electrochemical sensors. The progress of the research on nanomaterials in molecularly imprinted polymers and the application of nanomaterials in molecularly imprinted polymers is also reviewed.

Carbon Nanostructures for Tagging in Electrochemical Biosensing: A Review

Directory of Open Access Journals (Sweden)

Paloma Yáñez-Sedeño

2017-01-01

Full Text Available Growing demand for developing ultrasensitive electrochemical bioassays has led to the design of numerous signal amplification strategies. In this context, carbon-based nanomaterials have been demonstrated to be excellent tags for greatly amplifying the transduction of recognition events and simplifying the protocols used in electrochemical biosensing. This relevant role is due to the carbon-nanomaterials’ large surface area, excellent biological compatibility and ease functionalization and, in some cases, intrinsic electrochemistry. These carbon-based nanomaterials involve well-known carbon nanotubes (CNTs and graphene as well as the more recent use of other carbon nanoforms. This paper briefly discusses the advantages of using carbon nanostructures and their hybrid nanocomposites for amplification through tagging in electrochemical biosensing platforms and provides an updated overview of some selected examples making use of labels involving carbon nanomaterials, acting both as carriers for signal elements and as electrochemical tracers, applied to the electrochemical biosensing of relevant (biomarkers.

Nucleation and Growth of Porous MnO2 Coatings Prepared on Nickel Foam and Evaluation of Their Electrochemical Performance

Directory of Open Access Journals (Sweden)

Wenxin Huang

2018-05-01

Full Text Available Porous MnO2 was uniformly electrodeposited on nickel foam in MnSO4 solution, which was applied as the electrode of supercapacitors. The nucleation/growth mechanisms of porous MnO2 were investigated firstly. Then two kinds of electrochemical measuring technologies, corresponding to the cycle voltammetry (CV and galvanostatic charge-discharge, were adopted to assess the electrochemical performance of MnO2 electrodes. The results demonstrated that the deposition of MnO2 on nickel foam included four stages. Prior to the deposition, an extremely short incubation period of about 2 s was observed (the first stage. Then the exposed nickel foam was instantly covered by a large number of MnO2 crystal nuclei and crystal nuclei connected with each other in a very short time of about 3 s (the second stage. Nucleation predominated in the second stage. The sharply rise of current was caused by the increase in substrate surface area which due to nucleation of MnO2. Grain boundaries grew preferentially due to their high energy, accompanied with a honeycomb-like structure with the higher surface area was formed. However, accompanied with the electrochemical reactions gradually diffusion-controlled, the current presented the decline trend with increasing the time (the third stage. When the electrochemical reactions were completely diffusion-controlled, the porous MnO2 coating with an approximately constant surface area was formed (the fourth stage. MnO2 coatings deposited for different time (30, 60, 120, 300 s exhibited a similar specific capacitance (CV: about 224 F/g; galvanostatic charge-discharge: about 264 F/g. Comparatively speaking, the value of MnO2 deposited for 600 s was highest (CV: 270 F/g; galvanostatic charge-discharge: 400 F/g.

Controllability of Surface Water Networks

Science.gov (United States)

Riasi, M. Sadegh; Yeghiazarian, Lilit

2017-12-01

To sustainably manage water resources, we must understand how to control complex networked systems. In this paper, we study surface water networks from the perspective of structural controllability, a concept that integrates classical control theory with graph-theoretic formalism. We present structural controllability theory and compute four metrics: full and target controllability, control centrality and control profile (FTCP) that collectively determine the structural boundaries of the system's control space. We use these metrics to answer the following questions: How does the structure of a surface water network affect its controllability? How to efficiently control a preselected subset of the network? Which nodes have the highest control power? What types of topological structures dominate controllability? Finally, we demonstrate the structural controllability theory in the analysis of a wide range of surface water networks, such as tributary, deltaic, and braided river systems.

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

Application of electrochemical processes to membrane bioreactors for improving nutrient removal and fouling control.

Science.gov (United States)

Borea, Laura; Naddeo, Vincenzo; Belgiorno, Vincenzo

2017-01-01

Membrane bioreactor (MBR) technology is becoming increasingly popular as wastewater treatment due to the unique advantages it offers. However, membrane fouling is being given a great deal of attention so as to improve the performance of this type of technology. Recent studies have proven that the application of electrochemical processes to MBR represents a promising technological approach for membrane fouling control. In this work, two intermittent voltage gradients of 1 and 3 V/cm were applied between two cylindrical perforated electrodes, immersed around a membrane module, at laboratory scale with the aim of investigating the treatment performance and membrane fouling formation. For comparison purposes, the reactor also operated as a conventional MBR. Mechanisms of nutrient removal were studied and membrane fouling formation evaluated in terms of transmembrane pressure variation over time and sludge relative hydrophobicity. Furthermore, the impact of electrochemical processes on transparent exopolymeric particles (TEP), proposed as a new membrane fouling precursor, was investigated in addition to conventional fouling precursors such as bound extracellular polymeric substances (bEPS) and soluble microbial products (SMP). All the results indicate that the integration of electrochemical processes into a MBR has the advantage of improving the treatment performance especially in terms of nutrient removal, with an enhancement of orthophosphate (PO 4 -P) and ammonia nitrogen (NH 4 -N) removal efficiencies up to 96.06 and 69.34 %, respectively. A reduction of membrane fouling was also observed with an increase of floc hydrophobicity to 71.72 %, a decrease of membrane fouling precursor concentrations, and, thus, of membrane fouling rates up to 54.33 %. The relationship found between TEP concentration and membrane fouling rate after the application of electrochemical processes confirms the applicability of this parameter as a new membrane fouling indicator.

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

Diversity in electrochemical oxidation of dihydroxybenzenes in the ...

Indian Academy of Sciences (India)

Abstract. Electrochemical oxidation of some catechol derivatives (1a–e) have been studied in water/ acetonitrile solution containing 1-methylindole (3) as a nucleophile, using cyclic voltammetry and controlled- potential coulometry. An interesting diversity in the mechanisms has been observed in electrochemical oxidation ...

A facile electrochemical intercalation and microwave assisted exfoliation methodology applied to screen-printed electrochemical-based sensing platforms to impart improved electroanalytical outputs.

Science.gov (United States)

Pierini, Gastón D; Foster, Christopher W; Rowley-Neale, Samuel J; Fernández, Héctor; Banks, Craig E

2018-06-12

Screen-printed electrodes (SPEs) are ubiquitous with the field of electrochemistry allowing researchers to translate sensors from the laboratory to the field. In this paper, we report an electrochemically driven intercalation process where an electrochemical reaction uses an electrolyte as a conductive medium as well as the intercalation source, which is followed by exfoliation and heating/drying via microwave irradiation, and applied to the working electrode of screen-printed electrodes/sensors (termed EDI-SPEs) for the first time. This novel methodology results in an increase of up to 85% of the sensor area (electrochemically active surface area, as evaluated using an outer-sphere redox probe). Upon further investigation, it is found that an increase in the electroactive area of the EDI-screen-printed based electrochemical sensing platforms is critically dependent upon the analyte and its associated electrochemical mechanism (i.e. adsorption vs. diffusion). Proof-of-concept for the electrochemical sensing of capsaicin, a measure of the hotness of chillies and chilli sauce, within both model aqueous solutions and a real sample (Tabasco sauce) is demonstrated in which the electroanalytical sensitivity (a plot of signal vs. concentration) is doubled when utilising EDI-SPEs over that of SPEs.

Study of electrochemical phosphate conversion coating of metallic surfaces

International Nuclear Information System (INIS)

Gougelin, Patrick

1985-01-01

After an overview on phosphate conversion coating processes, on models of iron electrochemical dissolution, on the passivation phenomenon, and on the phosphate conversion coating treatment, this research thesis reports a detailed study of this last process. The author presents the experimental method, reports the study of this process and of passivation under constant polarization. He reports the use of various techniques and conditions: chrono-amperometry, chrono-potentiometry, cyclic volt-amperometry

Parabens abatement from surface waters by electrochemical advanced oxidation with boron doped diamond anodes.