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

NASA Astrophysics Data System (ADS)

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

2017-11-01

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

Electrochemical machining process for forming surface roughness elements on a gas turbine shroud

DOEpatents

Lee, Ching-Pang; Johnson, Robert Alan; Wei, Bin; Wang, Hsin-Pang

2002-01-01

The back side recessed cooling surface of a shroud defining in part the hot gas path of a turbine is electrochemically machined to provide surface roughness elements and spaces therebetween to increase the heat transfer coefficient. To accomplish this, an electrode with insulating dielectric portions and non-insulating portions is disposed in opposition to the cooling surface. By passing an electrolyte between the cooling surface and electrode and applying an electrical current between the electrode and a shroud, roughness elements and spaces therebetween are formed in the cooling surface in opposition to the insulating and non-insulating portions of the electrode, hence increasing the surface area and heat transfer coefficient of the shroud.

Sputtered Pd as Hydrogen Storage for a Chip-Integrated Microenergy System

PubMed Central

Slavcheva, E.; Ganske, G.; Schnakenberg, U.

2014-01-01

The work presents a research on preparation and physical and electrochemical characterisation of dc magnetron sputtered Pd films envisaged for application as hydrogen storage in a chip-integrated hydrogen microenergy system. The influence of the changes in the sputtering pressure on the surface structure, morphology, and roughness was analysed by X-ray diffraction (XRD), scanning electron microscopy (SEM), and atomic force microscopy (AMF). The electrochemical activity towards hydrogen adsorption/desorption and formation of PdH were investigated in 0.5 M H2SO4 using the methods of cyclic voltammetry and galvanostatic polarisation. The changes in the electrical properties of the films as a function of the sputtering pressure and the level of hydrogenation were evaluated before and immediately after the electrochemical charging tests, using a four-probe technique. The research resulted in establishment of optimal sputter regime, ensuring fully reproducible Pd layers with highly developed surface, moderate porosity, and mechanical stability. Selected samples were integrated as hydrogen storage in a newly developed unitized microenergy system and tested in charging (water electrolysis) and discharging (fuel cell) operative mode at ambient conditions demonstrating a stable recycling performance. PMID:24516356

Glass-ceramic coated Mg-Ca alloys for biomedical implant applications.

PubMed

Rau, J V; Antoniac, I; Fosca, M; De Bonis, A; Blajan, A I; Cotrut, C; Graziani, V; Curcio, M; Cricenti, A; Niculescu, M; Ortenzi, M; Teghil, R

2016-07-01

Biodegradable metals and alloys are promising candidates for biomedical bone implant applications. However, due to the high rate of their biodegradation in human body environment, they should be coated with less reactive materials, such, for example, as bioactive glasses or glass-ceramics. Fort this scope, RKKP composition glass-ceramic coatings have been deposited on Mg-Ca(1.4wt%) alloy substrates by Pulsed Laser Deposition method, and their properties have been characterized by a number of techniques. The prepared coatings consist of hydroxyapatite and wollastonite phases, having composition close to that of the bulk target material used for depositions. The 100μm thick films are characterized by dense, compact and rough morphology. They are composed of a glassy matrix with various size (from micro- to nano-) granular inclusions. The average surface roughness is about 295±30nm due to the contribution of micrometric aggregates, while the roughness of the fine-texture particulates is approximately 47±4nm. The results of the electrochemical corrosion evaluation tests evidence that the RKKP coating improves the corrosion resistance of the Mg-Ca (1.4wt%) alloy in Simulated Body Fluid. Copyright © 2016 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yan, Wei; Liu, Hongtao, E-mail: liuht100@126.com; Sun, Qinghe

A facile and quick fabrication method was proposed to prepare superhydrophobic surfaces on iron substrate by chemical immersion and subsequent stearic acid modification. The association between wettability and surface morphology was studied through altering the copper ion concentration and immersion time. Surface tension instrument, scanning electron microscopy, x-ray diffraction, x-ray photoelectron spectroscopy, and electrochemical workstation were used to characterize the wettability, physical morphology, chemical composition, and corrosion resistance ability of the prepared film. Results showed that both the rough micro/nanostructures and low surface energy material play critical roles in surface wettability. The superhydrophobic film achieved a better anticorrosion property comparedmore » to barrier iron by analysis of open circuit potential, potentiodynamic polarization curves, and Nyquist plots. In addition, the superhydrophobic surface showed excellent performance of acid and alkali resistance, anti-icing, and self-cleaning through a series of environmental tests. This study provides a valid method for quick-preparation of the stable superhydrophobic surfaces, which has a promising application in steel buildings and facilities.« less

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Erçarıkcı, Elif; Dağcı, Kader; Topçu, Ezgi

2014-07-01

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

Hybrid Coatings Enriched with Tetraethoxysilane for Corrosion Mitigation of Hot-Dip Galvanized Steel in Chloride Contaminated Simulated Concrete Pore Solutions

PubMed Central

Figueira, Rita B.; Callone, Emanuela; Silva, Carlos J. R.; Pereira, Elsa V.; Dirè, Sandra

2017-01-01

Hybrid sol-gel coatings, named U(X):TEOS, based on ureasilicate matrices (U(X)) enriched with tetraethoxysilane (TEOS), were synthesized. The influence of TEOS addition was studied on both the structure of the hybrid sol-gel films as well as on the electrochemical properties. The effect of TEOS on the structure of the hybrid sol-gel films was investigated by solid state Nuclear Magnetic Resonance. The dielectric properties of the different materials were investigated by electrochemical impedance spectroscopy. The corrosion behavior of the hybrid coatings on HDGS was studied in chloride-contaminated simulated concrete pore solutions (SCPS) by polarization resistance measurements. The roughness of the HDGS coated with hybrids was also characterized by atomic force microscopy. The structural characterization of the hybrid materials proved the effective reaction between Jeffamine® and 3-isocyanate propyltriethoxysilane (ICPTES) and indicated that the addition of TEOS does not seem to affect the organic structure or to increase the degree of condensation of the hybrid materials. Despite the apparent lack of influence on the hybrids architecture, the polarization resistance measurements confirmed that TEOS addition improves the corrosion resistance of the hybrid coatings (U(X):TEOS) in chloride-contaminated SCPS when compared to samples prepared without any TEOS (U(X)). This behavior could be related to the decrease in roughness of the hybrid coatings (due TEOS addition) and to the different metal coating interaction resulting from the increase of the inorganic component in the hybrid matrix. PMID:28772667

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

PubMed

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

2014-01-01

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

Superwetting and aptamer functionalized shrink-induced high surface area electrochemical sensors.

PubMed

Hauke, A; Kumar, L S Selva; Kim, M Y; Pegan, J; Khine, M; Li, H; Plaxco, K W; Heikenfeld, J

2017-08-15

Electrochemical sensing is moving to the forefront of point-of-care and wearable molecular sensing technologies due to the ability to miniaturize the required equipment, a critical advantage over optical methods in this field. Electrochemical sensors that employ roughness to increase their microscopic surface area offer a strategy to combatting the loss in signal associated with the loss of macroscopic surface area upon miniaturization. A simple, low-cost method of creating such roughness has emerged with the development of shrink-induced high surface area electrodes. Building on this approach, we demonstrate here a greater than 12-fold enhancement in electrochemically active surface area over conventional electrodes of equivalent on-chip footprint areas. This two-fold improvement on previous performance is obtained via the creation of a superwetting surface condition facilitated by a dissolvable polymer coating. As a test bed to illustrate the utility of this approach, we further show that electrochemical aptamer-based sensors exhibit exceptional signal strength (signal-to-noise) and excellent signal gain (relative change in signal upon target binding) when deployed on these shrink electrodes. Indeed, the observed 330% gain we observe for a kanamycin sensor is 2-fold greater than that seen on planar gold electrodes. Copyright © 2017 Elsevier B.V. All rights reserved.

Bio-active synthesis of tin oxide nanoparticles using eggshell membrane for energy storage application

NASA Astrophysics Data System (ADS)

Celina Selvakumari, J.; Nishanthi, S. T.; Dhanalakshmi, J.; Ahila, M.; Pathinettam Padiyan, D.

2018-05-01

Nano-sized tin oxide (SnO2) particles were synthesized using eggshell membrane (ESM), a natural bio-waste from the chicken eggshell. The crystallization of SnO2 into the tetragonal structure was confirmed from powder X-ray diffraction and the crystallite size ranged from 13 to 40 nm. Various shapes including rod, hexagonal and spherical SnO2 nanoparticles were observed from the morphological studies. The electrochemical impedance study revealed a lower charge transfer resistance (Rct) of 8.565 Ω and the presence of a constant phase element which arised due to surface roughness and porosity. Capacitive behavior seen in the cyclic voltammetry curve of the prepared SnO2 nanoparticles, find future applications in supercapacitors.

Corrosion Performance of Nano-ZrO₂ Modified Coatings in Hot Mixed Acid Solutions.

PubMed

Xu, Wenhua; Wang, Zhenyu; Han, En-Hou; Wang, Shuai; Liu, Qian

2018-06-01

A nano-ZrO₂ modified coating system was prepared by incorporation of nano-ZrO₂ concentrates into phenolic-epoxy resin. The corrosion performance of the coatings was evaluated in hot mixed acid solution, using electrochemical methods combined with surface characterization, and the effects of nano-ZrO₂ content were specially focused on. The results showed that 1% and 3% nano-ZrO₂ addition enhanced the corrosion resistance of the coatings, while 5% nano-ZrO₂ addition declined it. The coating with 3% nano-ZrO₂ presented the minimum amount of species diffusion, the lowest average roughness (5.94 nm), and the highest C/O ratio (4.55) and coating resistance, and it demonstrated the best corrosion performance among the coating specimens.

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

PubMed Central

2014-01-01

Two α-MnO2 crystals with caddice-clew-like and urchin-like morphologies are prepared by the hydrothermal method, and their structure and electrochemical performance are characterized by scanning electron microscope (SEM), X-ray diffraction (XRD), galvanostatic cell cycling, cyclic voltammetry, and electrochemical impedance spectroscopy (EIS). The morphology of the MnO2 prepared under acidic condition is urchin-like, while the one prepared under neutral condition is caddice-clew-like. The identical crystalline phase of MnO2 crystals is essential to evaluate the relationship between electrochemical performances and morphologies for lithium-ion battery application. In this study, urchin-like α-MnO2 crystals with compact structure have better electrochemical performance due to the higher specific capacity and lower impedance. We find that the relationship between electrochemical performance and morphology is different when MnO2 material used as electrochemical supercapacitor or as anode of lithium-ion battery. For lithium-ion battery application, urchin-like MnO2 material has better electrochemical performance. PMID:24982603

Electroactive polymer-peptide conjugates for adhesive biointerfaces.

PubMed

Maione, Silvana; Gil, Ana M; Fabregat, Georgina; Del Valle, Luis J; Triguero, Jordi; Laurent, Adele; Jacquemin, Denis; Estrany, Francesc; Jiménez, Ana I; Zanuy, David; Cativiela, Carlos; Alemán, Carlos

2015-10-15

Electroactive polymer-peptide conjugates have been synthesized by combining poly(3,4-ethylenedioxythiophene), a polythiophene derivative with outstanding properties, and an Arg-Gly-Asp (RGD)-based peptide in which Gly has been replaced by an exotic amino acid bearing a 3,4-ethylenedioxythiophene ring in the side chain. The incorporation of the peptide at the ends of preformed PEDOT chains has been corroborated by both FTIR and X-ray photoelectron spectroscopy. Although the morphology and topology are not influenced by the incorporation of the peptide at the ends of PEDOT chains, this process largely affects other surface properties. Thus, the wettability of the conjugates is considerably higher than that of PEDOT, independently of the synthetic strategy, whereas the surface roughness only increases when the conjugate is obtained using a competing strategy (i.e. growth of the polymer chains against termination by end capping). The electrochemical activity of the conjugates has been found to be higher than that of PEDOT, evidencing the success of the polymer-peptide links designed by chemical similarity. Density functional theory calculations have been used not only to ascertain the conformational preferences of the peptide but also to interpret the electronic transitions detected by UV-vis spectroscopy. Electroactive surfaces prepared using the conjugates displayed the higher bioactivities in terms of cell adhesion, with the relative viabilities being dependent on the roughness, wettability and electrochemical activity of the conjugate. In addition to the influence of the peptide fragment in the initial cell attachment and subsequent cell spreading and survival, the results indicate that PEDOT promotes the exchange of ions at the conjugate-cell interface.

Electrochemical behavior and biological response of Mesenchymal Stem Cells on cp-Ti after N-ions implantation

NASA Astrophysics Data System (ADS)

Rizwan, M.; Ahmad, A.; Deen, K. M.; Haider, W.

2014-11-01

Titanium and its alloys are most widely used as implant materials due to their excellent biocompatibility, mechanical properties and chemical stability. In this study Nitrogen ions of known dosage were implanted over cp-Ti by Pelletron accelerator with beam energy of 0.25 MeV.The atomic force microscopy of bare and nitrogen implanted specimens confirmed increase in surface roughness with increase in nitrogen ions concentration. X-ray diffraction patterns of ions implanted surfaces validated the formation of TiN0.3 and Ti3N2-xnitride phases. The tendency to form passive film and electrochemical behavior of these surfaces in ringer lactate (RL) solution was evaluated by Potentiodynamic polarization and electrochemical impedance spectroscopy respectively. It is proved that nitrogen ions implantation was beneficial to reduce corrosion rate and stabilizing passive film by increasing charge transfer resistance in RL. It was concluded that morphology and proliferation of Mesenchymal Stem Cells on nitrogen ions implanted surfaces strongly depends on surface roughness and nitride phases.

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.

PubMed

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.

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

PubMed Central

Neupane, Dharmendra; Nepal, Bishal; Mikhaylov, Vasilii; Stine, Keith J.

2018-01-01

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. PMID:29547580

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

PubMed

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.

Preparation of Conducting Polymers by Electrochemical Methods and Demonstration of a Polymer Battery

ERIC Educational Resources Information Center

Goto, Hiromasa; Yoneyama, Hiroyuki; Togashi, Fumihiro; Ohta, Reina; Tsujimoto, Akitsu; Kita, Eiji; Ohshima, Ken-ichi

2008-01-01

The electrochemical polymerization of aniline and pyrrole, and demonstrations of electrochromism and the polymer battery effect, are presented as demonstrations suitable for high school and introductory chemistry at the university level. These demonstrations promote student interest in the electrochemical preparation of conducting polymers, where…

Uniform β-Co(OH)2 disc-like nanostructures prepared by low-temperature electrochemical rout as an electrode material for supercapacitors

NASA Astrophysics Data System (ADS)

Aghazadeh, Mustafa; Shiri, Hamid Mohammad; Barmi, Abbas-Ali Malek

2013-05-01

Uniform nanostructures of cobalt hydroxide were successfully prepared by a low-temperature electrochemical method via galvanostatically deposition from a 0.005 M Co(NO3)3 bath at 10 °C. The XRD and FT-IR analyses showed that the prepared sample has a single crystalline hexagonal phase of the brucite-like Co(OH)2. Morphological characterization by SEM and TEM revealed that the prepared β-Co(OH)2 was composed of uniform compact disc-like nanostructures with diameters of 40-50 nm. The electrochemical performance of the prepared β-Co(OH)2 was evaluated using cyclic voltammetry and charge-discharge tests. A maximum specific capacitance of 736.5 F g-1 was obtained in aqueous 1 M KOH with the potential range of -0.2-0.5 V (vs. Ag/AgCl) at the scan rate of 10 mV s-1, suggesting the potential application of the prepared nanostructures as an electrode material in electrochemical supercapacitors. The results of this work showed that the low-temperature cathodic electrodeposition method can be recognized as a new and facile route for the synthesis of cobalt hydroxide nanodiscs as a promising candidate for the electrochemical supercapacitors.

Effect of hydrodynamics and surface roughness on the electrochemical behaviour of carbon steel in CSG produced water

NASA Astrophysics Data System (ADS)

Eyu, Gaius Debi; Will, Geoffrey; Dekkers, Willem; MacLeod, Jennifer

2015-12-01

The influence of fluid flow, surface roughness and immersion time on the electrochemical behaviour of carbon steel in coal seam gas produced water under static and hydrodynamic conditions has been studied. The disc electrode surface morphology before and after the corrosion test was characterized using scanning electron microscopy (SEM). The corrosion product was examined using X-ray photoelectron spectroscopy (XPS) and X-ray diffractometry (XRD).The results show that the anodic current density increased with increasing surface roughness and consequently a decrease in corrosion surface resistance. Under dynamic flow conditions, the corrosion rate increased with increasing rotating speed due to the high mass transfer coefficient and formation of non-protective akaganeite β-FeO(OH) and goethite α-FeO(OH) corrosion scale at the electrode surface. The corrosion rate was lowest at 0 rpm. The corrosion rate decreased in both static and dynamic conditions with increasing immersion time. The decrease in corrosion rate is attributed to the deposition of corrosion products on the electrode surface. SEM results revealed that the rougher surface exhibited a great tendency toward pitting corrosion.

Electrodeposition of gold thin films with controlled morphologies and their applications in electrocatalysis and SERS.

PubMed

Elias, Jamil; Gizowska, Magdalena; Brodard, Pierre; Widmer, Roland; Dehazan, Yoram; Graule, Thomas; Michler, Johann; Philippe, Laetitia

2012-06-29

Here, an easy and effective electrochemical route towards the synthesis of gold thin films with well-controlled roughness, morphology and crystallographic orientation is reported. To control these different factors, the applied potential during deposition played a major role. A tentative nucleation and growth mechanism is demonstrated by means of electrochemical characterizations and a formation mechanism is proposed. Interestingly, the differences in geometry and orientation of the different gold deposits have shown a clear correlation with the electrocatalytical activity in the case of oxygen sensing. In addition, not only the electrocatalytical activity but also the surface-enhanced Raman scattering of the gold deposits have been found to depend both on the roughness and on the size of the surface nanostructures, allowing a fine tuning by controlling these two parameters during deposition.

Electrodeposition of gold thin films with controlled morphologies and their applications in electrocatalysis and SERS

NASA Astrophysics Data System (ADS)

Elias, Jamil; Gizowska, Magdalena; Brodard, Pierre; Widmer, Roland; deHazan, Yoram; Graule, Thomas; Michler, Johann; Philippe, Laetitia

2012-06-01

Here, an easy and effective electrochemical route towards the synthesis of gold thin films with well-controlled roughness, morphology and crystallographic orientation is reported. To control these different factors, the applied potential during deposition played a major role. A tentative nucleation and growth mechanism is demonstrated by means of electrochemical characterizations and a formation mechanism is proposed. Interestingly, the differences in geometry and orientation of the different gold deposits have shown a clear correlation with the electrocatalytical activity in the case of oxygen sensing. In addition, not only the electrocatalytical activity but also the surface-enhanced Raman scattering of the gold deposits have been found to depend both on the roughness and on the size of the surface nanostructures, allowing a fine tuning by controlling these two parameters during deposition.

THE STRUCTURE OF THE COLLODION MEMBRANE AND ITS ELECTRICAL BEHAVIOR

PubMed Central

Sollner, Karl; Carr, Charles W.; Abrams, Irving

1942-01-01

1. Theoretical considerations lead to the conclusion that dissociable acidic groups present to a varying extent in different collodion preparations determine the electrochemical behavior of membranes cast from these preparations. It is further reasoned that the base exchange capacity of the collodion surfaces is the true quantitative measure of the abundance of the dissociable groups. 2. The concept of base exchange capacity and the base exchange method are discussed. The conditions which allow a purposeful application of the latter are stated. 3. The base exchange properties of a number of fibrous collodion preparations of different origins and after various types of treatment, having widely varying electrochemical activities, are determined. 4. With the chemical (titration) and physical (electrometric) methods employed, no regular correlation can be found between electrochemical activity and base exchange. The base exchange capacity which is necessary to cause even great electrochemical activity of collodion is extremely small. 5. Measurable to high base exchange capacity always seems to be associated with good or high electrochemical activity; but base exchange capacity too low to be definitely measurable with the available methods may be found with collodion preparations of high as well as with preparations of low electrochemical activity. 6. The bearing of these results upon the problem of the spatial and electrical structure of the collodion membrane is indicated briefly. PMID:19873284

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

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

Preparation of superhydrophobic titanium surfaces via electrochemical etching and fluorosilane modification

NASA Astrophysics Data System (ADS)

Lu, Yao; Xu, Wenji; Song, Jinlong; Liu, Xin; Xing, Yingjie; Sun, Jing

2012-12-01

The preparation of superhydrophobic surfaces on hydrophilic metal substrates depends on both surface microstructures and low surface energy modification. In this study, a simple and inexpensive electrochemical method for preparing robust superhydrophobic titanium surfaces is reported. The neutral sodium chloride solution is used as electrolyte. Fluoroalkylsilane (FAS) was used to reduce the surface energy of the electrochemically etched surface. Scanning electron microscopy (SEM) images, energy-dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FTIR) spectra, and contact angle measurement are performed to characterize the morphological features, chemical composition, and wettability of the titanium surfaces. Stability and friction tests indicate that the prepared titanium surfaces are robust. The analysis of electrolyte, reaction process, and products demonstrates that the electrochemical processing is very inexpensive and environment-friendly. This method is believed to be easily adaptable for use in large-scale industry productions to promote the application of superhydrophobic titanium surfaces in aviation, aerospace, shipbuilding, and the military industry.

Effect of surface roughness on the in vitro degradation behaviour of a biodegradable magnesium-based alloy

NASA Astrophysics Data System (ADS)

Walter, R.; Kannan, M. Bobby; He, Y.; Sandham, A.

2013-08-01

In this study, the in vitro degradation behaviour of AZ91 magnesium alloy with two different surface finishes was investigated using electrochemical impedance spectroscopy (EIS) in simulated body fluid (SBF). The polarisation resistance (Rp) of the rough surface alloy immersed in SBF for 3 h was ~30% lower as compared to that of the smooth surface alloy. After 12 h immersion in SBF, the Rp values for both the surface finishes decreased and were also similar. However, localised degradation occurred sooner, and to a noticeably higher severity in the rough surface alloy as compared to the smooth surface alloy.

A comparative study of electrochemical machining process parameters by using GA and Taguchi method

NASA Astrophysics Data System (ADS)

Soni, S. K.; Thomas, B.

2017-11-01

In electrochemical machining quality of machined surface strongly depend on the selection of optimal parameter settings. This work deals with the application of Taguchi method and genetic algorithm using MATLAB to maximize the metal removal rate and minimize the surface roughness and overcut. In this paper a comparative study is presented for drilling of LM6 AL/B4C composites by comparing the significant impact of numerous machining process parameters such as, electrolyte concentration (g/l),machining voltage (v),frequency (hz) on the response parameters (surface roughness, material removal rate and over cut). Taguchi L27 orthogonal array was chosen in Minitab 17 software, for the investigation of experimental results and also multiobjective optimization done by genetic algorithm is employed by using MATLAB. After obtaining optimized results from Taguchi method and genetic algorithm, a comparative results are presented.

Optimizing growth and post treatment of diamond for high capacitance neural interfaces.

PubMed

Tong, Wei; Fox, Kate; Zamani, Akram; Turnley, Ann M; Ganesan, Kumaravelu; Ahnood, Arman; Cicione, Rosemary; Meffin, Hamish; Prawer, Steven; Stacey, Alastair; Garrett, David J

2016-10-01

Electrochemical and biological properties are two crucial criteria in the selection of the materials to be used as electrodes for neural interfaces. For neural stimulation, materials are required to exhibit high capacitance and to form intimate contact with neurons for eliciting effective neural responses at acceptably low voltages. Here we report on a new high capacitance material fabricated using nitrogen included ultrananocrystalline diamond (N-UNCD). After exposure to oxygen plasma for 3 h, the activated N-UNCD exhibited extremely high electrochemical capacitance greater than 1 mF/cm(2), which originates from the special hybrid sp(2)/sp(3) structure of N-UNCD. The in vitro biocompatibility of the activated N-UNCD was then assessed using rat cortical neurons and surface roughness was found to be critical for healthy neuron growth, with best results observed on surfaces with a roughness of approximately 20 nm. Therefore, by using oxygen plasma activated N-UNCD with appropriate surface roughness, and considering the chemical and mechanical stability of diamond, the fabricated neural interfaces are expected to exhibit high efficacy, long-term stability and a healthy neuron/electrode interface. Copyright © 2016 Elsevier Ltd. All rights reserved.

Electrical behavior of natural manganese dioxide (NMD)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gorgulho, H.F.; Fernandes, R.Z.D.; Pernaut, J.M.

NMD samples from Brazil have been submitted to magnetic and particle size separations and characterized by X-ray diffraction and fluorescence and thermogravimetric analyses. Results showed that simple physical treatments can lead to more than 60% enriched MnO{sub 2} materials which could satisfy some electrochemical applications. The electrical properties of the samples conditioned as pressed pellets have been investigated by four-points direct current probe and impedance spectroscopy, varying the conditions of preparation and measurement. It is proposed that the higher frequency impedance is equivalent to the intrinsic electronic resistance of the MnO{sub 2} phases while at lower frequencies occurs an interphasemore » charge separation coupled with a possible ionic transport. The corresponding contact resistance depends on the particle size distribution of the material, the compactation pressure of pellets and the iron content of the materials. The interphase dielectric relaxation does not behave ideally; the depression of the impedance semicircles as shown in the Nyquist plane is assumed to be related to the roughness of the bulk interfaces. Recent developments have shown the possibility of using manganese oxides as reversible electrodes for battery or supercapacitor applications for electrical vehicle. In these perspectives it is important to study the electrical and electrochemical properties of NMD in order to estimate its suitability for this kind of applications.« less

Potentiostatic controlled nucleation and growth modes of electrodeposited cobalt thin films on n-Si(1 1 1)

NASA Astrophysics Data System (ADS)

Mechehoud, Fayçal; Khelil, Abdelbacet; Eddine Hakiki, Nour; Bubendorff, Jean-Luc

2016-08-01

The nucleation and growth of Co electrodeposits on n-Si(1 1 1) substrate have been investigated as a function of the applied potential in a large potential range using electrochemical techniques (voltammetry and chrono-amperometry) and surface imaging by atomic force microscopy (AFM). The surface preparation of the sample is crucial and we achieve a controlled n-Si(1 1 1) surface with mono-atomic steps and flat terraces. Using Scharifker-Hills models for fitting the current-time transients, we show that a transition from an instantaneous nucleation process to a progressive one occurs when the overpotential increases. A good agreement between the nucleation and growth parameters extracted from the models and the AFM data's is observed. The growth is of the Volmer-Weber type with a roughness and a spatial extension in the substrate plane of the deposited islands that increase with thickness.

Electrochemical detection of nitrite on poly(pyronin Y)/graphene nanocomposites modified ITO substrate

NASA Astrophysics Data System (ADS)

Şinoforoğlu, Mehmet; Dağcı, Kader; Alanyalıoğlu, Murat; Meral, Kadem

2016-06-01

The present study reports on an easy preparation of poly(pyronin Y)/graphene (poly(PyY)/graphene) nanocomposites thin films on indium tin oxide coated glass substrates (ITO). The thin films of poly(PyY)/graphene nanocomposites are prepared by a novel method consisting of three steps; (i) preparation of graphene oxide (GO) thin films on ITO by spin-coating method, (ii) self-assembly of PyY molecules from aqueous solution onto the GO thin film, (iii) surface-confined electropolymerization (SCEP) of the adsorbed PyY molecules on the GO thin film. The as-prepared poly(PyY)/graphene nanocomposites thin films are characterized by using electroanalytical and spectroscopic techniques. Afterwards, the graphene-based polymeric dye thin film on ITO is used as an electrode in an electrochemical cell. Its performance is tested for electrochemical detection of nitrite. Under optimized conditions, the electrocatalytical effect of the nanocomposites thin film through electrochemical oxidation of nitrite is better than that of GO coated ITO.

Specific anion effects on copper surface through electrochemical treatment: Enhanced photoelectrochemical CO2 reduction activity of derived nanostructures induced by chaotropic anions

NASA Astrophysics Data System (ADS)

Navaee, Aso; Salimi, Abdollah

2018-05-01

Copper derivatives are the most prominent CO2 reduction electrocatalyst. Herein, the metallic copper has been electrochemically treated with some of common ionic salts such as N3bar, HPO2bar, S2bar, Fbar, Clbar, Brbar and Ibar based on the dissolution of a metallic working electrode in an aqueous solution to derive the surface roughness incorporated with nanostructures. Diverse surface morphology can be obtained when the ionic radii of anions are changed. Surface study reveals various roughness shapes based on the size and polarity of the anions, where the ions with higher ionic radii have higher impact on the Cu surface. In comparison, polyatomic oxyanion such as HPO2bar even with large ionic radii do not have enough strength to create the surface roughness than that of oxygen-free anions with large ionic radii. The photoelectrochemical behavior of the modified surfaces toward CO2 reduction is studied at a wide potential window in bicarbonate aqueous solution. Based on our investigations, treated surfaces by Ibar, Clbar and S2bargive a more surface roughness, while Ibar and N3bar offer higher catalytic activity toward CO2 reduction due to possible complexing ability of these anions with Cu cations, followed by formation of the co-catalyst semiconductor and facilitate electron transfer. This methodology can be applied to investigate the effect of ions on transition metals along with obtaining different surface morphologies tailored to different applications.

Poly(vinyl Alcohol) Borate Gel Polymer Electrolytes Prepared by Electrodeposition and Their Application in Electrochemical Supercapacitors.

PubMed

Jiang, Mengjin; Zhu, Jiadeng; Chen, Chen; Lu, Yao; Ge, Yeqian; Zhang, Xiangwu

2016-02-10

Gel polymer electrolytes (GPEs) have been studied for preparing flexible and compact electrochemical energy storage devices. However, the preparation and use of GPEs are complex, and most GPEs prepared through traditional methods do not have good wettability with the electrodes, which retard them from achieving their performance potential. In this study, these problems are addressed by conceiving and implementing a simple, but effective, method of electrodepositing poly(vinyl alcohol) potassium borate (PVAPB) GPEs directly onto the surfaces of active carbon electrodes for electrochemical supercapacitors. PVAPB GPEs serve as both the electrolyte and the separator in the assembled supercapacitors, and their scale and shape are determined solely by the geometry of the electrodes. PVAPB GPEs have good bonding to the active electrode materials, leading to excellent and stable electrochemical performance of the supercapacitors. The electrochemical performance of PVAPB GPEs and supercapacitors can be manipulated simply by adjusting the concentration of KCl salt used during the electrodeposition process. With a 0.9 M KCl concentration, the as-prepared supercapacitors deliver a specific capacitance of 65.9 F g(-1) at a current density of 0.1 A g(-1) and retain more than 95% capacitance after 2000 charge/discharge cycles at a current density of 1 A g(-1). These supercapacitors also exhibit intelligent high voltage self-protection function due to the electrolysis-induced cross-linking effect of PVAPB GPEs.

Chemical etching of stainless steel 301 for improving performance of electrochemical capacitors in aqueous electrolyte

NASA Astrophysics Data System (ADS)

Jeżowski, P.; Nowicki, M.; Grzeszkowiak, M.; Czajka, R.; Béguin, F.

2015-04-01

The main purpose of the study was to increase the surface roughness of stainless steel 301 current collectors by etching, in order to improve the electrochemical performance of electrical double-layer capacitors (EDLC) in 1 mol L-1 lithium sulphate electrolyte. Etching was realized in 1:3:30 (HNO3:HCl:H2O) solution with times varying up to 10 min. For the considered 15 μm thick foil and a mass loss around 0.4 wt.%, pitting was uniform, with diameter of pits ranging from 100 to 300 nm. Atomic force microscopy (AFM) showed an increase of average surface roughness (Ra) from 5 nm for the as-received stainless steel foil to 24 nm for the pitted material. Electrochemical impedance spectroscopy realized on EDLCs with coated electrodes either on as-received or pitted foil in 1 mol L-1 Li2SO4 gave equivalent distributed resistance (EDR) of 8 Ω and 2 Ω, respectively, demonstrating a substantial improvement of collector/electrode interface after pitting. Correlatively, the EDLCs with pitted collector displayed a better charge propagation and low ohmic losses even at relatively high current of 20 A g-1. Hence, chemical pitting of stainless steel current collectors is an appropriate method for optimising the performance of EDLCs in neutral aqueous electrolyte.

High Power Electrochemical Capacitors

DTIC Science & Technology

2012-03-23

electrochemical properties of vanadium oxide aerogels prepared by a freeze-drying process. Journal of the Electrochemical Society, 2004. 151(5): p...Electrochemical Society, 2002. 149(1): p. A26-A30. 12. Rolison, D.R. and B. Dunn, Electrically conductive oxide aerogels : new materials in...surface area vanadium oxide aerogels . Electrochemical and Solid-State Letters, 2000. 3(10): p. 457-459. 14. Shembel, E., et al., Synthesis, investigation

One-pot preparation of PEDOT:PSS-reduced graphene decorated with Au nanoparticles for enzymatic electrochemical sensing of H2O2

NASA Astrophysics Data System (ADS)

Mercante, Luiza A.; Facure, Murilo H. M.; Sanfelice, Rafaela C.; Migliorini, Fernanda L.; Mattoso, Luiz H. C.; Correa, Daniel S.

2017-06-01

The development of novel graphene-based nanocomposites is a hotspot in materials science due to their unique optical, electronic, thermal, mechanical and catalytic properties for varied applications. The present work reports on the development of a graphene-based ternary nanocomposite of poly(3,4-ethylenedioxythiophene)-poly(styrenesulfonate), reduced graphene oxide and gold nanoparticles (PEDOT:PSS-rGO-AuNPs) for the detection of hydrogen peroxide (H2O2). The hybrid nanocomposite showed superior electrochemical properties and higher stability compared to each individual component as electrode materials, showing a synergistic effect between PEDOT, rGO and AuNPs. The nanocomposite was obtained via a facile one-step approach and was assembly with horseradish peroxidase (HRP). The PEDOT:PSS-rGO-AuNPs-HRP modified electrode has been used for the amperometric detection of H2O2 and exhibited a high sensitivity of up to 677 μA mM-1 cm-2, with a wide linear range from 5 to 400 μM and a low detection limit of 0.08 μM (S/N = 3). This developed enzymatic biosensor showed to be highly stable and unresponsive to potentially interfering substances, and it could be used for sensing H2O2 in real samples, including tap water and bovine milk samples. These enhanced sensing performance could be ascribed to the intimate contact of AuNPs onto the rough surface of the PEDOT:PSS-rGO nanocomposite, which has a high electrical conductivity and large surface area, providing it as an excellent substrate for the growth and support of nanoparticles. The method developed in this work opens up a general route to prepare a wide range of graphene-based hybrid nanocomposite films with multiple functions including sensing and biosensing.

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

NASA Astrophysics Data System (ADS)

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.

Preparing the key metabolite of Z-ligustilide in vivo by a specific electrochemical reaction.

PubMed

Duan, Feipeng; Xu, Wenjuan; Liu, Jie; Jia, Zhixin; Chen, Kuikui; Chen, Yijun; Wang, Mingxia; Ma, Kaiyue; Dong, Jiaojiao; Chen, Lianming; Xiao, Hongbin

2018-04-16

The key in vivo metabolites of a drug play an important role in its efficacy and toxicity. However, due to the low content and instability of these metabolites, they are hard to obtain through in vivo methods. Electrochemical reactions can be an efficient alternative to biotransformation in vivo for the preparation of metabolites. Accordingly, in this study, the metabolism of Z-ligustilide was investigated in vitro by electrochemistry coupled online to mass spectrometry. This work showed that five oxidation products of the electrochemical reaction were detected and that two of the oxidation products (senkyunolide I and senkyunolide H) were identified from liver microsomal incubation as well. Furthermore, after intragastric administration of Z-ligustilide in rats, senkyunolide I and senkyunolide H were detected in the rat plasma and liver, while 6,7-epoxyligustilide, a key intermediate metabolite of Z-ligustilide, was difficult to detect in vivo. By contrast, 6,7-epoxyligustilide was obtained from the electrochemical reaction. In addition, for the first time, 6 mg of 6,7-epoxyligustilide was prepared from 120 mg of Z-ligustilide. Therefore, electrochemical reactions represent an efficient laboratory method for preparing key drug metabolites. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Porous MnO2 prepared by sol-gel method for electrochemical supercapacitor

NASA Astrophysics Data System (ADS)

Bazzi, K.; Kumar, A.; Jayakumar, O. D.; Nazri, G. A.; Naik, V. M.; Naik, R.

2015-03-01

MnO2 has attracted great attention as material for electrochemical pseudocapacitor due to its high theoretical specific faradic capacitance (~ 1370 F .g-1) , environmental friendliness and wide potential window in both aqueous and nonaqueous electrolytes. However, the MnO2 has a low surface area which depresses its electrochemical performance. The amorphous α-MnO2 composite was synthesized by sol gel method in the presence of the tri-block copolymer P123. Our aim is to investigate the role of P123 on the electrochemical performance of MnO2. The samples with and without P123 were prepared and characterized by x-ray diffraction (XRD), SEM, TEM and Brunauer-Emmett-Teller (BET) method. The electrochemical performances of the amorphous MnO2 composites as the electrode materials for supercapacitors were evaluated by cyclic voltammetry and AC impedance measurements in a 1M Na2SO4 solution. The results show that the sample prepared without P123 exhibited a relatively low specific capacitance of 28F .g-1, whereas the porous MnO2 prepared with P123 exhibited 117 F .g-1at 5 mV/s. The results of crystalline MnO2 composites will also be presented. The authors acknowledge the support from the Richard J. Barber Foundation for Interdisciplinary Research.

Electrochemistry at Nanometer-Scaled Electrodes

ERIC Educational Resources Information Center

Watkins, John J.; Bo Zhang; White, Henry S.

2005-01-01

Electrochemical studies using nanometer-scaled electrodes are leading to better insights into electrochemical kinetics, interfacial structure, and chemical analysis. Various methods of preparing electrodes of nanometer dimensions are discussed and a few examples of their behavior and applications in relatively simple electrochemical experiments…

Microwave-assisted synthesis and electrochemical evaluation of VO 2 (B) nanostructures

DOE PAGES

Ashton, Thomas E.; Borras, David Hevia; Iadecola, Antonella; ...

2015-12-01

Understanding how intercalation materials change during electrochemical operation is paramount to optimising their behaviour and function and in situ characterisation methods allow us to observe these changes without sample destruction. Here, we first report the improved intercalation properties of bronze phase vanadium dioxide VO2 (B) prepared by a microwave assisted route which exhibits a larger electrochemical capacity (232 mAh g -1) compared to VO 2 (B) prepared by a solvothermal route (197 mAh g -1). These electrochemical differences have also been followed using in situ X-ray absorption spectroscopy allowing us to follow oxidation state changes as they occur during batterymore » operation.« less

Use of Nanostructures in Fabrication of Large Scale Electrochemical Film

NASA Astrophysics Data System (ADS)

Chen, Chien Chon; Chen, Shih Hsun; Shyu, Sheang Wen; Hsieh, Sheng Jen

Control of electrochemical parameters when preparing small-scale samples for academic research is not difficult. In mass production environments, however, maintenance of constant current density and temperature become a critical issue. This article describes the design of several molds for large work pieces. These molds were designed to maintain constant current density and to facilitate the occurrence of electrochemical reactions in designated areas. Large-area thin films with fine nanostructure were successfully prepared using the designed electrochemical molds and containers. In addition, current density and temperature could be controlled well. This electrochemical system has been verified in many experimental operations, including etching of Al surfaces; electro-polishing of Al, Ti and stainless steel; and fabrication of anodic alumina oxide (AAO), Ti-TiO2 interference membrane, TiO2 nanotubes, AAO-TiO2 nanotubes, Ni nanowires and porous tungsten

Influence of solution viscosity on hydrothermally grown ZnO thin films for DSSC applications

NASA Astrophysics Data System (ADS)

Marimuthu, T.; Anandhan, N.; Thangamuthu, R.; Surya, S.

2016-10-01

Zinc oxide (ZnO) nanowire arrays (NWAs) were grown onto zinc oxide-titanium dioxide (ZnO-TiO2) seeded fluorine doped tin oxide (FTO) conductive substrate by hydrothermal technique. X-ray diffraction (XRD) patterns depict that ZnO thin films are preferentially oriented along the (002) plane with hexagonal wurtzite structure. Viscosity measurements reveal that viscosity of the solutions linearly increases as the concentrations of the polyvinyl alcohol (PVA) increase in the growth solution. Field emission scanning electron microscope (FE-SEM) images show that the NWAs are vertically grown to seeded FTO substrate with hexagonal structure, and the growth of NWAs decreases as the concentration of the PVA increases. Stylus profilometer and atomic force microscopic (AFM) studies predict that the thickness and roughness of the films decrease with increasing the PVA concentrations. The NWAs prepared at 0.1% of PVA exhibits a lower transmittance and higher absorbance than that of the other films. The band gap of the optimized films prepared at 0.0 and 0.1% of PVA is found to be 3.270 and 3.268 eV, respectively. The photo to current conversion efficiency of the DSSC based on photoanodes prepared at 0.0 and 0.1% of PVA exhibits about 0.64 and 0.82%, respectively. Electrochemical impedance spectra reveal that the DSSC based on photoanode prepared at 0.1% of PVA has the highest charge transfer recombination resistance.

Rough gold films as broadband absorbers for plasmonic enhancement of TiO2 photocurrent over 400–800 nm

PubMed Central

Tan, Furui; Li, Tenghao; Wang, Ning; Lai, Sin Ki; Tsoi, Chi Chung; Yu, Weixing; Zhang, Xuming

2016-01-01

Recent years have witnessed an increasing interest in highly-efficient absorbers of visible light for the conversion of solar energy into electrochemical energy. This study presents a TiO2-Au bilayer that consists of a rough Au film under a TiO2 film, which aims to enhance the photocurrent of TiO2 over the whole visible region and may be the first attempt to use rough Au films to sensitize TiO2. Experiments show that the bilayer structure gives the optimal optical and photoelectrochemical performance when the TiO2 layer is 30 nm thick and the Au film is 100 nm, measuring the absorption 80–90% over 400–800 nm and the photocurrent intensity of 15 μA·cm−2, much better than those of the TiO2-AuNP hybrid (i.e., Au nanoparticle covered by the TiO2 film) and the bare TiO2 film. The superior properties of the TiO2-Au bilayer can be attributed to the rough Au film as the plasmonic visible-light sensitizer and the photoactive TiO2 film as the electron accepter. As the Au film is fully covered by the TiO2 film, the TiO2-Au bilayer avoids the photocorrosion and leakage of Au materials and is expected to be stable for long-term operation, making it an excellent photoelectrode for the conversion of solar energy into electrochemical energy in the applications of water splitting, photocatalysis and photosynthesis. PMID:27608836

Effect of substrate surface treatment on electrochemically assisted photocatalytic activity of N-S co-doped TiO2 films

NASA Astrophysics Data System (ADS)

Parada-Gamboa, N. J.; Pedraza-Avella, J. A.; Meléndez, A. M.

2017-01-01

To investigate whether different metal surface treatments, performed on meshes of stainless steel 304 and titanium, affect the photocatalytic activity (PCA) of supported modified anodic TiO2 films, metallic substrates were coated with titanium isopropoxide sol-gel precursor modified with thiourea. Substrates were pretreated by some of the following techniques: a) sandblasting, b) pickling, c) hydroxylation and d) passivation. The as-prepared electrode materials were characterized by X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), and voltammetry in the dark and under light UVA irradiation. PCA of modified N-S-TiO2 electrodes was evaluated by electrochemically assisted photocatalytic degradation of methyl orange. The results of XPS revealed that N and S were incorporated into the lattice of TiO2. FESEM showed that surface roughness and thickness of films varies depending on surface treatment. Voltammetric and XPS characterization of N-S co-doped TiO2 films supported on stainless steel revealed that their surface contains alpha-Fe2O3/FeOOH. Accordingly, iron contamination of the films coming from stainless steel was detrimental to the degradation of methyl orange. Prior to sol-gel coating process, sandblasting followed by nitric acid passivation for stainless steel or hydrofluoric acid pickling process in the case of titanium improved the PCA of N-S co-doped TiO2 films.

Superhydrophobicity of electrospray-synthesized fluorinated silica layers.

PubMed

Kim, Eun-Kyeong; Lee, Chul-Sung; Kim, Sang Sub

2012-02-15

The preparation of superhydrophobic SiO(2) layers through a combination of a nanoscale surface roughness and a fluorination treatment is reported. Electrospraying SiO(2) precursor solutions that had been prepared by a sol-gel chemical route produced very rough SiO(2) layers. Subsequent fluorination treatment with a solution containing trichloro(1H,1H,2H,2H-perfluorooctyl)silane resulted in highly rough, fluorinated SiO(2) layers. The fluorinated rough SiO(2) layers exhibited excellent repellency toward various liquid droplets. In particular, water repellency of 168° was observed. On the bases of Cassie-Baxter and Young-Dupre equations, the surface fraction and the work of adhesion of the rough, fluorinated SiO(2) layers were respectively estimated. In light of the durability in water, ultraviolet resistance, and thermal stability, the superhydrophobic SiO(2) layers prepared in this work hold promise in a range of practical applications. Copyright © 2011 Elsevier Inc. All rights reserved.

Effect of an Electrochemically Oxidized ZnO Seed Layer on ZnO Nanorods Grown by using Electrodeposition

NASA Astrophysics Data System (ADS)

Jeon, Woosung; Leem, Jae-Young

2018-05-01

ZnO nanorods were prepared on a Si substrate with and without a ZnO seed layer formed by electro-oxidation to investigate the effect of the seed layer on their growth. The ZnO nanorods grown on the ZnO seed layer had top surfaces that were flat whereas those grown without it had rough top surfaces, as observed in field-emission scanning electron microscopy images. In the Xray diffraction analysis, all ZnO nanorods showed preferential orientation with the (002) plane. In the case of ZnO nanorods prepared with a ZnO seed layer, the residual stress decreased, and the full width at half maximum of the ZnO (002) plane peak decreased. The photoluminescence spectra show a strong and narrow near-band-edge emission peak and high near-band-edge emission to deep-level emission peak ratio for the ZnO nanorods prepared with the seed layer. With respect to the photoresponse properties, the ZnO nanorods grown with the ZnO seed layer showed higher responsivity and faster rise/decay curves than those grown without it. Thus, the ZnO seed layer formed by electro-oxidation improves the structural, optical, and photoresponse properties of the ZnO nanorods formed on it. This method could serve as a new route for improving the properties of optoelectronic devices.

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

NASA Astrophysics Data System (ADS)

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.

Construction and Characterization of a Chitosan-Immobilized-Enzyme and β-Cyclodextrin-Included-Ferrocene-Based Electrochemical Biosensor for H₂O₂ Detection.

PubMed

Dong, Wenbo; Wang, Kaiyin; Chen, Yu; Li, Weiping; Ye, Yanchun; Jin, Shaohua

2017-07-28

An electrochemical detection biosensor was prepared with the chitosan-immobilized-enzyme (CTS-CAT) and β-cyclodextrin-included-ferrocene (β-CD-FE) complex for the determination of H₂O₂. Ferrocene (FE) was included in β-cyclodextrin (β-CD) to increase its stability. The structure of the β-CD-FE was characterized. The inclusion amount, inclusion rate, and electrochemical properties of inclusion complexes were determined to optimize the reaction conditions for the inclusion. CTS-CAT was prepared by a step-by-step immobilization method, which overcame the disadvantages of the conventional preparation methods. The immobilization conditions were optimized to obtain the desired enzyme activity. CTS-CAT/β-CD-FE composite electrodes were prepared by compositing the CTS-CAT with the β-CD-FE complex on a glassy carbon electrode and used for the electrochemical detection of H₂O₂. It was found that the CTS-CAT could produce a strong reduction peak current in response to H₂O₂ and the β-CD-FE could amplify the current signal. The peak current exhibited a linear relationship with the H₂O₂ concentration in the range of 1.0 × 10 -7 -6.0 × 10 -3 mol/L. Our work provided a novel method for the construction of electrochemical biosensors with a fast response, good stability, high sensitivity, and a wide linear response range based on the composite of chitosan and cyclodextrin.

Studies of SERS efficiency of gold coated porous silicon formed on rough silicon backside

NASA Astrophysics Data System (ADS)

Dridi, H.; Haji, L.; Moadhen, A.

2017-12-01

Starting from a rough backside of silicon wafer, we have formed a porous layer by electrochemical anodization and then coated by a thin film of gold. The morphological characteristics of the porous silicon and in turn the metal film are governed by the anodization process and also by the starting surface. So, in order to investigate the Plasmonic aspect of such rough surface which combines roughness inherent to the porous nature and that due to rough starting surface, we have used a dye target molecule to study its SERS signal using a porous silicon layer obtained on the rough backside surface. The use of unusual backside of silicon wafer could be, beside the others, an interesting way to made SERS effective substrate thanks to reproducible rough porous gold on porous layer from this starting face. The morphological results correspond to the silicon rough surface as a function of the crystallographic orientation showed the presence of two different substrate structure. The optical reflectivity results obtained of gold deposited on oxidized porous silicon showed a dependence of its Localized Surface Plasmon band frequency of the deposit time. SERS results, obtained for a dye target molecule (Rhodamine 6G), show a higher intensities in the case of the 〈110〉 orientation, which characterized by the higher roughness surface. Voici "the most relevant and important aspects of our work".

Preparation of Al-Ti Master Alloy by Electrochemical Recovery of Titanium-Reducing Slag in Molten Salts

NASA Astrophysics Data System (ADS)

Zhao, Kun; Wang, Yaowu; Feng, Naixiang

2018-02-01

An electrochemical method for the preparation of an Al-Ti master alloy in Al electrolysis melts of Na3AlF6-Al2O3-LiF at 980°C was investigated. The Ti-reducing slag (5.24 wt.% Ti in the Ti-reducing slag) was obtained from the aluminothermic reduction of Na2TiF6. The cold test (i.e., the aluminothermic reduction process without applying any voltages) result revealed the capability of the Al cathode to reduce the Ti slag, and the recovery rate could reach 45.8% at 980°C over 3.5 h with the addition of 10 wt.% Ti-reducing slag. In contrast, the recovery rate of Ti after electrolysis at 3.0 V could reach 99.2%. Thus, the electrochemical treatment for Ti-reducing slag is a cooperative process involving aluminothermic and electrochemical reduction reactions. Electrochemical analysis indicated that the Ti ions are reduced to metallic Ti according to Ti4+ → Ti3+ → Ti. An Al-Ti alloy layer could be prepared on the external surface of the Mo electrode after electrolysis with the addition of 12 wt.% Ti-reducing slag.

Growth mechanism of surface roughed platinum nanowires through electrodeposition current control and their electrochemical applications

NASA Astrophysics Data System (ADS)

Ruan, Dajiang

The aim of this work is to investigate the effect of current density on the grain size and surface morphology of electrodeposited platinum nanowires and their applications. Platinum (Pt) nanowires were fabricated by a galvanostatic electrodeposition method in a porous anodic alumina oxide (AAO) template with different current densities. Both direct current and pulse current electrodeposition were used to synthesize the Pt nanowires. The grain size and surface morphology of the Pt nanowires were studied by field emission scanning electron microscopy (FE-SEM), transmission electron microcopy (TEM) and X-ray diffraction (XRD). The experimental results showed that the current density was the key factor to control the surface roughness. The surface of the Pt nanowires became rougher and the grain sizes were increased by increasing the current densities. From the experimental results, a growth mechanism of Pt nanowires based on progressive nucleation and crystallization was proposed in order to find out the relationship between the surface morphology and current density. The electrochemical properties and catalytic activities of these surface roughed Pt nanowires were investigated in the detection of H20 2 and for the methanol oxidation. Cyclic voltammograms of Pt nanowire modified electrodes were obtained using a potentiostat, which showed that rougher Pt nanowires have higher response and better activity than that of smooth nanowires. For H202 detection, the effect of scan rate and H202 concentration were studied and it was found that the peak current for hydrogen peroxide reduction became larger with the increasing of either scan rate or H202 concentration. It can be inferred that the process of electrocatalytic hydrogen peroxide reduction may be controlled by diffusion of hydrogen peroxide and the Pt nanowire modified glassy carbon electrode (GCE) is well suited for the detection of H202. From the relationship between the peak current and square root of scan rates for methanol oxidation, it can be inferred that the process of electrocatalytic methanol oxidation was controlled by diffusion of methanol. To understand the effect of the morphological feature on the electrocatalytic activity of the Pt nanowire catalysts, the electrochemically active surface area (ECSA) as a function of deposited current density was investigated, which suggests that Pt nanowire catalysts deposited at highest current density had the most ECSA surface morphology of the Pt nanowires. The chronoamperometric curves and electrochemical impedance spectroscopy (EIS) results confirmed that the Pt nanowire catalyst synthesized at higher current density possessed longer durability and gave more efficient electrochemical performance.

Preparation of RuO2-TiO2/Nano-graphite composite anode for electrochemical degradation of ceftriaxone sodium.

PubMed

Li, Dong; Guo, Xiaolei; Song, Haoran; Sun, Tianyi; Wan, Jiafeng

2018-06-05

Graphite-like material is widely used for preparing various electrodes for wastewater treatment. To enhance the electrochemical degradation efficiency of Nano-graphite (Nano-G) anode, RuO 2 -TiO 2 /Nano-G composite anode was prepared through the sol-gel method and hot-press technology. RuO 2 -TiO 2 /Nano-G composite was characterized by X-ray diffraction, X-ray photoelectron spectroscopy, transmission electron microscopy and N 2 adsorption-desorption. Results showed that RuO 2 , TiO 2 and Nano-G were composited successfully, and RuO 2 and TiO 2 nanoparticles were distributed uniformly on the surface of Nano-G sheet. Specific surface area of RuO 2 -TiO 2 /Nano-G composite was higher than that of TiO 2 /Nano-G composite and Nano-G. Electrochemical performances of RuO 2 -TiO 2 /Nano-G anode were investigated by cyclic voltammetry, electrochemical impedance spectroscopy. RuO 2 -TiO 2 /Nano-G anode was applied to electrochemical degradation of ceftriaxone. The generation of hydroxyl radical (OH) was measured. Results demonstrated that RuO 2 -TiO 2 /Nano-G anode displayed enhanced electrochemical degradation efficiency towards ceftriaxone and yield of OH, which is derived from the synergetic effect between RuO 2 , TiO 2 and Nano-G, which enhance the specific surface area, improve the electrochemical oxidation activity and lower the charge transfer resistance. Besides, the possible degradation intermediates and pathways of ceftriaxone sodium were identified. This study may provide a viable and promising prospect for RuO 2 -TiO 2 /Nano-G anode towards effective electrochemical degradation of antibiotics from wastewater. Copyright © 2018 Elsevier B.V. All rights reserved.

Facile synthesis of porous graphene as binder-free electrode for supercapacitor application

NASA Astrophysics Data System (ADS)

Luo, Guangsheng; Huang, Haifu; Lei, Chenglong; Cheng, Zhenzhi; Wu, Xiaoshan; Tang, Shaolong; Du, Youwei

2016-03-01

Here, porous grapheme oxide (GO) gel deposited on nickel foam was prepared by using polystyrene (PS) colloidal particles as spacers for use as electrodes in high rate supercapacitors, then reduced by Vitamin C aqueous solution in ambient condition. The PS particles were surrounded by reduced graphene oxide (rGO) sheets, forming crinkles and rough textures. When PS particles were selectively removed, rGO gel coated on the skeleton of Ni foam can formed an open porous structure, which prevents elf-aggregation and restacking of graphene sheets. The porous rGO-based supercapacitors exhibit excellent electrochemical performances such as a specific capacitance of 152 F g-1 at 1 A g-1, high rate capability of 53% capacitance retention upon a current increase to 100 A g-1 and good cycle stability, due to effective rapid and short pathways for ionic and electronic transport provided by the sub-micrometer structure of rGO gel and 3D interconnected network of Ni foam.

Effects of Voltage on Microstructure and Corrosion Resistance of Micro-arc Oxidation Ceramic Coatings Formed on KBM10 Magnesium Alloy

NASA Astrophysics Data System (ADS)

Lu, J. P.; Cao, G. P.; Quan, G. F.; Wang, C.; Zhuang, J. J.; Song, R. G.

2018-01-01

Micro-arc oxidation (MAO) coatings on KBM10 magnesium alloy were prepared in an electrolyte system with sodium silicate, potassium hydroxide, sodium tungstate, and citric acid. The effects of voltage on the microstructure and corrosion resistance of MAO coatings were studied using stereoscopic microscopy, scanning electron microscopy, x-ray diffraction, scratch tests, potentiodynamic polarization, and electrochemical impedance spectroscopy. The results showed that the roughness of the MAO coatings, diameter, and number of pores increase with the increase in voltage. The coating formed at the voltage of 350 V exhibited the best adhesive strength when evaluated by the automatic scratch tester. The coatings were mainly composed of MgO, MgWO4, and Mg2SiO4, and the content of Mg2SiO4 increased with the increase in voltage. The corrosion resistance of MAO coatings could be improved by changing the applied voltage, and the best corrosion resistance of MAO coating was observed at the voltage of 350 V.

Electrochemical investigations of Cr-Ni-Mo stainless steel used in urology

NASA Astrophysics Data System (ADS)

Przondziono, J.; Walke, W.

2011-05-01

The influence of chemical passivation process on physical and chemical characteristics of samples made of X2CrNiMo 17-7-2 steel with differentiated hardening, in the solution simulating the environment of human urine was analysed in the study. Wire obtained in cold drawing process is used for the production of stents and appliances in urological treatment. Proper roughness of the surface was obtained through mechanical working - grinding (Ra = 0,40 μn) and electrochemical polishing (Ra = 0,12 μn). Chemical passivation process was carried out in 40% solution of HN03 within 60 minutes in the temperature of 65°C. The tests of corrosion resistance were made on the ground of registered anodic polarisation curves and Stern method. For evaluation of phenomena occurring on the surface of tested steel, electrochemical impedance spectroscopy (EIS) was applied.

Preparation and characterizations of activated carbon monolith from rubber wood and its effect on supercapacitor performances

NASA Astrophysics Data System (ADS)

Taer, E.; Taslim, R.; Deraman, M.

2016-02-01

Preparation of activated carbon monolith (ACM) from rubber wood was investigated. Two kind of preparation method were carried out by pre-carbonized of rubber wood saw dust and rubber wood material as it is naturally. The samples were prepared with pelletizing method and small cutting of rubber wood in cross sectional method. Both of samples were characterized by physical and electrochemical technique. The physical properties such as morphology and porosity were investigated. The electrochemical properties of both samples such as equivalent series resistances (ESR) and specific capacitances were also compared. In conclusion, this study showed that both of different preparation method would propose a simple method of ACM electrode preparation technique for supercapacitor applications.

Improvement of the process for electrochemical impregnation of nickel hydroxide electrodes

NASA Technical Reports Server (NTRS)

Comtat, M.; Lafage, B.; Leonardi, J.

1986-01-01

Nickel hydroxide electrodes containing 11g/dsqm hydroxide, with capacities of 3.6 to 3.8 Ah/dsqm were prepared at 353 K by electrochemical impregnation. The reproducibility of the results is obtained by readjusting the pH before each preparation. The control of each electrode is done during two cycles of charge and discharge following the manufacture by a potential relaxation method.

Effect of the synthesis conditions on the electrochemical properties of LiFePO{sub 4} obtained from NH{sub 4}FePO{sub 4}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Prosini, Pier Paolo, E-mail: pierpaolo.prosini@enea.it; Gislon, Paola; Cento, Cinzia

Graphical abstract: - Highlights: • Four different samples of FAP were synthesized by precipitation techniques. • The samples were used as precursors to synthesize electrochemical active LiFePO{sub 4}. • Their morphology, composition, structure and electrochemical performance were studied. • The LiFePO{sub 4} electrochemical performance resulted affected by the preparation method - Abstract: In this paper the morphological, structural and electrochemical properties of crystalline lithium iron phosphate (LiFePO{sub 4}) obtained from ferrous ammonium phosphate (FAP) have been studied. The FAP was obtained following four different processes, namely: (1) homogeneous phase precipitation, (2) heterogeneous phase precipitation from stoichiometric sodium phosphate, (3) heterogeneousmore » phase precipitation from stoichiometric ammonium phosphate, and (4) heterogeneous phase precipitation from over stoichiometric ammonium phosphate. Lithium iron phosphate was prepared by solid state reaction of FAP with lithium hydroxide. In order to evaluate the effect of reaction time and synthesis temperature the LiFePO{sub 4} was prepared varying the heating temperatures (550, 600 and 700 °C) and the reaction times (1 or 2 h). The morphology of the materials was evaluated by scanning electron microscopy while the chemical composition was determined by electron energy loss spectroscopy. X-ray diffraction was used to evaluate phase composition, crystal structure and crystallite size. The so obtained LiFePO{sub 4}'s were fully electrochemical characterized and a correlation was found between the crystal size and the electrochemical performance.« less

The electrochemical reduction processes of solid compounds in high temperature molten salts.

PubMed

Xiao, Wei; Wang, Dihua

2014-05-21

Solid electrode processes fall in the central focus of electrochemistry due to their broad-based applications in electrochemical energy storage/conversion devices, sensors and electrochemical preparation. The electrolytic production of metals, alloys, semiconductors and oxides via the electrochemical reduction of solid compounds (especially solid oxides) in high temperature molten salts has been well demonstrated to be an effective and environmentally friendly process for refractory metal extraction, functional materials preparation as well as spent fuel reprocessing. The (electro)chemical reduction of solid compounds under cathodic polarizations generally accompanies a variety of changes at the cathode/melt electrochemical interface which result in diverse electrolytic products with different compositions, morphologies and microstructures. This report summarizes various (electro)chemical reactions taking place at the compound cathode/melt interface during the electrochemical reduction of solid compounds in molten salts, which mainly include: (1) the direct electro-deoxidation of solid oxides; (2) the deposition of the active metal together with the electrochemical reduction of solid oxides; (3) the electro-inclusion of cations from molten salts; (4) the dissolution-electrodeposition process, and (5) the electron hopping process and carbon deposition with the utilization of carbon-based anodes. The implications of the forenamed cathodic reactions on the energy efficiency, chemical compositions and microstructures of the electrolytic products are also discussed. We hope that a comprehensive understanding of the cathodic processes during the electrochemical reduction of solid compounds in molten salts could form a basis for developing a clean, energy efficient and affordable production process for advanced/engineering materials.

Influence of oscillating and rotary cutting instruments with electric and turbine handpieces on tooth preparation surfaces.

PubMed

Geminiani, Alessandro; Abdel-Azim, Tamer; Ercoli, Carlo; Feng, Changyong; Meirelles, Luiz; Massironi, Domenico

2014-07-01

Rotary and nonrotary cutting instruments are used to produce specific characteristics on the axial and marginal surfaces of teeth being prepared for fixed restorations. Oscillating instruments have been suggested for tooth preparation, but no comparative surface roughness data are available. To compare the surface roughness of simulated tooth preparations produced by oscillating instruments versus rotary cutting instruments with turbine and electric handpieces. Different grit rotary cutting instruments were used to prepare Macor specimens (n=36) with 2 handpieces. The surface roughness obtained with rotary cutting instruments was compared with that produced by oscillating cutting instruments. The instruments used were as follows: coarse, then fine-grit rotary cutting instruments with a turbine (group CFT) or an electric handpiece (group CFE); coarse, then medium-grit rotary cutting instruments with a turbine (group CMT) or an electric handpiece (group CME); coarse-grit rotary cutting instruments with a turbine handpiece and oscillating instruments at a low-power (group CSL) or high-power setting (group CSH). A custom testing apparatus was used to test all instruments. The average roughness was measured for each specimen with a 3-dimensional optical surface profiler and compared with 1-way ANOVA and the Tukey honestly significant difference post hoc test for multiple comparisons (α=.05). Oscillating cutting instruments produced surface roughness values similar to those produced by similar grit rotary cutting instruments with a turbine handpiece. The electric handpiece produced smoother surfaces than the turbine regardless of rotary cutting instrument grit. Rotary cutting instruments with electric handpieces produced the smoothest surface, whereas the same instruments used with a turbine and oscillating instruments achieved similar surface roughness. Copyright © 2014 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Construction and Characterization of a Chitosan-Immobilized-Enzyme and β-Cyclodextrin-Included-Ferrocene-Based Electrochemical Biosensor for H2O2 Detection

PubMed Central

Dong, Wenbo; Wang, Kaiyin; Chen, Yu; Li, Weiping; Ye, Yanchun; Jin, Shaohua

2017-01-01

An electrochemical detection biosensor was prepared with the chitosan-immobilized-enzyme (CTS-CAT) and β-cyclodextrin-included-ferrocene (β-CD-FE) complex for the determination of H2O2. Ferrocene (FE) was included in β-cyclodextrin (β-CD) to increase its stability. The structure of the β-CD-FE was characterized. The inclusion amount, inclusion rate, and electrochemical properties of inclusion complexes were determined to optimize the reaction conditions for the inclusion. CTS-CAT was prepared by a step-by-step immobilization method, which overcame the disadvantages of the conventional preparation methods. The immobilization conditions were optimized to obtain the desired enzyme activity. CTS-CAT/β-CD-FE composite electrodes were prepared by compositing the CTS-CAT with the β-CD-FE complex on a glassy carbon electrode and used for the electrochemical detection of H2O2. It was found that the CTS-CAT could produce a strong reduction peak current in response to H2O2 and the β-CD-FE could amplify the current signal. The peak current exhibited a linear relationship with the H2O2 concentration in the range of 1.0 × 10−7–6.0 × 10−3 mol/L. Our work provided a novel method for the construction of electrochemical biosensors with a fast response, good stability, high sensitivity, and a wide linear response range based on the composite of chitosan and cyclodextrin. PMID:28773229

Electrochemical properties of monolithic nickel sulfide electrodes for use in sodium batteries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Go, Dae-Yeon; Park, Jinsoo, E-mail: jsp@ikw.ac.kr; Noh, Pan-Jin

2014-10-15

Highlights: • We succeeded in preparing monolithic Ni{sub 3}S{sub 2} integrated electrode through the sulfuration. • The sulfuration is a facile and useful method to synthesize metal sulfides with nanostructure. • As-prepared monolithic Ni{sub 3}S{sub 2} electrodes showed very stable and cycle performance over charge/discharge cycling. - Abstract: Monolithic nickel sulfide electrodes were prepared using a facile synthesis method, sulfuration and annealing. As-prepared Ni{sub 3}S{sub 2} electrodes were characterized by X-ray diffractometry and field emission scanning electron microscopy. Thermal stability was determined by thermal gravimetric analysis and differential scanning calorimetry. Electrochemical properties were measured by galvanostatic charge and discharge cyclingmore » for Na-ion batteries. Three kinds of Ni{sub 3}S{sub 2} electrodes were prepared by varying the sulfuration time (5, 15 and 25 min). The electrochemical results indicated that the capacities increased with an increase in sulfuration time and the cycle performance was stable as a result of monolithic integration of nanostructured Ni{sub 3}S{sub 2} on Ni plates, leading to low interfacial resistance.« less

Gold-carbon composite thin films for electrochemical gas sensor prepared by reactive plasma sputtering

NASA Astrophysics Data System (ADS)

Okamoto, A.; Suzuki, Y.; Yoshitake, M.; Ogawa, S.; Nakano, N.

1997-01-01

We have investigated the properties of gold-carbon composite thin films prepared by a plasma sputtering deposition using argon and methane mixture gas. These composite films have an uneven surface in submicron scale or consist of nano-scale particles of gold polycrystalline. Such morphological properties can be controlled by the sputtering voltage and the partial pressure of methane gas. The working electrode of electrochemical gas sensor has needed a stable gas sensitivity and a good gas selectivity. Our composite film is one of the excellent candidates for a thin film working electrode of electrochemical gas sensor. It is described that the output current of sensor is related to the preparation conditions of the thin films and increase linearly as the concentration of PH 3 gas ranging from 0.1 to 1.0 ppm is increasing.

Fast preparation of ultrafine monolayered transition-metal dichalcogenide quantum dots using electrochemical shock for explosive detection.

PubMed

Chen, Zhigang; Tao, Zhengxu; Cong, Shan; Hou, Junyu; Zhang, Dengsong; Geng, Fengxia; Zhao, Zhigang

2016-09-15

A simple, general and fast method called "electrochemical shock" is developed to prepare monolayered transition-metal dichalcogenide (TMD) QDs with an average size of 2-4 nm and an average thickness of 0.85 ± 0.5 nm with only about 10 min of ultrasonication. Just like nails hammered into a plate, the electrochemical shock with Al 3+ ions and the following extraction with the help of oleic acid can disintegrate bulk TMD crystals into ultrafine TMD QDs. The fast-prepared QDs are then applied to detect highly explosive molecules such as 2,4,6-trinitrophenol (TNP) with a low detection limit of 10 -6 M. Our versatile method could be broadly applicable for the fast production of ultrathin QDs of other materials with great promise for various applications.

Preparation of Ti/IrO2 Anode with Low Iridium Content by Thermal Decomposition Process: Electrochemical removal of organic pollutants in water

NASA Astrophysics Data System (ADS)

Yaqub, Asim; Isa, Mohamed Hasnain; Ajab, Huma; Kutty, S. R. M.; Ezechi, Ezerie H.; Farooq, Robina

2018-04-01

In this study IrO2 (Iridium oxide) was coated onto a titanium plate anode from a dilute (50 mg/10 ml) IrCl3×H2O salt solution. Coating was done at high temperature (550∘C) using thermal decomposition. Surface morphology and characteristics of coated surface of Ti/IrO2 anode were examined by FESEM and XRD. The coated anode was applied for electrochemical removal of organic pollutants from synthetic water samples in 100 mL compartment of batch electrochemical cell. About 50% COD removal was obtained at anode prepared with low Ir content solution while 72% COD removal was obtained with anode prepared at high Ir content. Maximum COD removal was obtained at 10 mA/cm2 current density.

Preparation and electrochemical characteristics of porous hollow spheres of NiO nanosheets as electrodes of supercapacitors

NASA Astrophysics Data System (ADS)

Yu, Wei; Jiang, Xinbing; Ding, Shujiang; Li, Ben Q.

2014-06-01

Porous hollow nanospheres (or spherical shells) made of NiO nanosheets are synthesized and tested for the electrochemical performance of the electrodes made of these materials for supercapacitors. Preparation of the NiO sheet hollow spheres starts with synthesis of polystyrene nanospheres with carboxyl groups (CPS), followed by a two-step activation procedure and the subsequent nucleation and growth by electroless deposition of Ni on the CPS core to obtain CPS@Ni core-shell nanoparticles. The CPS core is eliminated and metallic Ni nanoshell is converted into NiO by calcinations at high temperatures. The material properties of as-prepared hollow NiO nanospheres are characterized by TEM, XRD and N2-absorption measurements. The electrochemical characteristics of the electrodes made of these nanostructured NiO materials are determined by the CV and galvanostatic measurements. These electrochemical tests indicate that electrodes made of the NiO nanosheet hollow spheres exhibit an improved reversible capacitance of 600 F g-1 after 1000 cycles at a high current density of 10 A g-1. It is believed that the good electrochemical performance of these electrodes is attributed to the improved OH- transport in the porous network structures associated with the hollow spheres of randomly oriented NiO nanosheets.

Nano-sized Ni-doped carbon aerogel for supercapacitor.

PubMed

Lee, Yoon Jae; Jung, Ji Chul; Park, Sunyoung; Seo, Jeong Gil; Baeck, Sung-Hyeon; Yoon, Jung Rag; Yi, Jongheop; Song, In Kyu

2011-07-01

Carbon aerogel was prepared by polycondensation of resorcinol with formaldehyde using sodium carbonate as a catalyst in ambient conditions. Nano-sized Ni-doped carbon aerogel was then prepared by a precipitation method in an ethanol solvent. In order to elucidate the effect of nickel content on electrochemical properties, Ni-doped carbon aerogels (21, 35, 60, and 82 wt%) were prepared and their performance for supercapacitor electrode was investigated. Electrochemical properties of Ni-doped carbon aerogel electrodes were measured by cyclic voltammetry at a scan rate of 10 mV/sec and charge/discharge test at constant current of 1 A/g in 6 M KOH electrolyte. Among the samples prepared, 35 wt% Ni-doped carbon aerogel (Ni/CA-35) showed the highest capacitance (110 F/g) and excellent charge/discharge behavior. The enhanced capacitance of Ni-doped carbon aerogel was attributed to the faradaic redox reactions of nano-sized nickel oxide. Moreover, Ni-doped carbon aerogel exhibited quite stable cyclability, indicating long-term electrochemical stability.

Surfactant-assisted electrochemical deposition of α-cobalt hydroxide for supercapacitors

NASA Astrophysics Data System (ADS)

Zhao, Ting; Jiang, Hao; Ma, Jan

A N-methylpyrrolidone (NMP) assisted electrochemical deposition route has been developed to realize the synthesis of a dense α-Co(OH) 2 layered structure, which is composed of nanosheets, each with a thickness of 10 nm. The capacitive characteristics of the as-obtained α-Co(OH) 2 are investigated by means of cyclic voltammetry (CV), charge/discharge characterization, and electrochemical impedance spectroscopy (EIS), in 1 M KOH electrolyte. The results indicate that α-Co(OH) 2 prepared in the presence of 20 vol.% NMP has denser and thin layered structure which promotes an increased surface area and a shortened ion diffusion path. The as-prepared α-Co(OH) 2 shows better electrochemical performance with specific capacitance of 651 F g -1 in a potential range of -0.1 to 0.45 V. These findings suggest that the surfactant-assisted electrochemical deposition is a promising process for building densely packed material systems with enhanced properties, for application in supercapacitors.

Phytic acid/graphene oxide nanocomposites modified electrode for electrochemical sensing of dopamine.

PubMed

Wang, Donglei; Xu, Fei; Hu, Jiajie; Lin, Meng

2017-02-01

An electrochemical sensor for determining dopamine was developed by modifying phytic acid/graphene oxide (PA/GO) nanocomposites onto a glassy carbon electrode (GCE). PA functionalized GO was prepared by an ultra-sonication method. Subsequently, the PA/GO nanocomposites were drop-casted on a glassy carbon substrate. The structural feature of the PA/GO modified GCE was confirmed by attenuated total reflection infrared (ATR-IR) spectroscopy. The proposed electrochemical sensor was applied to detect various concentrations of DA by differential pulse voltammetry (DPV). The PA/GO/GCE was considered to be highly sensitive to DA in the range of 0.05-10μM. In addition, the PA/GO/GCE demonstrated high electrochemical selectivity toward DA in the presence of ascorbic acid (AA) and uric acid (UA). The prepared electrochemical DA sensor was applied for detection of DA in dopamine hydrochloride injection and spiked samples of human urine with satisfactory results. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis and electrochemical properties of layered structure Li[Ni{sub 0.5}Co{sub 0.25}Mn{sub 0.25}]O{sub 2} cathode material

DOE Office of Scientific and Technical Information (OSTI.GOV)

Prathibha, G.; Rosaiah, P.; Reddy, B. Purusottam

Lithium ion (Li-ion) batteries are currently the energy source of choice for cell phones, laptops, and other mobile electronic devices due to their balance of high energy density with high power density compared to other electrochemical energy carriers. In the present study, mixed hydroxide method is used to prepare Li[Ni{sub 0.5}Co{sub 0.25}Mn{sub 0.25}]O{sub 2} from the precursors and analyze qualitatively and studied the electrochemical properties. The XRD spectrum exhibited predominant (003) orientation at 2θ =18.39{sup o} corresponding to hexagonal layered structure of R3m symmetry with evaluated lattice parameters are a= 2.84 Å, c= 14.43 Å. Raman measurements were performed tomore » understand the microstructure and vibrational modes of the prepared sample. From the electrochemical (EC) studies an initial discharge capacity of about 140 mAhg{sup −1} with good cyclic stability was observed for the prepared sample in the potential range 0.0 −1.0V in aqueous medium.« less

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

NASA Astrophysics Data System (ADS)

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 2O-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 2O-PIII NiTi samples in simulated body fluids (SBF) at 37 °C as well as the mechanism. The H 2O-PIII NiTi sample showed a higher breakdown potential ( Eb) 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 2O-PIII is primarily responsible for the improvement in the surface corrosion resistance.

Hierarchical structured Sm2O3 modified CuO nanoflowers as electrode materials for high performance supercapacitors

NASA Astrophysics Data System (ADS)

Zhang, Xiaojuan; He, Mingqian; He, Ping; Liu, Hongtao; Bai, Hongmei; Chen, Jingchao; He, Shaoying; Zhang, Xingquan; Dong, Faqing; Chen, Yang

2017-12-01

By a simple and cost effective chemical precipitation-hydrothermal method, novel hierarchical structured Sm2O3 modified CuO nanoflowers are prepared and investigated as electrode materials for supercapacitors. The physical properties of prepared materials are characterized by XRD, FE-SEM, EDX and FTIR techniques. Furthermore, electrochemical performances of prepared materials are investigated by cyclic voltammetry, galvanostatic charge/discharge and electrochemical impedance spectrum in 1.0 M KOH electrolyte. The resulting Sm2O3 modified CuO based electrodes exhibit obviously enhanced capacitive properties owing to the unique nanostructures and strong synergistic effects. It is worth noting that the optimized SC-3 based electrode exhibits the best electrochemical performances in all prepared electrodes, including higher specific capacitance (383.4 F g-1 at 0.5 A g-1) and good rate capability (393.2 F g-1 and 246.3 F g-1 at 0.3 A g-1 and 3.0 A g-1, respectively), as well as excellent cycling stability (84.6% capacitance retention after 2000 cycles at 1.0 A g-1). The present results show that Sm2O3 is used as a promising modifier to change the morphology and improve electrochemical performances of CuO materials.

Molecular and electronic structure of thin films of protoporphyrin(IX)Fe(III)Cl

NASA Astrophysics Data System (ADS)

Snyder, Shelly R.; White, Henry S.

1991-11-01

Electrochemical, scanning tunneling microscopy (STM), and tunneling spectroscopy studies of the molecular and electronic properties of thin films of protoporphyrin(IX)Fe(III)Cl (abbreviated as PP(IX)Fe(III)Cl) on highly oriented pyrolytic graphite (HOPG) electrodes are reported. PP(IX)Fe(III)Cl films are prepared by two different methods: (1) adsorption, yielding an electrochemically-active film, and (2) irreversible electrooxidative polymerization, yielding an electrochemically-inactive film. STM images, in conjunction with electro-chemical results, indicate that adsorption of PP(IX)Fe(III)Cl from aqueous solutions onto freshly cleaved HOPG results in a film comprised of molecular aggregates. In contrast, films prepared by irreversible electrooxidative polymerization of PP(IX)Fe(III)Cl have a denser, highly structured morphology, including what appear to be small pinholes (approx. 50A diameter) in an otherwise continuous film.

Electrocatalytic Transformation of Carbon Dioxide into Low Carbon Compounds on Conducting Polymers Derived from Multimetallic Porphyrins.

PubMed

Dreyse, Paulina; Honores, Jessica; Quezada, Diego; Isaacs, Mauricio

2015-11-01

The electrochemical reduction of carbon dioxide is studied herein by using conducting polymers based on metallotetraruthenated porphyrins (MTRPs). The polymers on glassy carbon electrodes were obtained by electropolymerization processes of the monomeric MTRP. The linear sweep voltammetry technique resulted in polymeric films that showed electrocatalytic activity toward carbon dioxide reduction with an onset potential of -0.70 V. The reduction products obtained were hydrogen, formic acid, formaldehyde, and methanol, with a tendency for a high production of methanol with a maximum value of turnover frequency equal to 15.07 when using a zinc(II) polymeric surface. Studies of the morphology (AFM) and electrochemical impedance spectroscopy results provide an adequate background to explain that the electrochemical reduction is governed by the roughness of the polymer, for which the possible mechanism involves a series of one-electron reduction reactions. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Thin calcium phosphate coatings on titanium by electrochemical deposition in modified simulated body fluid.

PubMed

Peng, Ping; Kumar, Sunil; Voelcker, Nicolas H; Szili, Endre; Smart, Roger St C; Griesser, Hans J

2006-02-01

Adherent and optically semitransparent thin calcium phosphate (CaP) films were electrochemically deposited on titanium substrates in a modified simulated body fluid at 37 degrees C. Coatings deposited by using periodic pulsed potentials showed better adhesion and better mechanical properties than coatings deposited with use of a constant potential. Scanning electron microscopy was used to study the morphology of the coatings. The coatings displayed a polydispersed porous structure with pores in the range of a few nanometers to 1 mum. Furthermore, X-ray diffractometry and the O(1s) satellite peaks in X-ray photoelectron spectroscopy indicated that the coatings possessed a similar surface chemistry to that of natural bone minerals. These results were confirmed by inductively coupled plasma optical emission spectrometry, which yielded a Ca:P ratio of 1.65, close to that of hydroxyapatite. Contact mode atomic force microscopy (AFM) showed the average thickness of the coatings was in the order of 200 nm. Root-mean-square (RMS) roughness values, also derived by AFM, were shown to be much higher on the titanium-CaP surfaces in comparison with untreated titanium substrates, with RMS values of about 300 and 110 nm, respectively. Cell culture experiments showed that the CaP surfaces are nontoxic to MG63 osteoblastic cells in vitro and were able to support cell growth for up to 4 days, outperforming the untreated titanium surface in a direct comparison. These easily prepared coatings show promise for hard-tissue biomaterials. (c) 2005 Wiley Periodicals, Inc.

Evaluation of pulsed laser deposited SrNb0.1Co0.9O3-δ thin films as promising cathodes for intermediate-temperature solid oxide fuel cells

NASA Astrophysics Data System (ADS)

Chen, Dengjie; Chen, Chi; Gao, Yang; Zhang, Zhenbao; Shao, Zongping; Ciucci, Francesco

2015-11-01

SrNb0.1Co0.9O3-δ (SNC) thin films prepared on single-crystal yttria-stabilized zirconia (YSZ) electrolytes are evaluated as promising cathodes for intermediate-temperature solid oxide fuel cells (IT-SOFCs). Geometrically well-defined polycrystalline SNC thin films with low surface roughness and high surface oxygen vacancy concentration are successfully fabricated by pulsed laser deposition. The thin films are characterized by basic techniques, e.g., X-ray diffraction for phase structure identification, scanning electron microscopy and atomic force microscopy for microstructures measurement, and X-ray photoelectron spectroscopy for elements quantification. Electrochemical impedance spectroscopy (EIS) is used to investigate oxygen reduction reaction activities of SNC thin films in symmetric electrochemical cells. Current collectors (Ag paste, Ag strip, and Au strip) are found to have negligible impact on polarization resistances. A slight decrease of the electrode polarization resistances is observed after adding a samarium doped ceria (SDC) buffer layer between SNC and YSZ. SNC thin-film electrodes exhibit low electrode polarization resistances, e.g., 0.237 Ω cm2 (SNC/SDC/YSZ/SDC/SNC) and 0.274 Ω cm2 (SNC/YSZ/SNC) at 700 °C and 0.21 atm, demonstrating the promise of SNC materials for IT-SOFCs. An oxygen reduction reaction mechanism of SNC thin films is also derived by analyzing EIS at temperature of 550-700 °C under oxygen partial pressure range of 0.04-1 atm.

Pulse-reverse electrodeposition for mesoporous metal films: combination of hydrogen evolution assisted deposition and electrochemical dealloying.

PubMed

Cherevko, Serhiy; Kulyk, Nadiia; Chung, Chan-Hwa

2012-01-21

Hydrogen evolution assisted electrodeposition is a new bottom-up technique allowing the fast and simple synthesis of nanometals. Electrochemical dealloying is a top-down approach with the same purpose. In this work, we show that a combination of these two methods in sequence by pulse-reverse electrodeposition can be used to prepare high-surface-area nanostructured metals. Highly porous adherent platinum is obtained by the deposition of CuPt alloy during the cathodic cycles and the selective dissolution of copper during the anodic cycles. The convection created by the movement of the hydrogen bubbles increases the deposition rate and removes the dissolved copper ions from the diffusion layer, which ensures the deposition of a film with the same stoichiometry throughout the whole process. Due to the relatively high ratio of copper atoms on the surface in the as-deposited layer, it is proposed that the dealloying kinetics is significantly higher than that usually observed during the dealloying process in a model system. The proposed approach has several advantages over other methods, such as a very high growth rate and needlessness of any post-treatment processes. A detailed analysis of the effect of pulse-reverse waveform parameters on the properties of the films is presented. Mesoporous platinum with pores and ligaments having characteristic sizes of less than 10 nm, an equivalent surface area of up to ca. 220 m(2) cm(-3), and a roughness factor of more than 1000 is fabricated.

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

PubMed

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

2017-09-13

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kim, Eun-Kyeong; Yeong Kim, Ji; Sub Kim, Sang, E-mail: sangsub@inha.ac.kr

We describe the preparation of superhydrophobic SiO{sub 2} layers through a combination of surface roughness and fluorination. Electrospraying SiO{sub 2} precursor solutions that were prepared by a sol-gel route and included trichloro(1H,1H,2H,2H-perfluorooctyl)silane as a fluorination source produced highly rough, fluorinated SiO{sub 2} layers. In sharp contrast to the fluorinated flat SiO{sub 2} layer, the fluorinated rough SiO{sub 2} layer showed much enhanced repellency toward liquid droplets of different surface tensions. The surface fraction and the work of adhesion of the superhydrophobic SiO{sub 2} layers were determined, respectively, based on Cassie-Baxter and Young-Dupre equations. The satisfactory long-term stability for 30 days,more » the ultraviolet resistance and the thermal stability up to 400 {sup o}C of the superhydrophobic SiO{sub 2} layers prepared in this work confirm a promising practical application. - Graphical abstract: A schematic illustration of the electrospray deposition used for preparing SiO{sub 2} layers. Shapes of liquid droplets of water, glycerol, coffee, juice and milk created on the fluorinated rough SiO{sub 2} layer deposited on a silicon wafer. Highlights: Black-Right-Pointing-Pointer Superhydrophobic SiO{sub 2} layers are realized by a combination of surface roughness and fluorination. Black-Right-Pointing-Pointer The fluorinated rough SiO{sub 2} layer shows enhanced repellency toward various liquid droplets. Black-Right-Pointing-Pointer The wetting behavior is explained based on Cassie-Baxter and Young-Dupre equations. Black-Right-Pointing-Pointer The superhydrophobic SiO{sub 2} layers confirm a promising practical application.« less

Preparation of Graphene Sheets by Electrochemical Exfoliation of Graphite in Confined Space and Their Application in Transparent Conductive Films.

PubMed

Wang, Hui; Wei, Can; Zhu, Kaiyi; Zhang, Yu; Gong, Chunhong; Guo, Jianhui; Zhang, Jiwei; Yu, Laigui; Zhang, Jingwei

2017-10-04

A novel electrochemical exfoliation mode was established to prepare graphene sheets efficiently with potential applications in transparent conductive films. The graphite electrode was coated with paraffin to keep the electrochemical exfoliation in confined space in the presence of concentrated sodium hydroxide as the electrolyte, yielding ∼100% low-defect (the D band to G band intensity ratio, I D /I G = 0.26) graphene sheets. Furthermore, ozone was first detected with ozone test strips, and the effect of ozone on the exfoliation of graphite foil and the microstructure of the as-prepared graphene sheets was investigated. Findings indicate that upon applying a low voltage (3 V) on the graphite foil partially coated with paraffin wax that the coating can prevent the insufficiently intercalated graphite sheets from prematurely peeling off from the graphite electrode thereby affording few-layer (<5 layers) holey graphene sheets in a yield of as much as 60%. Besides, the ozone generated during the electrochemical exfoliation process plays a crucial role in the exfoliation of graphite, and the amount of defect in the as-prepared graphene sheets is dependent on electrolytic potential and electrode distance. Moreover, the graphene-based transparent conductive films prepared by simple modified vacuum filtration exhibit an excellent transparency and a low sheet resistance after being treated with NH 4 NO 3 and annealing (∼1.21 kΩ/□ at ∼72.4% transmittance).

Thermoelectric Properties of Cobalt Triantimonide (CoSb3) Prepared by an Electrochemical Technique

DTIC Science & Technology

2010-04-01

of the Co0.95Pd0.05Te0.05Sb2.95 material. Y. Lan et al . (5) suggested that the 9 mean free path for electrons in doped silicon (Si)-germanium...Sakamoto ARL-TR-5141 April 2010 Approved for public release; distribution unlimited...Adelphi, MD 20783-1197 ARL-TR-5141 April 2010 Thermoelectric Properties of Cobalt Triantimonide (CoSb3) Prepared by an Electrochemical

Hydrothermal Synthesis and Electrochemical Properties of CoS2-Reduced Graphene Oxide Nanocomposite for Supercapacitor Application

NASA Astrophysics Data System (ADS)

Venkateshalu, Sandhya; Rangappa, Dinesh; Grace, Andrews Nirmala

A Cobalt disulfide-reduced graphene oxide (CoS2-RGO) nanocomposite was prepared by a simple hydrothermal method and the prepared nanocomposite was characterized using various techniques like XRD, SEM and FTIR. The results of these techniques indicated the uniform deposition of CoS2 nanoparticles on Graphene sheets. Further, the prepared nanocomposites were tested for its activity towards energy storage and the test results showed a specific capacitance of 28F/g in an aqueous 20% KOH electrolyte at a current density of 0.5A/g. All these materials showed highly reversible charge-discharge cycles. The overall electrochemical performance of this composite is shown to be drastically improved when compared to bare CoS2 nanoparticles. Thus with the good electrochemical properties, CoS2-RGO nanocomposites could be effectively used as an electrode material for supercapacitors.

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

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

2015-10-15

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

Fabrication of surface micro- and nanostructures for superhydrophobic surfaces in electric and electronic applications

NASA Astrophysics Data System (ADS)

Xiu, Yonghao

In our study, the superhydrophobic surface based on biomimetic lotus leave is explored to maintain the desired properties for self-cleaning. Parameters in controlling bead-up and roll-off characteristics of water droplets were investigated on different model surfaces. The governing equations were proposed. Heuristic study is performed. First, the fundamental understanding of the effect of roughness on superhydrophobicity is performed. The effect of hierarchical roughness, i.e., two scale roughness effect on roughness is investigated using systems of (1) monodisperse colloidal silica sphere (submicron) arrays and Au nanoparticle on top and (2) Si micrometer pyramids and Si nanostructures on top from KOH etching and metal assisted etching of Si. The relation between the contact area fraction and water droplet contact angles are derived based on Wenzel and Cassie-Baxter equation for the systems and the two scale effect is explained regarding the synergistic combination of two scales. Previously the microscopic three-phase-contact line is thought to be the key factor in determining contact angles and hystereses. In our study, Laplace pressure was brought up and related to the three-phase-contact line and taken as a key figure of merit in determining superhydrophobicity. In addition, we are one of the first to study the effect of tapered structures (wall inclination). Combining with a second scale roughness on the tapered structures, stable Cassie state for both water and low surface energy oil may be achieved. This is of great significance for designing both superhydrophobicity and superoleophobicity. Regarding the origin of contact angle hysteresis, study of superhydrophobicity on micrometer Si pillars was performed. The relation between the interface work of function and contact angle hysteresis was proposed and derived mathematically based on the Young-Dupre equation. The three-phase-contact line was further related to a secondary scale roughness induced. Based on our understanding of the roughness effect on superhydrophobicity (both contact angle and hysteresis), structured surfaces from polybutadiene, polyurethane, silica, and Si etc. were successfully prepared. For engineering applications of superhydrophobic surfaces, stability issues regarding UV, mechanical robustness and humid environment need to be investigated. Among these factors, UV stability is the first one to be studied. However, most polymer surfaces we prepared failed the purpose. Silica surfaces with excellent UV stability were prepared. This method consists of preparation of rough silica surfaces, thermal treatment and the following surface hydrophobization by fluoroalkyl silane treatment. Fluoroalkyl groups are UV stable and the underlying species are silica which is also UV stable (UV transparent). UV stability on the surface currently is 5,500 h according the standard test method of ASTM D 4329. No degradation on surface superhydrophobicity was observed. New methods for preparing superhydrophobic and transparent silica surfaces were investigated using urea-choline chloride eutectic liquid to generate fine roughness and reduce the cost for preparation of surface structures. Another possible application for self-cleaning in photovoltaic panels was investigated on Si surfaces by construction of the two-scale rough structures followed by fluoroalkyl silane treatment. Metal (Au) assisted etching was employed to fabricate nanostructures on micrometer pyramid surfaces. The light reflection on the prepared surfaces was investigated. After surface texturing using KOH etching for micrometer pyramids and the following nanostructure using metal assisted etching, surface light reflection reduced to a minimum value which shows that this surface texturing technique is highly promising for improving the photovoltaic efficiency while imparting photovoltaics the self-cleaning feature. This surface is also expected to be UV stable due to the same fluoroalkyl silane used. Regarding the mechanical robustness, epoxy-silica superhydrophobic surfaces were prepared by O2 plasma etching to generate enough surface roughness of silica spheres followed by fluoroalkyl silane treatment. A robustness test method was proposed and the test results showed that the surface is among the most robust surfaces for the superhydrophobic surfaces we prepared and currently reported in literature.

One-step electrochemical deposition of a graphene-ZrO 2 nanocomposite: Preparation, characterization and application for detection of organophosphorus agents

DOE Office of Scientific and Technical Information (OSTI.GOV)

Du, Dan; Liu, Juan; Zhang, Xiao-Yan

2011-04-27

This paper described the preparation, characterization, and electrochemical properties of a graphene-ZrO 2 nanocomposite (GZN) and its application for both the enrichment and detection of methyl parathion (MP). GZN was fabricated using electrochemical deposition and characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), which showed the successful formation of nanocomposites. Due to the strong affinity to the phosphoric group and the fast electron-transfer kinetics of GZN, both the extraction and electrochemical detection of organophosphorus (OP) agents at the same GZN modified electrochemical sensor was possible. The combination of solid-phase extractionmore » and stripping voltammetric analysis allowed fast, sensitive, and selective determination of MP in garlic samples. The stripping response was highly linear over the MP concentrations ranging from 0.5 ng mL -1 to 100 ng mL -1, with a detection limit of 0.1 ng mL -1. This new nanocomposite-based electrochemical sensor provides an opportunity to develop a field-deployable, sensitive, and quantitative method for monitoring exposure to OPs.« less

Particles induced surface nanoroughness of titanium surface and its influence on adhesion of osteoblast-like MG-63 cells

NASA Astrophysics Data System (ADS)

Solař, P.; Kylián, O.; Marek, A.; Vandrovcová, M.; Bačáková, L.; Hanuš, J.; Vyskočil, J.; Slavínská, D.; Biederman, H.

2015-01-01

Titanium is one of the most common materials employed for production of implants, which is due to its good biocompatibility. However, the colonization of titanium surface by osteoblast cells may be influenced by its roughness and therefore precise control of roughness of titanium surface as well as identification of its optimal value for growth of cells is of high importance. In this study the nanorough titanium surfaces were prepared on polished disks of TiAlV by two step method of deposition. In the first step TiAlV were coated by nanoparticles generated by gas aggregation sources. Such prepared films of nanoparticles were subsequently covered with a titanium overlayer. Different values of surface roughness in the range 1-100 nm were achieved by variation of the size and number of the nanoparticles. Such prepared surfaces were subsequently used for investigation of influence of roughness of titanium surfaces on the adhesion of human osteoblast-like MG-63 cells. It was found out that 7 days after seeding the highest number of adhering cells was observed for samples with root-mean-square roughness of 30 nm.

Corrosion resistance of the microarc oxidation coatings prepared on magnesium alloy

NASA Astrophysics Data System (ADS)

Lv, Ying; Li, Jun Gang; Wu, Ming Zhong; Ma, Zhen; Zhang, Jing Qiang; Wang, Le Le

2018-06-01

Ceramic coatings were prepared on the surface of AZ91D magnesium alloy by microarc oxidation technology. The effects of different voltages on morphology, phase composition and thickness of the coatings were characterized by SEM and XRD. The corrosion resistance of the coatings was measured by electrochemical workstation. Results indicated that the microarc oxidation coatings prepared in sodium silicate electrolyte exhibited porous surface and mainly comprised MgO, Mg2SiO4 and a small amount of MgAl2O4. The thickness of the oxide coatings increased rapidly with the increase of voltage. The coating prepared at 400V voltage had good electrochemical corrosion resistance in 3.5wt% NaCl solution.

Outstanding resistance and passivation behaviour of new Fe-Co metal-metal glassy alloys in alkaline media

PubMed Central

Al-Harbi, Albandaree K.

2018-01-01

The electrochemical behavior of the oxide layers on two metal-metal glassy alloys, Fe78Co9Cr10Mo2Al1 (VX9)and Fe49Co49V2 (VX50) (at.%), were studied using electrochemical techniques including electrochemical frequency modulation (EFM), electrochemical impedance spectroscopy (EIS) and cyclic polarization (CP) measurements. The morphology and composition of the alloy surfaces were investigated using X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and atomic force microscopy (AFM). The corrosion rate and surface roughness of both alloys increased as the concentration of NaOH in aqueous solution was raised. The presence of some protective elements in the composition of the alloys led to the formation of a spontaneous passive layer on the alloy surface. The higher resistance values of both alloys were associated with the magnitude of the dielectric properties of the passive films formed on their surfaces. Both alloys are classified as having outstanding resistance to corrosion, which results from the formation of a passive film that acts as an efficient barrier to corrosion in alkaline solution. PMID:29337992

Outstanding resistance and passivation behaviour of new Fe-Co metal-metal glassy alloys in alkaline media.

PubMed

Emran, Khadijah M; Al-Harbi, Albandaree K

2018-01-01

The electrochemical behavior of the oxide layers on two metal-metal glassy alloys, Fe78Co9Cr10Mo2Al1 (VX9)and Fe49Co49V2 (VX50) (at.%), were studied using electrochemical techniques including electrochemical frequency modulation (EFM), electrochemical impedance spectroscopy (EIS) and cyclic polarization (CP) measurements. The morphology and composition of the alloy surfaces were investigated using X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and atomic force microscopy (AFM). The corrosion rate and surface roughness of both alloys increased as the concentration of NaOH in aqueous solution was raised. The presence of some protective elements in the composition of the alloys led to the formation of a spontaneous passive layer on the alloy surface. The higher resistance values of both alloys were associated with the magnitude of the dielectric properties of the passive films formed on their surfaces. Both alloys are classified as having outstanding resistance to corrosion, which results from the formation of a passive film that acts as an efficient barrier to corrosion in alkaline solution.

Electrochemical Performance of Ni-MOFs for Supercapacitors

NASA Astrophysics Data System (ADS)

Li, Yujuan; Song, Lili; Han, Yinghui; Wang, Guangyou

2018-03-01

In this work, the Ni-MOFs of electrode material has been synthesized, characterized and studied for the electrochemical properties of electrode materials. The effects of the doping amount of Ni, calcination temperature and time were studied in detail. The results suggested that the electrochemical properties were obviously improved by the Ni-MOFs of electrode material and the best preparation conditions can also improve the electrochemical properties of electrode materials. These results open a way for the design of tailored MOFs as electrode materials for supercapacitors.

An electrochemical rebalance cell for Redox systems

NASA Technical Reports Server (NTRS)

Acevedo, J. C.; Stalnaker, D. K.

1983-01-01

An electrochemical rebalance cell for maintaining electrochemical balance, at the system level, of the acidified aqueous iron chloride and chromium chloride reactant solutions in the redox energy storage system was constructed and evaluated. The electrochemical reaction for the cathode is Fe(+3) + e(-) yields Fe(+2), and that for the anode is 1/2H2 yields H(+) + e(-). The iron (carbon felt) electrode and the hydrogen (platinized carbon) electrode are separated by an anion exchange membrane. The performance of the rebalance cell is discussed as well as the assembly of a single rebalance cell and multicell stacks. Various cell configurations were tested and the results are presented and discussed. The rebalance cell was also used to demonstrate its ability, as a preparative tool, for making high purity solutions of soluble reduced metal ionic species. Preparations of titanium, copper, vanadium and chromium ions in acidified solutions were evaluated.

Electrochemical Detection of p-Aminophenol by Flexible Devices Based on Multi-Wall Carbon Nanotubes Dispersed in Electrochemically Modified Nafion

PubMed Central

Scandurra, Graziella; Antonella, Arena; Ciofi, Carmine; Saitta, Gaetano; Lanza, Maurizio

2014-01-01

A conducting composite prepared by dispersing multi-walled carbon nanotubes (MWCNTs) into a host matrix consisting of Nafion, electrochemically doped with copper, has been prepared, characterized and used to modify one of the gold electrodes of simply designed electrochemical cells having copier grade transparency sheets as substrates. Electrical measurements performed in deionized water show that the Au/Nafion/Au-MWCNTs–Nafion:Cu cells can be successfully used in order to detect the presence of p-aminophenol (PAP) in water, without the need for any supporting electrolyte. The intensity of the redox peaks arising when PAP is added to deionized water is found to be linearly related to the analyte in the range from 0.2 to 1.6 μM, with a detection limit of 90 nM and a sensitivity of 7 μA·(μM−1)·cm−2. PMID:24854357

An investigation into magnetic electrolytic abrasive turning

NASA Astrophysics Data System (ADS)

Mahdy, M. A. M.; Ismaeial, A. L.; Aly, F. F.

2013-07-01

The magnetic electrolytic abrasive turning (MEAT) process as a non-traditional machining is used to obtain surface finishing like mirror. MEAT provides one of the best alternatives for producing complex shapes with good finish in advanced materials used in aircraft and aerospace industries. The improvement of machining accuracy of MEAT continues to be a major challenge for modern industry. MEAT is a hybrid machining which combines two or more processes to remove material. The present research focuses on the development of precision electrochemical turning (ECT) under the effects of magnetic field and abrasives. The effect of magnetic flux density, electrochemical conditions and abrasive parameters on finishing efficiency and surface roughness are investigated. An empirical relationship is deduced.

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

PubMed

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

2018-02-12

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

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

PubMed Central

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

2018-01-01

Electrochemical polymerization of aniline is one of the most promising methods to prepare polyaniline (PANI) materials. However, during this process, the electrolyte solution must be replaced after electropolymerization of a certain time because of the generation and the accumulation of the by-products, which have significant effects on the morphology, purity and properties of PANI products. Treatment and recycling of the used electrolyte solution are worthwhile to study to reduce the high treatment cost of the used electrolyte solution containing aniline and its polymerization by-products. Here, the composition of the used electrolyte solution was separated and determined by high performance liquid chromatography coupled with diode array detection (HPLC-DAD) in the range of ultraviolet and visible (UV-Vis) light. The analysis results revealed that the used electrolyte solution consisted of aniline, p-hydroquinone (HQ), p-benzoquinone (BQ), co-oligomers of aniline and p-benzoquinone (CAB) and acid. Then, n-octanol and 2-octanone were selected as extracts to remove HQ, BQ and CAB from the used electrolyte solution. Following that, the recycled electrolyte solution was prepared by adjusting the concentration of aniline and acid of the aqueous phase, and the electrochemical polymerization process was conducted. Finally, the obtained PANI was characterized by scanning electron microscope (SEM) and electrochemical methods. The experimental results clearly demonstrate that the morphology and specific capacitance of PANI produced from the recycled electrolyte solution can be recovered completely. This research paves the way for reusing the used electrolyte solution for aniline electrochemical polymerization. PMID:29439514

Electrocatalyst compositions

DOEpatents

Mallouk, Thomas E.; Chan, Benny C.; Reddington, Erik; Sapienza, Anthony; Chen, Guoying; Smotkin, Eugene; Gurau, Bogdan; Viswanathan, Rameshkrishnan; Liu, Renxuan

2001-09-04

Compositions for use as catalysts in electrochemical reactions are described. The compositions are alloys prepared from two or more elemental metals selected from platinum, molybdenum, osmium, ruthenium, rhodium, and iridium. Also described are electrode compositions including such alloys and electrochemical reaction devices including such catalysts.

Synthesis and electrochemical properties of polyaniline nanofibers by interfacial polymerization.

PubMed

Manuel, James; Ahn, Jou-Hyeon; Kim, Dul-Sun; Ahn, Hyo-Jun; Kim, Ki-Won; Kim, Jae-Kwang; Jacobsson, Per

2012-04-01

Polyaniline nanofibers were prepared by interfacial polymerization with different organic solvents such as chloroform and carbon tetrachloride. Field emission scanning electron microscopy and transmission electron microscopy were used to study the morphological properties of polyaniline nanofibers. Chemical characterization was carried out using Fourier transform infrared spectroscopy, UV-Vis spectroscopy, and X-ray diffraction spectroscopy and surface area was measured using BET isotherm. Polyaniline nanofibers doped with lithium hexafluorophosphate were prepared and their electrochemical properties were evaluated.

Morphological Behavior of Printed Silver Electrodes with Protective Self-Assembled Monolayers for Electrochemical Migration.

PubMed

Sekine, Tomohito; Sato, Jun; Takeda, Yasunori; Kumaki, Daisuke; Tokito, Shizuo

2018-05-09

We evaluated the electrochemical behaviors and reliability of printed silver (Ag) electrodes prepared from nanoparticle inks with the use of protective self-assembled monolayers (SAMs) under electronic bias conditions. The printed Ag electrodes were fabricated by inkjet printing on a hydrophobic substrate. The SAMs, which acted as barriers to moisture, were prepared by immersing the substrate in a pentafluorobenzenethiol solution at ambient temperature (25 °C). We investigated the electrochemical migration phenomenon using the water drop method, and the results showed that the formation of dendrites connecting the cathode and the anode, which can affect the electrochemical reliability of an electric device, was suppressed in the presence of the SAMs. The time before short circuit occurred was found to depend on the spacing between the electrodes, i.e., 130 s, when the distance between the electrodes was 200 μm in the presence of an SAM. We demonstrated that Ag electrodes treated using the procedure described in this work suppress the occurrence of electrical short circuits caused by Ag dendrite formation and thus their electrochemical properties are substantially improved.

Dye-doped nanostructure polypyrrole film for electrochemically switching solid-phase microextraction of Ni(II) and ICP-OES analysis of waste water.

PubMed

Shamaeli, Ehsan; Alizadeh, Naader

2012-01-01

A nanostructure fiber based on conducting polypyrrole synthesized by an electrochemical method has been developed, and used for electrochemically switching solid-phase microextraction (ES-SPME). The ES-SPME was prepared by the doping of eriochrome blue in polypyrrole (PPy-ECB) and used for selectively extracting the Ni(II) cation in the presence of some transition and heavy metal ions. The cation-exchange behavior of electrochemically prepared polypyrrole on stainless-steel with and without eriochrome blue (ECB) dye was characterized using ICP-OES analysis. The effects of the scan rate for electrochemical synthesis, uptake and the release potential on the extraction behavior of the PPy-ECB conductive fiber were studied. Uptake and release time profiles show that the process of electrically switched cation exchange could be completed within 250 s. The results of the present study point concerning the possibility of developing a selective extraction process for Ni(II) from waste water was explored using such a nanostructured PPy-ECB film through an electrically switched cation exchange. 2012 © The Japan Society for Analytical Chemistry

Preparation, electrochemical and spectral properties of free-base and manganese N-methyl-pyridylethynyl porphyrins.

PubMed

Lin, Ching-Yao; Chen, Yen-Chuan; Yao, Chi-Wen; Huang, Sung-Chou; Cheng, Yi-Hui

2008-02-14

Two series of free-base and manganese N-methyl-pyridylethynyl-5,15-biphenyl porphyrins were synthesized, and their UV-Visible, electrochemical and spectro-electrochemical properties were studied. Cyclic voltammetry experiments showed positive shifts in the reduction potentials and the UV-Visible spectra showed significant red-shifts in the absorption wavelengths of these porphyrins, indicating the effects of N-methyl-pyridylethynyl substituents.

Electrochemical preparation of MnO2 nanobelts through pulse base-electrogeneration and evaluation of their electrochemical performance

NASA Astrophysics Data System (ADS)

Aghazadeh, Mustafa; Maragheh, Mohammad Ghannadi; Ganjali, Mohammad Reza; Norouzi, Parviz; Faridbod, Farnoush

2016-02-01

Cathodic electrodeposition of MnO2 from a nitrate solution, via pulsed base (OH-) electrogeneration was performed for the first time. The deposition experiments were performed in a pulse current mode in typical on-times and off-times (i.e. ton = 1 s and toff = 1 s) with a peak current density of 2 mA cm-2 (Ia = 2 mA cm-2). The structural characterizations conducted by XRD and FTIR techniques revealed that the prepared MnO2 is composed of both α and γ phases. Morphological observation by SEM and TEM showed that the prepared MnO2 is made up of nanobelts with uniform shapes (an average diameter and length of 50 nm and 1 μm, respectively). Further electrochemical measurements by cyclic voltammetry and charge-discharge techniques revealed that the prepared MnO2 nanostructures have excellent capacitive behaviors, like a specific capacitance of 235.5 F g-1 and capacity retention of 91.3% after 1000 cycling at the scan rate of 25 mV s-1.

High performance electrode material for supercapacitors based on α-Co(OH)2 nano-sheets prepared through pulse current cathodic electro-deposition (PC-CED)

NASA Astrophysics Data System (ADS)

Aghazadeh, Mustafa; Rashidi, Amir; Ganjali, Mohammad Reza

2018-01-01

In this paper, the well-defined nano-sheets of α-Co(OH)2 were prepared through the cathodic electrosynthesis from an additive-free aqueous cobalt nitrate bath. The pulse current cathodic electro-deposition (PC-CED) was used as the means for the controlling the OH- electrogeneration on the cathode surface. The characteristics and electrochemical behavior of the prepared cobalt hydroxide were also assessed through SEM, TEM, XRD, BET, and IR. The results proved the product to be composed of crystalline pure α phase of cobalt hydroxide with sheet-like morphology at nanoscale. Evaluations of the electrochemical behaviour of the α-Co(OH)2 nano-sheets revealed that they are capable to delivering the specific capacitance of 1122 F g-1 at a discharge load of 3 A g-1 and SC retention of 84% after 4000 continues discharging cycles, suggesting the nano-sheets as promising candidates for use in electrochemical supercapacitors. Further, the method used for the preparation of the compounds enjoys the capability of being scaled up. [Figure not available: see fulltext.

Electrochemical properties of Ti3+ doped Ag-Ti nanotube arrays coated with hydroxyapatite

NASA Astrophysics Data System (ADS)

Zhang, Hangzhou; Shi, Xiaoguo; Tian, Ang; Wang, Li; Liu, Chuangwei

2018-04-01

Ag-Ti nanotube array was prepared by simple anodic oxidation method and uniform hydroxyapatite were electrochemically deposited on the nanotubes, and then characterized by SEM, XRD, XPS and EIS. In order to investigate the influence of Ti3+ on the electrochemical deposition of hydroxyapatite on the nanotubes, the Ag-Ti nanotube array self-doped with Ti3+ was prepared by one step reduction method. The experiment results revealed that the Ti3+ can promote the grow rate of hydroxyapatite coatings on nanotube surface. The hydroxyapatite coated Ag-Ti nanotube arrays with Ti3+ exhibit excellent stability and higher corrosion resistance. Moreover, the compact and dense hydroxyapatite coating can also prevent the Ag atom erosion from the Ag-Ti nanotube.

Electrochemical slurry compositions and methods for preparing the same

DOEpatents

Doherty, Tristan; Limthongkul, Pimpa; Butros, Asli; Duduta, Mihai; Cross, III, James C.

2016-11-01

Embodiments described herein generally relate to semi-solid suspensions, and more particularly to systems and methods for preparing semi-solid suspensions for use as electrodes in electrochemical devices such as, for example batteries. In some embodiments, a method for preparing a semi-solid electrode includes combining a quantity of an active material with a quantity of an electrolyte to form an intermediate material. The intermediate material is then combined with a conductive additive to form an electrode material. The electrode material is mixed to form a suspension having a mixing index of at least about 0.80 and is then formed into a semi-solid electrode.

Physicochemical properties of precursors of Al2O3-ZrO2 oxide ceramics prepared by electrochemical method

NASA Astrophysics Data System (ADS)

Petrova, E. V.; Dresvyannikov, A. F.; Ahmadi Daryakenari, M.; Khairullina, A. I.

2016-05-01

Scanning electron microscopy, X-ray, and thermal analysis are used to examine the structure and properties of dispersive systems based on aluminum and zirconium oxides prepared electrochemically. The effect the conditions of synthesis have on the structure and morphology of Al2O3-ZrO2 particles is studied. It is shown that the effect of an electric field on the reaction medium allows us to adjust the physicochemical properties and morphology.

Electrochemical Behavior of the Oxide Formed by Reduction of RuO4(2-): A ph-Dependent Ruthenium Oxide-Based Microelectrochemical Transistor

DTIC Science & Technology

1990-05-16

Angerstein-Kozlowska, H.; Vukovic , M.; Conway, B. E. J . Electrochem. Soc. 1978, 125, 1473. 15. Earke, L. D.; Mulcahy, J . K.; Venkatesan, S. J ...90 5f / . j . CON 16. SUPPLEMENTARY NOTATION Prepared for publication in Chemistry of Materials 17. COSATI CODES 18. SUBJECT ;ERMS (Continue on reverse...Microelectrochemical Transistor by Donald F. Lyons, Martin 0. Schloh, James J . Hickman and Mark S. Wrighton Prepared for Publication in Chemistry of Materials

A study for hypergolic vapor sensor development

NASA Technical Reports Server (NTRS)

Stetter, J. R.

1977-01-01

The use of an electrochemical technique for MMH and N02 measurement was investigated. Specific MMH and N02 electrochemical sensors were developed. Experimental techniques for preparation, handling, and analysis of hydrazine's vapor mixtures at ppb and ppm levels were developed. Two approaches to N02 instrument design were evaluated including specific adsorption and specific electrochemical reduction. Two approaches to hydrazines monitoring were evaluated including catalytic conversion to N0 with subsequent N0 detection and direct specific electrochemical oxidation. Two engineering prototype MMH/N02 monitors were designed and constructed.

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

PubMed

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.

HYDROGENATION OF OLEFINS USING PALLADIUM NANOPARTICLES PREPARED WITH PULSE ELECTROCHEMICAL DEPOSITION

EPA Science Inventory

Electrochemistry has been used to synthesize nano-structured materials. In this project, we have conducted the application of electrochemistry for the synthesis of nano-palladium catalysts that may have application in the area of green chemistry. The electrochemical technique use...

Platinum-Free Counter Electrode Comprised of Metal-Organic-Framework (MOF)-Derived Cobalt Sulfide Nanoparticles for Efficient Dye-Sensitized Solar Cells (DSSCs)

PubMed Central

Hsu, Shao-Hui; Li, Chun-Ting; Chien, Heng-Ta; Salunkhe, Rahul R.; Suzuki, Norihiro; Yamauchi, Yusuke; Ho, Kuo-Chuan; Wu, Kevin C.-W.

2014-01-01

We fabricated a highly efficient (with a solar-to-electricity conversion efficiency (η) of 8.1%) Pt-free dye-sensitized solar cell (DSSC). The counter electrode was made of cobalt sulfide (CoS) nanoparticles synthesized via surfactant-assisted preparation of a metal organic framework, ZIF-67, with controllable particle sizes (50 to 320 nm) and subsequent oxidation and sulfide conversion. In contrast to conventional Pt counter electrodes, the synthesized CoS nanoparticles exhibited higher external surface areas and roughness factors, as evidenced by X-ray diffraction (XRD), scanning electron microscopy (SEM) element mapping, and electrochemical analysis. Incident photon-to-current conversion efficiency (IPCE) results showed an increase in the open circuit voltage (VOC) and a decrease in the short-circuit photocurrent density (Jsc) for CoS-based DSSCs compared to Pt-based DSSCs, resulting in a similar power conversion efficiency. The CoS-based DSSC fabricated in the study show great potential for economically friendly production of Pt-free DSSCs. PMID:25382139

[Corrosion resistant properties of different anodized microtopographies on titanium surfaces].

PubMed

Fangjun, Huo; Li, Xie; Xingye, Tong; Yueting, Wang; Weihua, Guo; Weidong, Tian

2015-12-01

To investigate the corrosion resistant properties of titanium samples prepared by anodic oxidation with different surface morphologies. Pure titanium substrates were treated by anodic oxidation to obtain porous titanium films in micron, submicron, and micron-submicron scales. The surface morphologies, coating cross-sectional morphologies, crystalline structures, and surface roughness of these samples were characterized. Electrochemical technique was used to measure the corrosion potential (Ecorr), current density of corrosion (Icorr), and polarization resistance (Rp) of these samples in a simulated body fluid. Pure titanium could be modified to exhibit different surface morphologies by the anodic oxidation technique. The Tafel curve results showed that the technique can improve the corrosion resistance of pure titanium. Furthermore, the corrosion resistance varied with different surface morphologies. The submicron porous surface sample demonstrated the best corrosion resistance, with maximal Ecorr and Rp and minimal Icorr. Anodic oxidation technology can improve the corrosion resistance of pure titanium in a simulated body fluid. The submicron porous surface sample exhibited the best corrosion resistance because of its small surface area and thick barrier layer.

One-pot synthesis of MoS2/In2S3 ultrathin nanoflakes with mesh-shaped structure on indium tin oxide as photocathode for enhanced photo-and electrochemical hydrogen evolution reaction

NASA Astrophysics Data System (ADS)

Sun, Baoliang; Shan, Fei; Jiang, Xinxin; Ji, Jing; Wang, Feng

2018-03-01

A bifunctional MoS2/In2S3 hybrid composite that has both photo- and electrocatalytic activity toward hydrogen evolution reaction (HER) is prepared by a facile one pot hydrothermal method. The characterizations by scanning electron microscope (SEM), high resolution transmission electron microscope (HRTEM) and Photoluminescence (PL) shows that the MoS2/In2S3 hybrid exhibits ultrathin nanoflakes with mesh-shaped structure on transparent conductive substrates, and the as prepared catalyst composite obviously improves the separation of electro-hole pairs. The as prepared hybrid nanosheets with Mo:In of 1/2 integrate In-doped MoS2 to reduce the stacking and increase the active surface area. The novel mesh-shaped nanostructure with a moderate degree of disorder provides not only simultaneously intrinsic conductivity and defects but also higher electrochemically active surface area (ECSA). By electrochemical measurements, such as linear sweep voltammetry (LSV), electrochemical impedance spectroscope (EIS) and cyclic voltammetry (CV), we find that the MoS2/In2S3 hybrid possesses much better photo/electrochemical activity than pristine MoS2 or In2S3. MoS2/In2S3 ultrathin nanoflaks are anticipated to be a superior photoelectrocatalyst for PEC cells, and the rational use of the MoS2/In2S3 cathode offers a new avenue toward achieving effective photo-assistant electrocatalytic activity.

Preparation of activated carbon hollow fibers from ramie at low temperature for electric double-layer capacitor applications.

PubMed

Du, Xuan; Zhao, Wei; Wang, Yi; Wang, Chengyang; Chen, Mingming; Qi, Tao; Hua, Chao; Ma, Mingguo

2013-12-01

Activated carbon hollow fibers (ACHFs) with high surface area were prepared from inexpensive, renewable ramie fibers (RFs) by a single-step activation method under lower temperature than that of other reports. The effects of activation conditions on the pore structure and turbostratic structure of ACHFs were investigated systematically. The results show that ACHFs surface area decreased but micropore volume and conductivity increased as the increase of activation temperature and activation time. The electrochemical measurements of supercapacitors fabricated from these ACHFs electrodes reveal that the electrochemical properties improved with the enhancing of activation degree. However, too high activation temperature can make the ion diffusion resistance increase. It suggests that pore structure and conductivity are as important as surface area to decide the electrochemical performances of ACHFs electrode materials. A maximum capacity of 287 F g(-1) at 50 mA g(-1) was obtained for the ACHFs electrode prepared under suitable conditions. Copyright © 2013 Elsevier Ltd. All rights reserved.

Preparation and electrochemical characterization of polymer electrolytes based on electrospun poly(vinylidene fluoride- co-hexafluoropropylene)/polyacrylonitrile blend/composite membranes for lithium batteries

NASA Astrophysics Data System (ADS)

Raghavan, Prasanth; Zhao, Xiaohui; Shin, Chorong; Baek, Dong-Ho; Choi, Jae-Won; Manuel, James; Heo, Min-Yeong; Ahn, Jou-Hyeon; Nah, Changwoon

Apart from PEO based solid polymer electrolytes, tailor-made gel polymer electrolytes based on blend/composite membranes of poly(vinylidene fluoride- co-hexafluoropropylene) and polyacrylonitrile are prepared by electrospinning using 14 wt% polymer solution in dimethylformamide. The membranes show uniform morphology with an average fiber diameter of 320-490 nm, high porosity and electrolyte uptake. Polymer electrolytes are prepared by soaking the electrospun membranes in 1 M lithium hexafluorophosphate in ethylene carbonate/dimethyl carbonate. Temperature dependent ionic conductivity and their electrochemical performance are studied. The blend/composite polymer electrolytes show good ionic conductivity in the range of 10 -3 S cm -1 at ambient temperature and good electrochemical performance. All the Polymer electrolytes show an anodic stability >4.6 V with stable interfacial resistance with storage time. The prototype cell shows good charge-discharge properties and stable cycle performance with comparable capacity fade compared to liquid electrolyte under the test conditions.

Surface characteristics and biocompatibility of cranioplasty titanium implants following different surface treatments.

PubMed

Hatamleh, Muhanad M; Wu, Xiaohong; Alnazzawi, Ahmad; Watson, Jason; Watts, David

2018-04-01

Surface and mechanical properties of titanium alloys are integral for their use in restoring bone defects of skull and face regions. These properties are affected by the method of constructing and surface treatment of the titanium implant. This study aimed to investigate the effects of titanium finishing protocols on the surface morphology, hardness and biocompatibility of TiAl6V4. Square shaped TiAl6V4 specimens (ASTM F68) (10×10×0.5mm) were divided into seven groups of different surface treatments (n=10). The treatments included mechanical polishing, sandblasting with AL 2 O 3 (50μm), immersion in different acids, and/or electro-chemical anodization. Weight loss %; 3D micro-roughness; Knoop micro-hardness, and osteoblast cell attachment and proliferation (after 3 days) were determined for each specimen. Data was analysed using one way ANOVA and Dunett T3 post-hoc tests, and t-test (p<0.05). Weight loss % was in the range of 1.70-5.60 as mechanical polishing produced the highest weight loss, followed by sandblasting, and combined protocol of mechanical polishing and acid treatment (p<0.05). Micro-roughness values (μm) were in the range of 2.81-16.68. It was the highest for control specimens (p<0.05), and smoothest surfaces after combined mechanical polishing and acid treatment; or after electro-chemical treatment (p<0.05). Micro-hardness values (MPa) ranged 170.90-442.15 as sandblasting with/without acid treatment caused statically significantly the highest values (p<0.05) while control and mechanically polished specimens had the lowest values (p<0.05). All treatments produced equally biocompatible surfaces (p>0.05) after 1h or 3 days. Furthermore, osteoblast cell proliferation statistically significantly increased after 3days among each surface treatment (p<0.05). Different finishing treatments have variable effect on cranioplasty titanium surface loss, micro-roughness and micro-hardness but constant improved biocompatibility effect. Electro-chemical treatment caused less material loss and produced biocompatible smoothest surface of comparable hardness; hence it can be suitable for cranioplasty titanium surface finishing. Copyright © 2018 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Preparation and electrochemical characterization of polyaniline/activated carbon composites as an electrode material for supercapacitors.

PubMed

Oh, Misoon; Kim, Seok

2012-01-01

Polyaniline (PANI)/activated carbon (AC) composites were prepared by a chemical oxidation polymerization. To find an optimum ratio between PANI and AC which shows superior electrochemical properties, the preparation was carried out in changing the amount of added aniline monomers. The morphology of prepared composites was investigated by scanning electron microscopy (SEM) and transmission electron microscope (TEM). The structural and thermal properties were investigated by Fourier transform infrared spectra (FT-IR) and thermal gravimetric analysis (TGA), respectively. The electrochemical properties were characterized by cyclic voltammetry (CV). Composites showed a summation of capacitances that consisted of two origins. One is double-layer capacitance by ACs and the other is faradic capacitance by redox reaction of PANI. Fiber-like PANIs are coated on the surface of ACs and they contribute to the large surface for redox reaction. The vacancy among fibers provided the better diffusion and accessibility of ion. High capacitances of composites were originated from the network structure having vacancy made by PANI fibers. It was found that the composite prepared with 5 ml of aniline monomer and 0.25 g of AC showed the highest capacitance. Capacitance of 771 F/g was obtained at a scan rate of 5 mV/s.

Dynamic and Tunable Threshold Voltage in Organic Electrochemical Transistors.

PubMed

Doris, Sean E; Pierre, Adrien; Street, Robert A

2018-04-01

In recent years, organic electrochemical transistors (OECTs) have found applications in chemical and biological sensing and interfacing, neuromorphic computing, digital logic, and printed electronics. However, the incorporation of OECTs in practical electronic circuits is limited by the relative lack of control over their threshold voltage, which is important for controlling the power consumption and noise margin in complementary and unipolar circuits. Here, the threshold voltage of OECTs is precisely tuned over a range of more than 1 V by chemically controlling the electrochemical potential at the gate electrode. This threshold voltage tunability is exploited to prepare inverters and amplifiers with improved noise margin and gain, respectively. By coupling the gate electrode with an electrochemical oscillator, single-transistor oscillators based on OECTs with dynamic time-varying threshold voltages are prepared. This work highlights the importance of electrochemistry at the gate electrode in determining the electrical properties of OECTs, and opens a path toward the system-level design of low-power OECT-based electronics. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

An electrochemical sensor based on nitrogen doped carbon material prepared from nitrogen-containing precursors

NASA Astrophysics Data System (ADS)

Cui, G. Y.; Wang, C. Y.; Xiang, G. Q.; Zhou, B.

2018-01-01

In this work, a nitrogen doped carbon material (NDC) was prepared by using a copper adenine complex as precursor and applied to electrochemical sensing of Vitamin B2 (VB2). The experimental results show that the nitrogen doped carbon material is obtained after calcination at 650 °C under argon atmosphere, afterwards, which were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), fourier transform infrared (FT-IR), and electrochemical method. According to the XRD data, the product was a carbon material, and infrared data demonstrates that there are two kinds of carbonyl nitrogen combination, respectively, C-N and C = N combination of ways. Importantly, we used NDC to construct electrochemical biosensor to detect VB2 by differential pulse voltammetry (DPV). The linear range was 6 × 10-6 - 3.5 × 10-4 M (R=0.9962), the minimum detection limit was 5.4 × 10-6 M, and the sensitivity is better. Consequently, it has better sensing performance.

Synthesis and electrochemical performance of hole-rich Li4Ti5O12 anode material for lithium-ion secondary batteries

NASA Astrophysics Data System (ADS)

Zhu, Weibo; Zhuang, Zhenyuan; Yang, Yanmin; Zhang, Ruidan; Lin, Zhiya; Lin, Yingbin; Huang, Zhigao

2016-06-01

Hole-rich Li4Ti5O12 composites are synthesized by spray drying using carbon nanotubes as additives in precursor solution, subsequently followed calcinated at high temperature in air. The structure, morphology, and texture of the as-prepared composites are characterized with XRD, Raman, BET and SEM techniques. The electrochemical properties of the as-prepared composites are investigated systematically by charge/discharge testing, cyclic voltammograms and AC impedance spectroscopy, respectively. In comparison with the pristine Li4Ti5O12, the hole-rich Li4Ti5O12 induced by carbon nanotubes exhibits superior electrochemical performance, especially at high rates. The obtained excellent electrochemical performances of should be attributed to the hole-rich structure of the materials, which offers more connection-area with the electrolyte, shorter diffusion-path length as well faster migration rate for both Li ions and electrons during the charge/discharge process.

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

NASA Astrophysics Data System (ADS)

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

2017-03-01

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

Electric Arc and Electrochemical Surface Texturing Technologies

NASA Technical Reports Server (NTRS)

Banks, Bruce A.; Rutledge, Sharon K.; Snyder, Scott A.

1997-01-01

Surface texturing of conductive materials can readily be accomplished by means of a moving electric arc which produces a plasma from the environmental gases as well as from the vaporized substrate and arc electrode materials. As the arc is forced to move across the substrate surface, a condensate from the plasma re-deposits an extremely rough surface which is intimately mixed and attached to the substrate material. The arc textured surfaces produce greatly enhanced thermal emittance and hold potential for use as high temperature radiator surfaces in space, as well as in systems which use radiative heat dissipation such as computer assisted tomography (CAT) scan systems. Electrochemical texturing of titanium alloys can be accomplished by using sodium chloride solutions along with ultrasonic agitation to produce a random distribution of craters on the surface. The crater size and density can be controlled to produce surface craters appropriately sized for direct bone in-growth of orthopaedic implants. Electric arc texturing and electrochemical texturing techniques, surface properties and potential applications will be presented.

Production and Precipitation Hardening of Beta-Type Ti-35Nb-10Cu Alloy Foam for Implant Applications

NASA Astrophysics Data System (ADS)

Mutlu, Ilven; Yeniyol, Sinem; Oktay, Enver

2016-04-01

In this study, beta-type Ti-35Nb-10Cu alloy foams were produced by powder metallurgy method for dental implant applications. 35% Nb was added to stabilize the beta-Ti phase with low Young's modulus. Cu addition enhanced sinterability and gave precipitation hardening capacity to the alloy. Sintered specimens were precipitation hardened in order to enhance the mechanical properties. Electrochemical corrosion behavior of the specimens was examined by electrochemical impedance spectroscopy in artificial saliva. Electrochemical impedance spectroscopy results indicated that the oxide film on the surface of foam is a bi-layer structure consisting of outer porous layer and inner barrier layer. Impedance values of barrier layer were higher than porous layer. Corrosion resistance of specimens decreased at high fluoride concentrations and at low pH of artificial saliva. Corrosion resistance of alloys was slightly decreased with aging. Mechanical properties, microstructure, and surface roughness of the specimens were also examined.

Molecular architecture: construction of self-assembled organophosphonate duplexes and their electrochemical characterization.

PubMed

Cattani-Scholz, Anna; Liao, Kung-Ching; Bora, Achyut; Pathak, Anshuma; Hundschell, Christian; Nickel, Bert; Schwartz, Jeffrey; Abstreiter, Gerhard; Tornow, Marc

2012-05-22

Self-assembled monolayers of phosphonates (SAMPs) of 11-hydroxyundecylphosphonic acid, 2,6-diphosphonoanthracene, 9,10-diphenyl-2,6-diphosphonoanthracene, and 10,10'-diphosphono-9,9'-bianthracene and a novel self-assembled organophosphonate duplex ensemble were synthesized on nanometer-thick SiO(2)-coated, highly doped silicon electrodes. The duplex ensemble was synthesized by first treating the SAMP prepared from an aromatic diphosphonic acid to form a titanium complex-terminated one; this was followed by addition of a second equivalent of the aromatic diphosphonic acid. SAMP homogeneity, roughness, and thickness were evaluated by AFM; SAMP film thickness and the structural contributions of each unit in the duplex were measured by X-ray reflection (XRR). The duplex was compared with the aliphatic and aromatic monolayer SAMPs to determine the effect of stacking on electrochemical properties; these were measured by impedance spectroscopy using aqueous electrolytes in the frequency range 20 Hz to 100 kHz, and data were analyzed using resistance-capacitance network based equivalent circuits. For the 11-hydroxyundecylphosphonate SAMP, C(SAMP) = 2.6 ± 0.2 μF/cm(2), consistent with its measured layer thickness (ca. 1.1 nm). For the anthracene-based SAMPs, C(SAMP) = 6-10 μF/cm(2), which is attributed primarily to a higher effective dielectric constant for the aromatic moieties (ε = 5-10) compared to the aliphatic one; impedance spectroscopy measured the additional capacitance of the second aromatic monolayer in the duplex (2ndSAMP) to be C(Ti/2ndSAMP) = 6.8 ± 0.7 μF/cm(2), in series with the first.

Fabrication of (Co,Mn)3O4/rGO Composite for Lithium Ion Battery Anode by a One-Step Hydrothermal Process with H2O2 as Additive

PubMed Central

Li, Zuohua; Cui, Yanhui; Chen, Jun; Deng, Lianlin

2016-01-01

Binary transition metal oxides have been regarded as one of the most promising candidates for high-performance electrodes in energy storage devices, since they can offer high electrochemical activity and high capacity. Rational designing nanosized metal oxide/carbon composite architectures has been proven to be an effective way to improve the electrochemical performance. In this work, the (Co,Mn)3O4 spinel was synthesized and anchored on reduced graphene oxide (rGO) nanosheets using a facile and single hydrothermal step with H2O2 as additive, no further additional calcination required. Analysis showed that this method gives a mixed spinel, i.e. (Co,Mn)3O4, having 2+ and 3+ Co and Mn ions in both the octahedral and tetrahedral sites of the spinel structure, with a nanocubic morphology roughly 20 nm in size. The nanocubes are bound onto the rGO nanosheet uniformly in a single hydrothermal process, then the as-prepared (Co,Mn)3O4/rGO composite was characterized as the anode materials for Li-ion battery (LIB). It can deliver 1130.6 mAh g-1 at current density of 100 mA g-1 with 98% of coulombic efficiency after 140 cycles. At 1000 mA g-1, the capacity can still maintain 750 mAh g-1, demonstrating excellent rate capabilities. Therefore, the one-step process is a facile and promising method to fabricate metal oxide/rGO composite materials for energy storage applications. PMID:27788161

Fabrication of (Co,Mn)3O4/rGO Composite for Lithium Ion Battery Anode by a One-Step Hydrothermal Process with H2O2 as Additive.

PubMed

Li, Zuohua; Cui, Yanhui; Chen, Jun; Deng, Lianlin; Wu, Junwei

2016-01-01

Binary transition metal oxides have been regarded as one of the most promising candidates for high-performance electrodes in energy storage devices, since they can offer high electrochemical activity and high capacity. Rational designing nanosized metal oxide/carbon composite architectures has been proven to be an effective way to improve the electrochemical performance. In this work, the (Co,Mn)3O4 spinel was synthesized and anchored on reduced graphene oxide (rGO) nanosheets using a facile and single hydrothermal step with H2O2 as additive, no further additional calcination required. Analysis showed that this method gives a mixed spinel, i.e. (Co,Mn)3O4, having 2+ and 3+ Co and Mn ions in both the octahedral and tetrahedral sites of the spinel structure, with a nanocubic morphology roughly 20 nm in size. The nanocubes are bound onto the rGO nanosheet uniformly in a single hydrothermal process, then the as-prepared (Co,Mn)3O4/rGO composite was characterized as the anode materials for Li-ion battery (LIB). It can deliver 1130.6 mAh g-1 at current density of 100 mA g-1 with 98% of coulombic efficiency after 140 cycles. At 1000 mA g-1, the capacity can still maintain 750 mAh g-1, demonstrating excellent rate capabilities. Therefore, the one-step process is a facile and promising method to fabricate metal oxide/rGO composite materials for energy storage applications.

Electrodeposition synthesis and electrochemical properties of nanostructured γ-MnO 2 films

NASA Astrophysics Data System (ADS)

Chou, Shulei; Cheng, Fangyi; Chen, Jun

The thin films of carambola-like γ-MnO 2 nanoflakes with about 20 nm in thickness and at least 200 nm in width were prepared on nickel sheets by combination of potentiostatic and cyclic voltammetric electrodeposition techniques. The as-prepared MnO 2 nanomaterials, which were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS), were used as the active material of the positive electrode for primary alkaline Zn/MnO 2 batteries and electrochemical supercapacitors. Electrochemical measurements showed that the MnO 2 nanoflake films displayed high potential plateau (around 1.0 V versus Zn) in primary Zn/MnO 2 batteries at the discharge current density of 500 mA g -1 and high specific capacitance of 240 F g -1 at the current density of 1 mA cm -2. This indicated the potential application of carambola-like γ-MnO 2 nanoflakes in high-power batteries and electrochemical supercapacitors. The growth process for the one- and three-dimensional nanostructured MnO 2 was discussed on the basis of potentiostatic and cyclic voltammetric techniques. The present synthesis method can be extended to the preparation of other nanostructured metal-oxide films.

A robust electrochemical immunosensor based on hydroxyl pillar[5]arene@AuNPs@g-C3N4 hybrid nanomaterial for ultrasensitive detection of prostate specific antigen.

PubMed

Zhou, Xu; Yang, Long; Tan, Xiaoping; Zhao, Genfu; Xie, Xiaoguang; Du, Guanben

2018-07-30

Prostate specific antigen (PSA) is the most significant biomarker for the screening of prostate cancer in human serum. However, most methods for the detection of PSA often require major laboratories, precisely analytical instruments and complicated operations. Currently, the design and development of satisfying electrochemical biosensors based on biomimetic materials (e.g. synthetic receptors) and nanotechnology is highly desired. Thus, we focused on the combination of molecular recognition and versatile nanomaterials in electrochemical devices for advancing their analytical performance and robustness. Herein, by using the present prepared multifunctional hydroxyl pillar[5]arene@gold nanoparticles@graphitic carbon nitride (HP5@AuNPs@g-C 3 N 4 ) hybrid nanomaterial as robust biomimetic element, a high-performance electrochemical immunosensor for detection of PSA was constructed. The as-prepared immunosensor, with typically competitive advantages of low cost, simple preparation and fast detection, exhibited remarkable robustness, ultra-sensitivity, excellent selectivity and reproducibility. The limit of detection (LOD) and linear range were 0.12 pg mL -1 (S/N = 3) and 0.0005-10.00 ng mL -1 , respectively. The satisfying results provide a promising approach for clinical detection of PSA in human serum. Copyright © 2018 Elsevier B.V. All rights reserved.

Dual-responsive immunosensor that combines colorimetric recognition and electrochemical response for ultrasensitive detection of cancer biomarkers.

PubMed

Hong, Wooyoung; Lee, Sooyeon; Cho, Youngnam

2016-12-15

We developed a nanoroughened, biotin-doped polypyrrole immunosensor for the detection of tumor markers through dual-signal (electrochemical and colorimetric) channels, electrochemical and colorimetric, that demonstrates remarkable analytical performance. A rapid, one-step electric field-mediated method was employed to fabricate the immunosensor with nanoscale roughness by simply modulating the applied electrical potential. We demonstrated the successful detection of three tumor markers (CA125, CEA, and PSA) via the double enzymatic signal amplifications in the presence of a target antigen, ultimately leading to desired diagnostic accuracy and reliability. The addition of multiple horseradish peroxidase (HRP)- and antibody-labeled nanoparticles greatly amplified the signal and simplified the measurement of cancer biomarker proteins by sequentially magnifying electrochemical and colorimetric signals in a single platform. The two parallel assays performed using the proposed immunosensor have yielded highly consistent and reproducible results. Additionally, for the analysis of plasma samples in a clinical setting, the values obtained with our immunosensor were validated by correlating the results with those of a standard radioimmunoassay (RIA), which obtained very similar clinically valid responses. Copyright © 2016 Elsevier B.V. All rights reserved.

Surface roughness measurement in the submicrometer range using laser scattering

NASA Astrophysics Data System (ADS)

Wang, S. H.; Quan, Chenggen; Tay, C. J.; Shang, H. M.

2000-06-01

A technique for measuring surface roughness in the submicrometer range is developed. The principle of the method is based on laser scattering from a rough surface. A telecentric optical setup that uses a laser diode as a light source is used to record the light field scattered from the surface of a rough object. The light intensity distribution of the scattered band, which is correlated to the surface roughness, is recorded by a linear photodiode array and analyzed using a single-chip microcomputer. Several sets of test surfaces prepared by different machining processes are measured and a method for the evaluation of surface roughness is proposed.

Preparation of Ni3B2O6 nanosheet-based flowerlike architecture by a precursor method and its electrochemical properties in lithium-ion battery

NASA Astrophysics Data System (ADS)

Liang, Pan; Du, Lu; Wang, Xia; Liu, Zhi-Hong

2014-11-01

A novel flower-like nickel borate of Ni3B2O6 nanostructure was prepared through a hydrothermal treatment and sequential thermal decomposition of precursor without employing any template or surfactant. All the samples were characterized by XRD, IR, XPS, TG-DTA, nitrogen adsorption, SEM and TEM. The flower-like Ni3B2O6 nanostructure was self-assembled by nanosheets with the thickness of about 40 nm. The electrochemical properties in lithium-ion battery of flower-like Ni3B2O6 nanostructure were studied by the cyclic voltammetry, galvanostatic cycling test, and electrochemical impedance spectroscopy, which showed it had a high initial discharge capacity and a good reversibility.

Preparation of electrochemically active silicon nanotubes in highly ordered arrays

PubMed Central

Grünzel, Tobias; Lee, Young Joo; Kuepper, Karsten

2013-01-01

Summary Silicon as the negative electrode material of lithium ion batteries has a very large capacity, the exploitation of which is impeded by the volume changes taking place upon electrochemical cycling. A Si electrode displaying a controlled porosity could circumvent the difficulty. In this perspective, we present a preparative method that yields ordered arrays of electrochemically competent silicon nanotubes. The method is based on the atomic layer deposition of silicon dioxide onto the pore walls of an anodic alumina template, followed by a thermal reduction with lithium vapor. This thermal reduction is quantitative, homogeneous over macroscopic samples, and it yields amorphous silicon and lithium oxide, at the exclusion of any lithium silicides. The reaction is characterized by spectroscopic ellipsometry for thin silica films, and by nuclear magnetic resonance and X-ray photoelectron spectroscopy for nanoporous samples. After removal of the lithium oxide byproduct, the silicon nanotubes can be contacted electrically. In a lithium ion electrolyte, they then display the electrochemical waves also observed for other bulk or nanostructured silicon systems. The method established here paves the way for systematic investigations of how the electrochemical properties (capacity, charge/discharge rates, cyclability) of nanoporous silicon negative lithium ion battery electrode materials depend on the geometry. PMID:24205460

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

NASA Astrophysics Data System (ADS)

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.

MOF-derived Cu-Pd/nanoporous carbon composite as an efficient catalyst for hydrogen evolution reaction: A comparison between hydrothermal and electrochemical synthesis

NASA Astrophysics Data System (ADS)

Mandegarzad, Sakineh; Raoof, Jahan Bakhsh; Hosseini, Sayed Reza; Ojani, Reza

2018-04-01

In this study, a novel catalyst based on Cu-Pd bimetallic nanoparticles supported on nanoporous carbon composite (NPCC) is successfully fabricated through three-step process and used as an electrocatalyst towards hydrogen evolution reaction (HER). At the first step, MOF-199 is synthesized via two distinct strategies; (1) hydrothermal (HT) and (2) electrochemical (EC). Next, the synthesized MOF-199 is used as a template in order to prepare Cu/NPCC by direct carbonization under N2 atmosphere followed by galvanic replacement reaction of Cu metals by PdII ions. All the prepared materials are characterized by X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM), and nitrogen adsorption/desorption measurements. The effect of synthesis method of MOF-199 on the electrocatalytic activity of the final product towards HER is investigated. The electrochemical measurements indicate that Cu-Pd/NPCC derived from the MOF prepared by EC method (Cu-Pd/NPCC/EC) exhibits an enhanced catalytic activity towards HER in H2SO4 solution than the Cu-Pd/NPCC/HT. This improvement may be attributed to using of supporting electrolyte in the preparation of Cu-Pd/NPCC/EC.

Synthesis and electrochemical property of few-layer molybdenum disulfide nanosheets

NASA Astrophysics Data System (ADS)

Fu, Yanjue; Wang, Chunrui; Wang, Linlin; Peng, Xia; Wu, Binhe; Sun, Xingqu; Chen, Xiaoshuang

2016-12-01

Large-scale few-layer MoS2 nanosheets have been fabricated via a simple hydrothermal route using molybdenum powder as precursors. The as-prepared MoS2 samples were characterized by X-ray powder diffraction (XRD) analysis, transmission electron microscopy (TEM), and Raman and photoluminescence (PL) spectral analyses at room temperature. The results confirm that the as-prepared MoS2 displays a sheet-like morphology with a thickness of few (bi- to tri-) layers. Electrochemical measurements showed that the as-prepared few-layer MoS2 exhibited the highest reversible capacity of 1127 mAh g-1 and a stable reversible capacity of 1057 mAh g-1 after 30 cycles.

Studies on the preparation of Caro’s acid by ultrasonic enhanced electrochemistry

NASA Astrophysics Data System (ADS)

Li, Linbo; Yu, Zeli; Hong, Tao; Fang, Zhao; Peng, Jishi; Yang, Zhao

2017-06-01

Ultrasonic cavitation effects can generate hydroxyl radicals and high energy, which is widely applied in the field of oxidation currently. Ultrasound-enhanced electrochemical is used to prepare Caro’s acid, which improves the generate rate of Caro’s acid. In this article, the influences of ultrasonic frequency and ultrasonic power on the electrolysis voltage, electrolyte temperature, electrolyte concentration and the concentration of additive in the process of electrochemical preparation of Caro’s acid was studied. And the optimal production conditions were determined. The research results showed that ultrasonic can significantly improve the production of Caro’s acid and the product can increase by about 20 g/L under the best condition.

Elaboration and use of nickel planar macrocyclic complex-based sensors for the direct electrochemical measurement of nitric oxide in biological media.

PubMed

Bedioui, F; Trevin, S; Devynck, J; Lantoine, F; Brunet, A; Devynck, M A

1997-01-01

We describe here the electrochemical detection of nitric oxide, NO, in biological systems by using chemically modified ultramicro carbon electrodes. In the first part of the paper, the different steps involved in the electrochemical preparation and characterization of the nickel-based sensor are described. This is illustrated by the use of nickel(II) tetrasulfonated phthalocyanine complex. The second part of the paper describes two examples of the direct electrochemical measurement of NO production in human blood platelets and endothelial cells from umbilical cord vein.

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

PubMed

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

2014-09-01

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

Preparation of silver nanoparticles/graphene nanosheets as a catalyst for electrochemical oxidation of methanol

DOE Office of Scientific and Technical Information (OSTI.GOV)

Han, Kun; Miao, Peng; Tang, Yuguo, E-mail: tangyg@sibet.ac.cn

2014-02-03

In this report, silver nanoparticles (AgNPs) decorated graphene nanosheets have been prepared based on the reduction of Ag ions by hydroquinone, and their catalytic performance towards the electrochemical oxidation of methanol is investigated. The synthesis of the nano-composite is confirmed by transmission electron microscope measurements and UV-vis absorption spectra. Excellent electrocatalytic performance of the material is demonstrated by cyclic voltammograms. This material also contributes to the low peak potential of methanol oxidation compared with most of the other materials.

Total synthesis of TMG-chitotriomycin based on an automated electrochemical assembly of a disaccharide building block.

PubMed

Isoda, Yuta; Sasaki, Norihiko; Kitamura, Kei; Takahashi, Shuji; Manmode, Sujit; Takeda-Okuda, Naoko; Tamura, Jun-Ichi; Nokami, Toshiki; Itoh, Toshiyuki

2017-01-01

The total synthesis of TMG-chitotriomycin using an automated electrochemical synthesizer for the assembly of carbohydrate building blocks is demonstrated. We have successfully prepared a precursor of TMG-chitotriomycin, which is a structurally-pure tetrasaccharide with typical protecting groups, through the methodology of automated electrochemical solution-phase synthesis developed by us. The synthesis of structurally well-defined TMG-chitotriomycin has been accomplished in 10-steps from a disaccharide building block.

Development of the Electrochemical Biosensor for Organophosphate Chemicals Using CNT/Ionic Liquid Bucky Gel Electrode

DTIC Science & Technology

2010-04-01

www.elsevier .com/locate /e lecomDevelopment of the electrochemical biosensor for organophosphate chemicals using CNT/ ionic liquid bucky gel electrode Bong...hydrolase Ionic liquid CNT Electrochemical property1388-2481/$ - see front matter 2009 Elsevier B.V. A doi:10.1016/j.elecom.2009.01.006 * Corresponding...kaist.ac.kr (S.Y. Lee), whhOrganophosphorus hydrolase (OPH) immobilized on CNT/ ionic liquid (IL) electrodes were prepared by using three different intrinsic

Ferrocene conjugated oligonucleotide for electrochemical detection of DNA base mismatch.

PubMed

Hasegawa, Yusuke; Takada, Tadao; Nakamura, Mitsunobu; Yamana, Kazushige

2017-08-01

We describe the synthesis, binding, and electrochemical properties of ferrocene-conjugated oligonucleotides (Fc-oligos). The key step for the preparation of Fc-oligos contains the coupling of vinylferrocene to 5-iododeoxyuridine via Heck reaction. The Fc-conjugated deoxyuridine phosphoramidite was used in the Fc-oligonucleotide synthesis. We show that thiol-modified Fc-oligos deposited onto gold electrodes possess potential ability in electrochemical detection of DNA base mismatch. Copyright © 2017 Elsevier Ltd. All rights reserved.

Synthesis of hetero compounds using dialkylcarbonate quaternation

DOEpatents

Friesen, Cody A.; Wolfe, Derek; Johnson, Paul Bryan

2017-10-17

Methods of preparing hetero ionic complexes, and ionic liquids from bisulfate salts of heteroatomic compounds using dialkylcarbonates as a primary quaternizing reactant are disclosed. Also disclosed are methods of making electrochemical cells comprising the ionic liquids, and an electrochemical cell comprising an alkaline electrolyte and a hetero ionic complex additive.

Electrochemical Cell with Improved Water or Gas Management

NASA Technical Reports Server (NTRS)

LaGrange, Jay W. (Inventor); Smith, William F. (Inventor); McElroy, James F. (Inventor)

2015-01-01

An electrochemical cell having a water/gas porous separator prepared from a polymeric material and one or more conductive cell components that pass through, or are located in close proximity to, the water/gas porous separator, is provided. The inventive cell provides a high level of in-cell electrical conductivity.

Synthesis of hetero ionic compounds using dialkylcarbonate quaternization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Friesen, Cody A.; Wolfe, Derek; Johnson, Paul Bryan

2017-09-19

Methods of preparing hetero ionic complexes, and ionic liquids from bisulfate salts of heteroatomic compounds using dialkylcarbonates as a primary quaternizing reactant are disclosed. Also disclosed are methods of making electrochemical cells comprising the ionic liquids, and an electrochemical cell comprising an alkaline electrolyte and a hetero ionic complex additive.

Synthesis of hetero ionic compounds using dialkylcarbonate quaternization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Friesen, Cody A.; Wolfe, Derek; Johnson, Paul Bryan

2018-04-03

Methods of preparing hetero ionic complexes, and ionic liquids from bisulfate salts of heteroatomic compounds using dialkylcarbonates as a primary quaternizing reactant are disclosed. Also disclosed are methods of making electrochemical cells comprising the ionic liquids, and an electrochemical cell comprising an alkaline electrolyte and a hetero ionic complex additive.

Measuring Skew in Average Surface Roughness as a Function of Surface Preparation

NASA Technical Reports Server (NTRS)

Stahl, Mark

2015-01-01

Characterizing surface roughness is important for predicting optical performance. Better measurement of surface roughness reduces polishing time, saves money and allows the science requirements to be better defined. This study characterized statistics of average surface roughness as a function of polishing time. Average surface roughness was measured at 81 locations using a Zygo white light interferometer at regular intervals during the polishing process. Each data set was fit to a normal and Largest Extreme Value (LEV) distribution; then tested for goodness of fit. We show that the skew in the average data changes as a function of polishing time.

Cemented fixation with PMMA or Bis-GMA resin hydroxyapatite cement: effect of implant surface roughness.

PubMed

Walsh, W R; Svehla, M J; Russell, J; Saito, M; Nakashima, T; Gillies, R M; Bruce, W; Hori, R

2004-09-01

Implant surface roughness is an important parameter governing the overall mechanical properties at the implant-cement interface. This study investigated the influence of surface roughness using polymethylmethcrylate (PMMA) and a Bisphenol-a-glycidylmethacyrlate resin-hydroxyapatite cement (CAP). Mechanical fixation at the implant-cement interface was evaluated in vitro using static shear and fatigue loading with cobalt chrome alloy (CoCr) dowels with different surface roughness preparations. Increasing surface roughness improved the mechanical properties at the implant-cement interface for both types of cement. CAP cement fixation was superior to PMMA under static and dynamic loading.

Electrochemical surface modification of titanium in dentistry.

PubMed

Kim, Kyo-Han; Ramaswamy, Narayanan

2009-01-01

Titanium and its alloys have good biocompatibility with body cells and tissues and are widely used for implant applications. However, clinical procedures place more stringent and tough requirements on the titanium surface necessitating artificial surface treatments. Among the many methods of titanium surface modification, electrochemical techniques are simple and cheap. Anodic oxidation is the anodic electrochemical technique while electrophoretic and cathodic depositions are the cathodic electrochemical techniques. By anodic oxidation it is possible to obtain desired roughness, porosity and chemical composition of the oxide. Anodic oxidation at high voltages can improve the crystallinity of the oxide. The chief advantage of this technique is doping of the coating of the bath constituents and incorporation of these elements improves the properties of the oxide. Electrophoretic deposition uses hydroxyapatite (HA) powders dispersed in a suitable solvent at a particular pH. Under these operating conditions these particles acquire positive charge and coatings are obtained on the cathodic titanium by applying an external electric field. These coatings require a post-sintering treatment to improve the coating properties. Cathodic deposition is another type of electrochemical method where HA is formed in situ from an electrolyte containing calcium and phosphate ions. It is also possible to alter structure and/or chemistry of the obtained deposit. Nano-grained HA has higher surface energy and greater biological activity and therefore emphasis is being laid to produce these coatings by cathodic deposition.

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

PubMed Central

Choi, Woong-Kirl; Kim, Seong-Hyun; Choi, Seung-Geon; Lee, Eun-Sang

2018-01-01

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. PMID:29351235

Preparation of anticoagulant PyC biomaterials with super-hydrophobic surface.

PubMed

Ze, Wang; Wen-Sheng, Tan; Ye-Xia; Ming, Zhang; Xiao-Ping, Li; Jian-Guo, Qiu; Xiao-Hong, Yang

2018-01-01

Pyrolytic carbon (PyC) is a kind of biomaterial which is chemically inert and has excellent biocompatibility. In order to obtain a super-hydrophobic PyC surface to improve anticoagulation and inhibit thrombus, this study prepares grating pair structure, microhole array structure, helix structure on PyC surface by nanoseconds laser etching. Rod-like ZnO film and ball-like ZnO film are prepared on the PyC surface by the hydrothermal method; polyvinyl pyrrolidone (PVP) nanofiber film and PVP/TiO 2 complex nanofiber film are prepared on the PyC surface by the electrospinning method; the PyC surface is silanized. Finally, surface microstructure and surface energy are characterized by scanning electron microscopy and contact angle meter (OCA20, German DataPhysics Co.). The periodical microstructures are formed respectively by nanoseconds laser etching. The surface roughness is increased by the hydrothermal and electrospinning method. Through infiltration experiment on rough and smooth PyC surfaces, rough PyC surface with microstructure is super-hydrophobic and has greater than 150° contact angle, which decreases blood flow resistance and inhibits thrombus.

Rupture preparation process controlled by surface roughness on meter-scale laboratory fault

NASA Astrophysics Data System (ADS)

Yamashita, Futoshi; Fukuyama, Eiichi; Xu, Shiqing; Mizoguchi, Kazuo; Kawakata, Hironori; Takizawa, Shigeru

2018-05-01

We investigate the effect of fault surface roughness on rupture preparation characteristics using meter-scale metagabbro specimens. We repeatedly conducted the experiments with the same pair of rock specimens to make the fault surface rough. We obtained three experimental results under the same experimental conditions (6.7 MPa of normal stress and 0.01 mm/s of loading rate) but at different roughness conditions (smooth, moderately roughened, and heavily roughened). During each experiment, we observed many stick-slip events preceded by precursory slow slip. We investigated when and where slow slip initiated by using the strain gauge data processed by the Kalman filter algorithm. The observed rupture preparation processes on the smooth fault (i.e. the first experiment among the three) showed high repeatability of the spatiotemporal distributions of slow slip initiation. Local stress measurements revealed that slow slip initiated around the region where the ratio of shear to normal stress (τ/σ) was the highest as expected from finite element method (FEM) modeling. However, the exact location of slow slip initiation was where τ/σ became locally minimum, probably due to the frictional heterogeneity. In the experiment on the moderately roughened fault, some irregular events were observed, though the basic characteristics of other regular events were similar to those on the smooth fault. Local stress data revealed that the spatiotemporal characteristics of slow slip initiation and the resulting τ/σ drop for irregular events were different from those for regular ones even under similar stress conditions. On the heavily roughened fault, the location of slow slip initiation was not consistent with τ/σ anymore because of the highly heterogeneous static friction on the fault, which also decreased the repeatability of spatiotemporal distributions of slow slip initiation. These results suggest that fault surface roughness strongly controls the rupture preparation process, and generally increases its complexity with the degree of roughness.

Structural and electrochemical properties of Gd-doped Li4Ti5O12 as anode material with improved rate capability for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Zhang, Qianyu; Verde, Michael G.; Seo, Joon Kyo; Li, Xi; Meng, Y. Shirley

2015-04-01

Pristine and Gd-doped Li4Ti5O12 (LTO) in the form of Li4-x/3Ti5-2x/3GdxO12 (x = 0.05, 0.10 and 0.15) were prepared by a simple solid-state reaction in air. The structural and electrochemical properties of the as-prepared powders were characterized using X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). XRD revealed that only a small amount of the dopant can enter the lattice structure of LTO; excessive addition beyond x = 0.10 resulted in a discrete Gd2O3 impurity phase. The Gd doping did not change the spinel structure and electrochemical reaction process of LTO. The average particle size of as-prepared samples ranged between 0.5 and 1.5 μm. The Gd-doped materials showed much improved rate capability and specific capacity compared with undoped LTO. In particular, Li4-x/3Ti5-2x/3GdxO12 (x = 0.5) exhibited the best rate capability and cycling stability among all samples. Beyond this doping level, however, Gd2O3 impurity phase in the LTO led to adverse electrochemical performance. The rate capability of the anode material made from the modified powder is significantly improved when discharged at high current rates due to the reduced charge transfer resistance and fast lithium insertion/extraction kinetics.

High performance and durability of order-structured cathode catalyst layer based on TiO2@PANI core-shell nanowire arrays

NASA Astrophysics Data System (ADS)

Chen, Ming; Wang, Meng; Yang, Zhaoyi; Wang, Xindong

2017-06-01

In this paper, an order-structured cathode catalyst layer consisting of Pt-TiO2@PANI core-shell nanowire arrays that in situ grown on commercial gas diffusion layer (GDL) are prepared and applied to membrane electrode assembly (MEA) of proton exchange membrane fuel cell (PEMFC). In order to prepare the TiO2@PANI core-shell nanowire arrays with suitable porosity and prominent conductivity, the morphologies of the TiO2 nanoarray and electrochemical polymerization process of aniline are schematically investigated. The MEA with order-structured cathode catalyst layer is assembled in the single cell to evaluate the electrochemical performance and durability of PEMFC. As a result, the PEMFC with order-structured cathode catalyst layer shows higher peak power density (773.54 mW cm-2) than conventional PEMFC (699.30 mW cm-2). Electrochemically active surface area (ECSA) and charge transfer impedance (Rct) are measured before and after accelerated degradation test (ADT), and the corresponding experimental results indicate the novel cathode structure exhibits a better stability with respect to conventional cathode. The enhanced electrochemical performance and durability toward PEMFC can be ascribed to the order-structured cathode nanoarray structure with high specific surface area increases the utilization of catalyst and reduces the tortuosity of transport pathways, and the synergistic effect between TiO2@PANI support and Pt nanoparticles promotes the high efficiency of electrochemical reaction and improves the stability of catalyst. This research provides a facile and controllable method to prepare order-structured membrane electrode with lower Pt loading for PEMFC in the future.

Effect of grit-blasting on substrate roughness and coating adhesion

NASA Astrophysics Data System (ADS)

Varacalle, Dominic J.; Guillen, Donna Post; Deason, Douglas M.; Rhodaberger, William; Sampson, Elliott

2006-09-01

Statistically designed experiments were performed to compare the surface roughness produced by grit blasting A36/1020 steel using different abrasives. Grit blast media, blast pressure, and working distance were varied using a Box-type statistical design of experiment (SDE) approach. The surface textures produced by four metal grits (HG16, HG18, HG25, and HG40) and three conventional grits (copper slag, coal slag, and chilled iron) were compared. Substrate roughness was measured using surface profilometry and correlated with operating parameters. The HG16 grit produced the highest surface roughness of all the grits tested. Aluminum and zinc-aluminum coatings were deposited on the grit-blasted substrates using the twin-wire electric are (TWEA) process. Bond strength of the coatings was measured with a portable adhesion tester in accordance with ASTM standard D 4541. The coatings on substrates roughened with steel grit exhibit superior bond strength to those prepared with conventional grit. For aluminum coatings sprayed onto surfaces prepared with the HG16 grit, the bond strength was most influenced by current, spray distance, and spray gun pressure (in that order). The highest bond strength for the zinc-aluminum coatings was attained on surfaces prepared using the metal grits.

Formation of different micro-morphologies from VO2 and ZnO crystallization using macro-porous silicon substrates

NASA Astrophysics Data System (ADS)

Salazar-Kuri, U.; Antúnez, E. E.; Estevez, J. O.; Olive-Méndez, Sion F.; Silva-González, N. R.; Agarwal, V.

2017-05-01

Square-shaped macropores produced by electrochemical anodization of n- and p-type Si wafers have been used as centers of nucleation to crystallize VO2 and ZnO. Substrate roughness dependent formation of different morphologies is revealed in the form of squared particles, spheres, bars and ribbons in the case of VO2 and hexagonal piles and spheres in the case of ZnO, have been observed.The presence of nano-/micro-metric crystals was studied through field emission scanning electron microscopy and energy dispersive X-ray spectroscopy mapping. Crystal structure of metal oxides was confirmed by micro-Raman spectroscopy. The growth of the different morphologies has been explained in terms of the surface free energy of a bare Si/SiO2 substrate and its modification originated from the roughness of the surface and of the walls of the porous substrates. This energy plays a crucial role on the minimization of the required energy to induce heterogeneous nucleation and crystal growth. Present work strengthens and provides an experimental evidence of roughness dependent metal oxide crystal growth with well-defined habits from pore corners and rough sides of the pore walls, similar to already reported protein crystals.

Graphene as a signal amplifier for preparation of ultrasensitive electrochemical biosensors.

PubMed

Filip, Jaroslav; Kasák, Peter; Tkac, Jan

2015-01-01

Early diagnostics of diseases performed with minimal money and time consumption has become achievable due to recent advances in development of biosensors. These devices use biorecognition elements for selective interaction with an analyte and signal readout is obtained via different types of transducers. Operational characteristics of biosensors have been reported to improve substantially, when a diverse range of nanomaterials was employed. This review presents construction of electrochemical biosensors based on graphene, atomically thin 2D carbon crystals, which is currently intensively studied nanomaterial. The most attractive directions of graphene applications in biosensor preparation are discussed here including novel detection and amplification schemes exploiting graphene's unique electrochemical, physical and chemical properties. The future of graphene-based biosensors is most likely bright, but there is still a lot of work to do to fulfill high expectations.

Covalent organic framework-derived microporous carbon nanoparticles coated with conducting polypyrrole as an electrochemical capacitor

NASA Astrophysics Data System (ADS)

Kim, Dong Jun; Yoon, Jung Woon; Lee, Chang Soo; Bae, Youn-Sang; Kim, Jong Hak

2018-05-01

We report a high-performance electrochemical capacitor based on covalent organic framework (COF)-derived microporous carbon (MPC) nanoparticles and electrochemically polymerized polypyrrole (Ppy) as a pseudocapacitive material. The COF, Schiff-based network-1 (SNW-1) nanoparticles are prepared via a condensation reaction between melamine and terephthalaldehyde, and the resultant MPC film is prepared via a screen-printing method. The MPC film exhibits a bimodal porous structure with micropores and macropores, resulting in both a large surface area and good electrolyte infiltration. Ppy is synthesized potentio-statically (0.8 V vs. Ag/AgCl) by varying the reaction time, and successful synthesis of Ppy is confirmed via Raman spectroscopy. The specific capacitance with the Ppy coating is enhanced by up to 2.55 F cm-2 due to the synergetic effect of pseudocapacitance and reduced resistance.

Crystal structure and electrochemical properties of rare earth non-stoichiometric AB5-type alloy as negative electrode material in Ni-MH battery

NASA Astrophysics Data System (ADS)

Zhang, Xinbo; Chai, Yujun; Yin, Wenya; Zhao, Minshou

2004-07-01

The La 0.85Mg xNi 4.5Co 0.35Al 0.15 (0.05⩽ x⩽0.35) system compounds have been prepared by arc melting method under Ar atmosphere. X-ray diffraction (XRD) analysis reveals that the as-prepared alloys have different lattice parameters and cell volumes. The electrochemical properties of these alloys have been studied through the charge-discharge recycle testing at different temperatures and discharge currents. It is found that the La 0.85Mg 0.25Ni 4.5Co 0.35Al 0.15 alloy electrode is capable of performing high-rate discharge. Moreover, it has very excellent electrochemical properties as negative electrode materials in Ni-MH battery at low temperature, even at -40°C.

Diazonium-functionalized horseradish peroxidase immobilized via addressable electrodeposition: direct electron transfer and electrochemical detection.

PubMed

Polsky, Ronen; Harper, Jason C; Dirk, Shawn M; Arango, Dulce C; Wheeler, David R; Brozik, Susan M

2007-01-16

A simple one-step procedure is introduced for the preparation of diazonium-enzyme adducts. The direct electrically addressable deposition of diazonium-modified enzymes is examined for electrochemical sensor applications. The deposition of diazonium-horseradish peroxidase leads to the direct electron transfer between the enzyme and electrode exhibiting a heterogeneous rate constant, ks, of 10.3 +/- 0.7 s-1 and a DeltaEp of 8 mV (v = 150 mV/s). The large ks and low DeltaEp are attributed to the intimate contact between enzyme and electrode attached by one to three phenyl molecules. Such an electrode shows high nonmediated catalytic activity toward H2O2 reduction. Future generations of arrayed electrochemical sensors and studies of direct electron transfer of enzymes can benefit from protein electrodes prepared by this method.

Investigation on the electrochemical interfacial properties of 2-aminothiophenol functionalized graphene oxide modified electrode

NASA Astrophysics Data System (ADS)

Immanuel, Susan; Aparna T., K.; Sivasubramanian, R.

2018-04-01

In this paper the interfacial behavior of graphene oxide and 2-aminothiophenol functionalized graphene oxide was investigated by electrochemical method. The GO was prepared by modified Hummers method and the 2-aminothiophenol was covalently attached on the surface of GO sheets. The electrochemical properties were investigated using a redox couple and the electrokinetic parameter was inferred. It was found that the ATP-GO exhibited slow kinetics compared to GO due to the increased deformation of GO sheets after ATP functionalization.

Total synthesis of TMG-chitotriomycin based on an automated electrochemical assembly of a disaccharide building block

PubMed Central

Isoda, Yuta; Sasaki, Norihiko; Kitamura, Kei; Takahashi, Shuji; Manmode, Sujit; Takeda-Okuda, Naoko; Tamura, Jun-ichi

2017-01-01

The total synthesis of TMG-chitotriomycin using an automated electrochemical synthesizer for the assembly of carbohydrate building blocks is demonstrated. We have successfully prepared a precursor of TMG-chitotriomycin, which is a structurally-pure tetrasaccharide with typical protecting groups, through the methodology of automated electrochemical solution-phase synthesis developed by us. The synthesis of structurally well-defined TMG-chitotriomycin has been accomplished in 10-steps from a disaccharide building block. PMID:28684973

Electrochemical synthesis of gold nanoparticles on the surface of multi-walled carbon nanotubes with glassy carbon electrode and their application

NASA Astrophysics Data System (ADS)

Song, Y. Z.; Li, X.; Song, Y.; Cheng, Z. P.; Zhong, H.; Xu, J. M.; Lu, J. S.; Wei, C. G.; Zhu, A. F.; Wu, F. Y.; Xu, J.

2013-01-01

Gold nanoparticles on the surface of multi-walled carbon nanotubes with glassy carbon electrode were prepared using electrochemical synthesis method. The thin films of gold Nanoparticles/multi-walled carbon nanotubes were characterized by scanning electron microscopy, powder X-ray diffraction, and cyclic voltammetry. Electrochemical behavior of adrenaline hydrochloride at gold nanoparticles/multi-walled carbon nanotube modified glassy carbon electrode was investigated. A simple, sensitive, and inexpensive method for determination of adrenaline hydrochloride was proposed.

Studies on activated carbon derived from neem (azadirachta indica) bio-waste, and its application as supercapacitor electrode

NASA Astrophysics Data System (ADS)

Ahmed, Sultan; Parvaz, M.; Johari, Rahul; Rafat, M.

2018-04-01

The present study reports the preparation of quasi solid-state supercapacitor employing activated carbon (AC) electrodes and gel polymer electrolyte (GPE). AC was derived from Neem leaves by means of chemical activation using zinc chloride as activating agent. GPE was prepared using solution-cast technique and comprises of LiClO 4 salt, dispersed in EC:PC (1:1 vol.) and entrapped in PVdF-HFP solution. Extensive physical and electrochemical characterization of synthesized AC and GPE was done. AC was characterized using the techniques of SEM, TEM, XRD, Raman spectroscopy, TGA and BET tests while GPE was characterized by electrochemical stability window (ESW) and conductivity test. The fabricated supercapacitor cell was tested using standard electrochemical characterization techniques. It was found that the fabricated cell offers high values of specific capacitance (74.41 F g‑1), specific energy (10.33 Wh kg‑1) and specific power (4.66 kW kg‑1). These results demonstrate the suitability of prepared AC as promising electrode material for supercapacitor applications.

Spray pyrolysed Ru:TiO2 thin film electrodes prepared for electrochemical supercapacitor

NASA Astrophysics Data System (ADS)

Fugare, B. Y.; Thakur, A. V.; Kore, R. M.; Lokhande, B. J.

2018-04-01

Ru doped TiO2 thin films are prepared by using 0.06 M aqueous solution of potassium titanium oxalate (pto), and 0.005 M aqueous solution of ruthenium tri chloride (RuCl3) precursors. The deposition was carried on stainless steel (SS) by using well known ultrasonic spray pyrolysis technique (USPT) at 723° K by maintaining the spray rate 12 cc/min and compressed air flow rate 10 Lmin-1. Prepared Ru:TiO2 thin films were characterized by structurally, morphologically and electrochemically. Deposited RuO2 shows amorphous structure and TiO2 shows tetragonal crystal structure with rutile as prominent phase at very low decomposition temperature. SEM micrographs of RuO2 exhibits porous, interconnected, spherical grains type morphology and TiO2 shows porous, nanorods and nanoplates like morphology and also Ru doped TiO2 shows porous, spherical, granular and nanorods type morphology. The electrochemical cyclic voltammetery shows mixed capacitive behavior. The achieved highest value of specific capacitance 2692 F/g was Ru doped TiO2 electrode in 0.5 M H2SO4.

Poly(3,4-ethylenedioxythiophene)/reduced graphene oxide composites as counter electrodes for high efficiency dye-sensitized solar cells

NASA Astrophysics Data System (ADS)

Ma, Jinfu; Yuan, Shenghua; Yang, Shaolin; Lu, Hui; Li, Yingtao

2018-05-01

A facile, low cost, easy-controllable method to prepare Poly(3,4-ethylenedioxythiophene) (PEDOT)/reduced graphene oxide (rGO) composites by electrochemical deposition onto fluorinated tin oxide (FTO) as counter electrodes (CEs) in high performance dye-sensitized solar cells (DSSCs) is reported. The electro-deposition process was accomplished by electro-polymerization of graphene oxide (GO)/PEDOT composites onto FTO substrates followed by electrochemical reduction of the GO component. Electrochemical measurements show that the I-/I3- catalytic activity of the as-prepared PEDOT/rGO CE is improved compared with that of the pure PEDOT and PEDOT/GO electrode. Through the analysis of photoelectric properties, the performance of the electrodes fabricated with different polymerization times are compared, and the optimal preparation condition is determined. The photoelectric conversion efficiency (PCE) of the DSSC assembled with PEDOT/rGO electrode reaches 7.79%, close to 8.33% of the cell with Platinum (Pt) electrode, and increases by 13.2% compared with 6.88% of the device with the PEDOT electrode.

Plasma surface modification of polypropylene track-etched membrane to improve its performance properties

NASA Astrophysics Data System (ADS)

Kravets, L. I.; Elinson, V. M.; Ibragimov, R. G.; Mitu, B.; Dinescu, G.

2018-02-01

The surface and electrochemical properties of polypropylene track-etched membrane treated by plasma of nitrogen, air and oxygen are studied. The effect of the plasma-forming gas composition on the surface morphology is considered. It has been found that the micro-relief of the membrane surface formed under the gas-discharge etching, changes. Moreover, the effect of the non-polymerizing gas plasma leads to formation of oxygen-containing functional groups, mostly carbonyl and carboxyl. It is shown that due to the formation of polar groups on the surface and its higher roughness, the wettability of the plasma-modified membranes improves. In addition, the presence of polar groups on the membrane surface layer modifies its electrochemical properties so that conductivity of plasma-treated membranes increase.

Recent Advances in Voltammetry

PubMed Central

Batchelor-McAuley, Christopher; Kätelhön, Enno; Barnes, Edward O; Compton, Richard G; Laborda, Eduardo; Molina, Angela

2015-01-01

Recent progress in the theory and practice of voltammetry is surveyed and evaluated. The transformation over the last decade of the level of modelling and simulation of experiments has realised major advances such that electrochemical techniques can be fully developed and applied to real chemical problems of distinct complexity. This review focuses on the topic areas of: multistep electrochemical processes, voltammetry in ionic liquids, the development and interpretation of theories of electron transfer (Butler–Volmer and Marcus–Hush), advances in voltammetric pulse techniques, stochastic random walk models of diffusion, the influence of migration under conditions of low support, voltammetry at rough and porous electrodes, and nanoparticle electrochemistry. The review of the latter field encompasses both the study of nanoparticle-modified electrodes, including stripping voltammetry and the new technique of ‘nano-impacts’. PMID:26246984

Method of preparing an electrochemical cell in uncharged state

DOEpatents

Shimotake, Hiroshi; Bartholme, Louis G.; Arntzen, John D.

1977-02-01

A secondary electrochemical cell is assembled in an uncharged state for the preparation of a lithium alloy-transition metal sulfide cell. The negative electrode includes a material such as aluminum or silicon for alloying with lithium as the cell is charged. The positive electrode is prepared by blending particulate lithium sulfide, transition metal powder and electrolytic salt in solid phase. The mixture is simultaneously heated to a temperature in excess of the melting point of the electrolyte and pressed onto an electrically conductive substrate to form a plaque. The plaque is assembled as a positive electrode within the cell. During the first charge cycle lithium alloy is formed within the negative electrode and transition metal sulfide such as iron sulfide is produced within the positive electrode.

Preparation of a DNA matrix via an electrochemically directed copolymerization of pyrrole and oligonucleotides bearing a pyrrole group.

PubMed Central

Livache, T; Roget, A; Dejean, E; Barthet, C; Bidan, G; Téoule, R

1994-01-01

A new methodology for the preparation of addressed DNA matrices is described. The process includes an electrochemically directed copolymerization of pyrrole and oligonucleotides bearing on their 5' end a pyrrole moiety introduced by phosphoramidite chemistry. The electro-controlled synthesis of the copolymer (poly-pyrrole) gives, in one step, a solid conducting film deposited on the surface of an electrode. The resulting polymer consists of pyrrole chains bearing covalently linked oligonucleotide. The polymer growth is limited to the electrode surface, so that it is possible to prepare a DNA matrix on a multiple electrode device by successive copolymerizations. A support bearing four oligonucleotides was used to detect three ras mutations on a synthetic DNA fragment. PMID:8065902

Method of preparing porous, rigid ceramic separators for an electrochemical cell

DOEpatents

Bandyopadhyay, Gautam; Dusek, Joseph T.

1981-01-01

Porous, rigid separators for electrochemical cells are prepared by first calcining particles of ceramic material at temperatures above about 1200.degree. C. for a sufficient period of time to reduce the sinterability of the particles. A ceramic powder that has not been calcined is blended with the original powder to control the porosity of the completed separator. The ceramic blend is then pressed into a sheet of the desired shape and sintered at a temperature somewhat lower than the calcination temperature. Separator sheets of about 1 to 2.5 mm thickness and 30 to 70% porosity can be prepared by this technique. Ceramics such as yttria, magnesium oxide and magnesium-aluminum oxide have advantageously been used to form separators by this method.

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

PubMed

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

2016-05-01

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

Ni-Co bimetal nanowires filled multiwalled carbon nanotubes for the highly sensitive and selective non-enzymatic glucose sensor applications

PubMed Central

Ramachandran, K.; Raj kumar, T.; Babu, K. Justice; Gnana kumar, G.

2016-01-01

The facile, time and cost efficient and environmental benign approach has been developed for the preparation of Nickel (Ni)-Cobalt (Co) alloy nanowires filled multiwalled carbon nanotubes (MWCNTs) with the aid of mesoporous silica nanoparticles (MSN)/Ni-Co catalyst. The controlled incorporation of Ni-Co nanostructures in the three dimensional (3D) pore structures of MSN yielded the catalytically active system for the MWCNT growth. The inner surface of MWCNTs was quasi-continuously filled with face-centered cubic (fcc) structured Ni-Co nanowires. The as-prepared nanostructures were exploited as non-enzymatic electrochemical sensor probes for the reliable detection of glucose. The electrochemical measurements illustrated that the fabricated sensor exhibited an excellent electrochemical performance toward glucose oxidation with a high sensitivity of 0.695 mA mM−1 cm−2, low detection limit of 1.2 μM, a wide linear range from 5 μM–10 mM and good selectivity. The unprecedented electrochemical performances obtained for the prepared nanocomposite are purely attributed to the synergistic effects of Ni-Co nanowires and MWCNTs. The constructed facile, selective and sensitive glucose sensor has also endowed its reliability in analyzing the human serum samples, which wide opened the new findings for exploring the novel nanostructures based glucose sensor devices with affordable cost and good stability. PMID:27833123

The relationship between structural stability and electrochemical performance of multi-element doped alpha nickel hydroxide

NASA Astrophysics Data System (ADS)

Miao, Chengcheng; Zhu, Yanjuan; Huang, Liangguo; Zhao, Tengqi

2015-01-01

The multi-element doped alpha nickel hydroxide has been prepared by supersonic co-precipitation method. Three kinds of samples A, B and C are prepared by chemically coprecipitating Ni/Al, Ni/Al/Mn and Ni/Al/Mn/Yb, respectively. Inductively coupled plasma atomic emission spectroscopy (ICP-AES), Particle size distribution (PSD) measurement, X-ray diffraction (XRD), scanning electron microscope (SEM) and Fourier transform infrared spectroscopy (FT-IR) are used to characterize the physical properties of the synthesized α-Ni(OH)2 samples, such as chemical composition, morphology, structural stability of the crystal. The results show that all samples are nano-sized materials and the interlayer spacing becomes larger and the structural stability becomes better with the increase of doped elements and doped ratio. The prepared alpha nickel hydroxide samples are added into micro-sized beta nickel hydroxide to form biphase electrode materials for Ni-MH battery. The electrochemical characterization of the biphase electrodes, including cyclic voltammetry (CV) and charge/discharge test, are also performed. The results demonstrate that the biphase electrode with sample C exhibits better electrochemical reversibility and cyclic stability, higher charge efficient and discharge potential, larger proton diffusion coefficient (5.81 × 10-12 cm2 s-1) and discharge capacity (309.0 mAh g-1). Hence, it indicates that all doped elements can produce the synergic effect and further improve the electrochemical properties of the alpha nickel hydroxide.

Ni-Co bimetal nanowires filled multiwalled carbon nanotubes for the highly sensitive and selective non-enzymatic glucose sensor applications

NASA Astrophysics Data System (ADS)

Ramachandran, K.; Raj Kumar, T.; Babu, K. Justice; Gnana Kumar, G.

2016-11-01

The facile, time and cost efficient and environmental benign approach has been developed for the preparation of Nickel (Ni)-Cobalt (Co) alloy nanowires filled multiwalled carbon nanotubes (MWCNTs) with the aid of mesoporous silica nanoparticles (MSN)/Ni-Co catalyst. The controlled incorporation of Ni-Co nanostructures in the three dimensional (3D) pore structures of MSN yielded the catalytically active system for the MWCNT growth. The inner surface of MWCNTs was quasi-continuously filled with face-centered cubic (fcc) structured Ni-Co nanowires. The as-prepared nanostructures were exploited as non-enzymatic electrochemical sensor probes for the reliable detection of glucose. The electrochemical measurements illustrated that the fabricated sensor exhibited an excellent electrochemical performance toward glucose oxidation with a high sensitivity of 0.695 mA mM-1 cm-2, low detection limit of 1.2 μM, a wide linear range from 5 μM-10 mM and good selectivity. The unprecedented electrochemical performances obtained for the prepared nanocomposite are purely attributed to the synergistic effects of Ni-Co nanowires and MWCNTs. The constructed facile, selective and sensitive glucose sensor has also endowed its reliability in analyzing the human serum samples, which wide opened the new findings for exploring the novel nanostructures based glucose sensor devices with affordable cost and good stability.

A simple and sensitive methodology for voltammetric determination of valproic acid in human blood plasma samples using 3-aminopropyletriethoxy silane coated magnetic nanoparticles modified pencil graphite electrode.

PubMed

Zabardasti, Abedin; Afrouzi, Hossein; Talemi, Rasoul Pourtaghavi

2017-07-01

In this work, we have prepared a nano-material modified pencil graphite electrode for the sensing of valproic acid (VA) by immobilization 3-aminopropyletriethoxy silane coated magnetic nanoparticles (APTES-MNPs) on the pencil graphite surface (PGE). Electrochemical studies indicated that the APTES-MNPs efficiently increased the electron transfer kinetics between VA and the electrode and the free NH 2 groups of the APTES on the outer surface of magnetic nanoparticles can interact with carboxyl groups of VA. Based on this, we have proposed a sensitive, rapid and convenient electrochemical method for VA determination. Under the optimized conditions, the reduction peak current of VA is found to be proportional to its concentration in the range of 1.0 (±0.2) to 100.0 (±0.3) ppm with a detection limit of 0.4 (±0.1) ppm. The whole sensor fabrication process was characterized by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) methods with using [Fe(CN) 6 ] 3-/4- as an electrochemical redox indicator. The prepared modified electrode showed several advantages such as high sensitivity, selectivity, ease of preparation and good repeatability, reproducibility and stability. The proposed method was applied to determination of valproic acid in blood plasma samples and the obtained results were satisfactory accurate. Copyright © 2017. Published by Elsevier B.V.

Method for the electro-addressable functionalization of electrode arrays

DOEpatents

Harper, Jason C.; Polsky, Ronen; Dirk, Shawn M.; Wheeler, David R.; Arango, Dulce C.; Brozik, Susan M.

2015-12-15

A method for preparing an electrochemical biosensor uses bias-assisted assembly of unreactive -onium molecules on an electrode array followed by post-assembly electro-addressable conversion of the unreactive group to a chemical or biological recognition group. Electro-addressable functionalization of electrode arrays enables the multi-target electrochemical sensing of biological and chemical analytes.

Preparation of Chemically Etched Tips for Ambient Instructional Scanning Tunneling Microscopy

ERIC Educational Resources Information Center

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

2010-01-01

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

Production of battery grade materials via an oxalate method

DOEpatents

Belharouak, Ilias; Amine, Khalil

2016-05-17

An active electrode material for electrochemical devices such as lithium ion batteries includes a lithium transition metal oxide which is free of sodium and sulfur contaminants. The lithium transition metal oxide is prepared by calcining a mixture of a lithium precursor and a transition metal oxalate. Electrochemical devices use such active electrodes.

Production of battery grade materials via an oxalate method

DOEpatents

Belharouak, Ilias; Amine, Khalil

2014-04-29

An active electrode material for electrochemical devices such as lithium ion batteries includes a lithium transition metal oxide which is free of sodium and sulfur contaminants. The lithium transition metal oxide is prepared by calcining a mixture of a lithium precursor and a transition metal oxalate. Electrochemical devices use such active electrodes.

In-situ synthesis of Co3O4/graphite nanocomposite for high-performance supercapacitor electrode applications

NASA Astrophysics Data System (ADS)

Gopalakrishnan, M.; Srikesh, G.; Mohan, A.; Arivazhagan, V.

2017-05-01

In this work, a low cost and pollution free in-situ synthesis of phase pure Co3O4 nanoparticles and Co3O4/graphite nanocomposite have been successfully developed via co-precipitation method followed by the thermal treatment process. The prepared samples were characterized by powder X-ray diffraction, scanning electron microscope, high resolution transmission electron microscope, Fourier Transform Infrared Spectroscopy and electrochemical measurements. Electrochemical measurements such as cyclic voltammetry, galvanostatic charge-discharge, electrochemical impedance spectroscopy were carried out in 6 M KOH aqueous electrolytic solution. The results show the excellent maximum specific capacitive behavior of 239.5 F g-1 for pure and 395.04 F g-1 for Co3O4/graphite nanocomposite at a current density of 0.5 A g-1. This composite exhibits a good cyclic stability, with a small loss of 2.68% of maximum capacitance over a consecutive 1000 cycles. The investigation indicates that the prepared electrode material could be a potential and promising candidate for electrochemical supercapacitors.

A facile electrode preparation method for accurate electrochemical measurements of double-side-coated electrode from commercial Li-ion batteries

NASA Astrophysics Data System (ADS)

Zhou, Ge; Wang, Qiyu; Wang, Shuo; Ling, Shigang; Zheng, Jieyun; Yu, Xiqian; Li, Hong

2018-04-01

The post mortem electrochemical analysis, including charge-discharge and electrochemical impedance spectroscopy (EIS) measurements, are critical steps for revealing the failure mechanisms of commercial lithium-ion batteries (LIBs). These post measurements usually require the reassembling of coin-cell with electrode which is often double-side-coated in commercial LIBs. It is difficult to use such double-side-coated electrode to perform accurate electrochemical measurements because the back side of the electrode is coated with active materials, rather than single-side-coated electrode that is often used in coin-cell measurements. In this study, we report a facile tape-covering sample preparation method, which can effectively suppress the influence of back side of the double-side-coated electrodes on capacity and EIS measurements in coin-cells. By tape-covering the unwanted side, the areal capacity of the desired investigated side of the electrode has been accurately measured with an experimental error of about 0.5% at various current densities, and accurate EIS measurements and analysis have been conducted as well.

Nickel-copper oxide nanowires for highly sensitive sensing of glucose

NASA Astrophysics Data System (ADS)

Bai, Xiaofang; Chen, Wei; Song, Yanfang; Zhang, Jiazhou; Ge, Ruipeng; Wei, Wei; Jiao, Zheng; Sun, Yuhan

2017-10-01

Accurate determination of glucose is of considerable importance in diverse fields such as clinical diagnostics, biotechnology, and food industry. A low-cost and easy to scale-up approach has been developed for the preparation of nickel-copper oxide nanowires (Ni-CuO NWs) with hierarchical structures comprising porous NiO substrate and CuO nanowires. The successfully prepared Ni-CuO NWs were exploited as non-enzymatic electrochemical sensing probes for the reliable detection of glucose. Electrochemical measurements such as cyclic voltammetry (CV) and chronoamperometry (CA) illustrated that the Ni-CuO NWs exhibited excellent electrochemical performance toward glucose oxidation with a superior sensitivity of 5610.6 μA mM-1 cm-2, a low detection limit of 0.07 μM, a wide linear range from 0.2 to 3.0 mM, and a good selectivity. This was attributed to the synergetic effect of the hierarchical structures and active Ni(OH)2 surface species in Ni-CuO NWs. The rational design of the metal oxide composites provided an efficient strategy for the fabrication of electrochemical non-enzymatic sensors.

Synthesis of a new π-conjugated redox oligomer: Electrochemical and optical investigation

NASA Astrophysics Data System (ADS)

Blili, Saber; Zaâboub, Zouhour; Maaref, Hassen; Haj Said, Ayoub

2017-01-01

A new π-conjugated redox oligomer was prepared according a two-Step Synthesis. Firstly, an oligophenylene (OMPA) was obtained from the anodic oxidation of the (4-methoxyphenyl)acetonitrile. Then, the resulting material was chemically modified by the Knoevenagel condensation with the ferrocenecarboxaldehyde. This reaction led to a redox-conjugated oligomer the Fc-OMPA. The synthesized material was characterized using different spectroscopic techniques: NMR, FTIR, UV-vis and photoluminescence (PL) spectroscopy. The Fc-OMPA was used to modify a platinum electrode surface and the electrochemical response of the ferrocene redox-center was investigated by cyclic voltammetry. Moreover, the room temperature PL spectra of Fc-OMPA revealed that the ferrocene moiety, which acts as an electron donor, can effectively quench the oligomer luminescence. However, when ferrocene was oxidized to ferrocenium ion, the intramolecular charge transfer process was prevented which consequently enhanced the light emission. Thus, the oligomer light-emission can be, chemically or electrochemically tuned. The obtained results showed that the prepared material is a good candidate for the elaboration of electrochemical sensors and for the development of luminescent Redox-switchable devices.

Uniform manganese hexacyanoferrate hydrate nanocubes featuring superior performance for low-cost supercapacitors and nonenzymatic electrochemical sensors

NASA Astrophysics Data System (ADS)

Pang, Huan; Zhang, Yizhou; Cheng, Tao; Lai, Wen-Yong; Huang, Wei

2015-09-01

Uniform manganese hexacyanoferrate hydrate nanocubes are prepared via a simple chemical precipitation method at room temperature. Due to both micro/mesopores of the Prussian blue analogue and nanocubic structures, the manganese hexacyanoferrate hydrate nanocubes allow the efficient charge transfer and mass transport for electrolyte solution and chemical species. Thus, the manganese hexacyanoferrate hydrate nanocube electrode shows a good rate capability and cycling stability for electrochemical capacitors. Furthermore, electrodes modified with manganese hexacyanoferrate hydrate nanocubes demonstrate a sensitive electrochemical response to hydrogen peroxide (H2O2) in buffer solutions with a high selectivity.Uniform manganese hexacyanoferrate hydrate nanocubes are prepared via a simple chemical precipitation method at room temperature. Due to both micro/mesopores of the Prussian blue analogue and nanocubic structures, the manganese hexacyanoferrate hydrate nanocubes allow the efficient charge transfer and mass transport for electrolyte solution and chemical species. Thus, the manganese hexacyanoferrate hydrate nanocube electrode shows a good rate capability and cycling stability for electrochemical capacitors. Furthermore, electrodes modified with manganese hexacyanoferrate hydrate nanocubes demonstrate a sensitive electrochemical response to hydrogen peroxide (H2O2) in buffer solutions with a high selectivity. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr04322k

Formation of Sn–M (M=Fe, Al, Ni) alloy nanoparticles by DC arc-discharge and their electrochemical properties as anodes for Li-ion batteries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gao, Song; Huang, Hao, E-mail: huanghao@dlut.edu.cn; Wu, Aimin

2016-10-15

A direct current arc-discharge method was applied to prepare the Sn–M (M=Fe, Al, Ni) bi-alloy nanoparticles. Thermodynamic is introduced to analyze the energy circumstances for the formation of the nanoparticles during the physical condensation process. The electrochemical properties of as-prepared Sn–M alloy nanoparticles are systematically investigated as anodes of Li-ion batteries. Among them, Sn–Fe nanoparticles electrode exhibits high Coulomb efficiency (about 71.2%) in the initial charge/discharge (257.9 mA h g{sup −1}/366.6 mA h g{sup −1}) and optimal cycle stability (a specific reversible capacity of 240 mA h g{sup −1} maintained after 20 cycles) compared with others. Large differences in themore » electrochemical behaviors indicate that the chemical composition and microstructure of the nanoparticles determine the lithium-ion storage properties and the long-term cyclic stability during the charge/discharge process. - Graphical abstract: The growth mechanism and electrochemical performance of Sn-based alloy nanoparticles. - Highlights: • Thermodynamic analyses of oxides on Sn-M nanoparticles surface. • The relationship between chemical components and electrochemical responses. • Sn-Fe nanoparticles show excellent electrode performance.« less

Sol-gel derived electrode materials for supercapacitor applications

NASA Astrophysics Data System (ADS)

Lin, Chuan

1998-12-01

Electrochemical capacitors have been receiving increasing interest in recent years for use in energy storage systems because of their high energy and power density and long cycle lifes. Possible applications of electrochemical capacitors include high power pulsed lasers, hybrid power system for electric vehicles, etc. In this dissertation, the preparation of electrode materials for use as electrochemical capacitors has been studied using the sol-gel process. The high surface area electrode materials explored in this work include a synthetic carbon xerogel for use in a double-layer capacitor, a cobalt oxide xerogel for use in a pseudocapacitor, and a carbon-ruthenium xerogel composite, which utilizes both double-layer and faradaic capacitances. The preparation conditions of these materials were investigated in detail to maximize the surface area and optimize the pore size so that more energy could be stored while minimizing mass transfer limitations. The microstructures of the materials were also correlated with their performance as electrochemical capacitors to improve their energy and power densities. Finally, an idealistic mathematical model, including both double-layer and faradaic processes, was developed and solved numerically. This model can be used to perform the parametric studies of an electrochemical capacitor so as to gain a better understanding of how the capacitor works and also how to improve cell operations and electrode materials design.

Graphene-Selenium Hybrid Microballs as Cathode Materials for High-performance Lithium-Selenium Secondary Battery Applications.

PubMed

Youn, Hee-Chang; Jeong, Jun Hui; Roh, Kwang Chul; Kim, Kwang-Bum

2016-08-02

In this study, graphene-selenium hybrid microballs (G-SeHMs) are prepared in one step by aerosol microdroplet drying using a commercial spray dryer, which represents a simple, scalable continuous process, and the potential of the G-SeHMs thus prepared is investigated for use as cathode material in applications of lithium-selenium secondary batteries. These morphologically unique graphene microballs filled with Se particles exhibited good electrochemical properties, such as high initial specific capacity (642 mA h g(-1) at 0.1 C, corresponding to Se electrochemical utilisation as high as 95.1%), good cycling stability (544 mA h g(-1) after 100 cycles at 0.1 C; 84.5% retention) and high rate capability (specific capacity of 301 mA h g(-1) at 5 C). These electrochemical properties are attributed to the fact that the G-SeHM structure acts as a confinement matrix for suppressing the dissolution of polyselenides in the organic electrolyte, as well as an electron conduction path for increasing the transport rate of electrons for electrochemical reactions. Notably, based on the weight of hybrid materials, electrochemical performance is considerably better than that of previously reported Se-based cathode materials, attributed to the high Se loading content (80 wt%) in hybrid materials.

Electrochemical growth of CoNi and Pt-CoNi soft magnetic composites on an alkanethiol monolayer-modified ITO substrate.

PubMed

Escalera-López, D; Gómez, E; Vallés, E

2015-07-07

CoNi and Pt-CoNi magnetic layers on indium-tin oxide (ITO) substrates modified by an alkanethiol self-assembled monolayer (SAM) have been electrochemically obtained as an initial stage to prepare semiconducting layer-SAM-magnetic layer hybrid structures. The best conditions to obtain the maximum compactness of adsorbed layers of dodecanethiol (C12-SH) on ITO substrate have been studied using contact angle, AFM, XPS and electrochemical tests. The electrochemical characterization (electrochemical probe or voltammetric response in blank solutions) is fundamental to ensure the maximum blocking of the substrate. Although the electrodeposition process on the SAM-modified ITO substrate is very slow if the blocking of the surface is significant, non-cracked metallic layers of CoNi, with or without a previously electrodeposited seed-layer of platinum, have been obtained by optimizing the deposition potentials. Initial nucleation is expected to take place at the pinhole defects of the C12-SH SAM, followed by a mushroom-like growth regime through the SAM interface that allows the formation of a continuous metallic layer electrically connected to the ITO surface. Due to the potential of the methodology, the preparation of patterned metallic deposits on ITO substrate using SAMs with different coverage as templates is feasible.

Measuring skew in average surface roughness as a function of surface preparation

NASA Astrophysics Data System (ADS)

Stahl, Mark T.

2015-08-01

Characterizing surface roughness is important for predicting optical performance. Better measurement of surface roughness reduces polishing time, saves money and allows the science requirements to be better defined. This study characterized statistics of average surface roughness as a function of polishing time. Average surface roughness was measured at 81 locations using a Zygo® white light interferometer at regular intervals during the polishing process. Each data set was fit to a normal and Largest Extreme Value (LEV) distribution; then tested for goodness of fit. We show that the skew in the average data changes as a function of polishing time.

Nanomaterials for Electrochemical Immunosensing

PubMed Central

Pan, Mingfei; Gu, Ying; Yun, Yaguang; Li, Min; Jin, Xincui; Wang, Shuo

2017-01-01

Electrochemical immunosensors resulting from a combination of the traditional immunoassay approach with modern biosensors and electrochemical analysis constitute a current research hotspot. They exhibit both the high selectivity characteristics of immunoassays and the high sensitivity of electrochemical analysis, along with other merits such as small volume, convenience, low cost, simple preparation, and real-time on-line detection, and have been widely used in the fields of environmental monitoring, medical clinical trials and food analysis. Notably, the rapid development of nanotechnology and the wide application of nanomaterials have provided new opportunities for the development of high-performance electrochemical immunosensors. Various nanomaterials with different properties can effectively solve issues such as the immobilization of biological recognition molecules, enrichment and concentration of trace analytes, and signal detection and amplification to further enhance the stability and sensitivity of the electrochemical immunoassay procedure. This review introduces the working principles and development of electrochemical immunosensors based on different signals, along with new achievements and progress related to electrochemical immunosensors in various fields. The importance of various types of nanomaterials for improving the performance of electrochemical immunosensor is also reviewed to provide a theoretical basis and guidance for the further development and application of nanomaterials in electrochemical immunosensors. PMID:28475158

Evaluation of the effect of a home-bleaching agent on the surface characteristics of indirect esthetic restorative materials: part I--roughness.

PubMed

Torabi, Kianoosh; Rasaeipour, Sasan; Khaledi, Amir Alireza; Vojdani, Mahroo; Ghodsi, Safoura

2014-05-01

Pressing esthetic demands of good looking make people undergo bleaching procedures. However, the effect of bleaching agents on esthetic restorative materials with different surface preparations has been poorly studied. The aim of this study was to examine the effect of a homebleaching agent (carbamide peroxide: CP 38%) on the surface roughness of the polished fiber reinforced composite (FRC), overglazed, autoglazed, or polished ceramic samples. Twenty standardized cylindrical specimens were made of each of the following groups: over-glazed, autoglazed, polished porcelain and also FRC. The test specimens exposed to the CP 38%, 15 minutes, twice a day for 2 weeks according to the manufacturer's recommendation. Six samples from each group were selected randomly to form negative controls. Surface roughness measurements (Ra, micrometer) for baseline, test and control specimens were performed by use of a profilometer. Paired t-test, Mann-Whitney test, and Kruskal-Wallis test were used for statistical analyses. The data showed that bleaching with CP 38% significantly increased the surface roughness of all the test samples (p < 0.05). The type of surface preparation caused significant differences between the susceptibility of porcelain subgroups to bleaching (p < 0.05). The polished porcelain specimens showed the highest changes after bleaching. CP 38% significantly increases the surface roughness of the porcelains and FRC. The type of surface condition affects the amenability of the porcelain surface to the bleaching agent. Glazed porcelains were more resistant to roughness than the polished porcelains and also the composite. Roughening of porcelain and FRC occur following bleaching procedure. No special surface preparation of indirect esthetic restorative materials can completely preserve these materials from adverse effects of bleaching agents.

Development of a system for treatment of coconut industry wastewater using electrochemical processes followed by Fenton reaction.

PubMed

Gomes, Lúcio de Moura; Duarte, José Leandro da Silva; Pereira, Nathalia Marcelino; Martínez-Huitle, Carlos A; Tonholo, Josealdo; Zanta, Carmen Lúcia de Paiva E Silva

2014-01-01

The coconut processing industry generates a significant amount of liquid waste. New technologies targeting the treatment of industrial effluents have emerged, including advanced oxidation processes, the Fenton reaction, and electrochemical processes, which produce strong oxidizing species to remove organic matter. In this study we combined the Fenton reaction and electrochemical process to treat wastewater generated by the coconut industry. We prepared a synthetic wastewater consisting of a mixture of coconut milk and water and assessed how the Fenton reagents' concentration, the cathode material, the current density, and the implementation of associated technologies affect its treatment. Electrochemical treatment followed by the Fenton reaction diminished turbidity and chemical oxygen demand (COD) by 85 and 95%, respectively. The Fenton reaction followed by the electrochemical process reduced turbidity and COD by 93 and 85%, respectively. Therefore, a combination of the Fenton and electrochemical technologies can effectively treat the effluent from the coconut processing industry.

Porous silicon in drug delivery devices and materials☆

PubMed Central

Anglin, Emily J.; Cheng, Lingyun; Freeman, William R.; Sailor, Michael J.

2009-01-01

Porous Si exhibits a number of properties that make it an attractive material for controlled drug delivery applications: The electrochemical synthesis allows construction of tailored pore sizes and volumes that are controllable from the scale of microns to nanometers; a number of convenient chemistries exist for the modification of porous Si surfaces that can be used to control the amount, identity, and in vivo release rate of drug payloads and the resorption rate of the porous host matrix; the material can be used as a template for organic and biopolymers, to prepare composites with a designed nanostructure; and finally, the optical properties of photonic structures prepared from this material provide a self-reporting feature that can be monitored in vivo. This paper reviews the preparation, chemistry, and properties of electrochemically prepared porous Si or SiO2 hosts relevant to drug delivery applications. PMID:18508154

Highly selective dopamine electrochemical sensor based on electrochemically pretreated graphite and nafion composite modified screen printed carbon electrode.

PubMed

Ku, Shuhao; Palanisamy, Selvakumar; Chen, Shen-Ming

2013-12-01

Herein, we report a highly selective dopamine electrochemical sensor based on electrochemically pretreated graphite/nafion composite modified screen printed carbon (SPC) electrode. Electrochemically activated graphite/nafion composite was prepared by using a simple electrochemical method. Scanning electron microscope (SEM) used to characterize the surface morphology of the fabricated composite electrode. The SEM result clearly indicates that the graphitic basal planes were totally disturbed and leads to the formation of graphite nanosheets. The composite modified electrode showed an enhanced electrocatalytic activity toward the oxidation of DA when compared with either electrochemical pretreated graphite or nafion SPC electrodes. The fabricated composite electrode exhibits a good electrocatalytic oxidation toward DA in the linear response range from 0.5 to 70 μM with the detection limit of 0.023 μM. The proposed sensor also exhibits very good selectivity and stability, with the appreciable sensitivity. In addition, the proposed sensor showed satisfactory recovery results toward the commercial pharmaceutical DA samples. Copyright © 2013 Elsevier Inc. All rights reserved.

Synthesis and electrochemical properties of Ti-doped DLC films by a hybrid PVD/PECVD process

NASA Astrophysics Data System (ADS)

Jo, Yeong Ju; Zhang, Teng Fei; Son, Myoung Jun; Kim, Kwang Ho

2018-03-01

Low electrical conductivity and poor adhesion to metallic substrates are the main drawbacks of diamond-like carbon (DLC) films when used in electrode applications. In this study, Ti-doped DLC films with various Ti contents were synthesized on metal Ti substrates by a hybrid PVD/PECVD process, where PECVD was used for deposition of DLC films and PVD was used for Ti doping. The effects of the Ti doping ratio on the microstructure, adhesion strength, and electrical and electrochemical properties of the DLC films were systematically investigated. An increase in the Ti content led to increased surface roughness and a higher sp2/sp3 ratio of the Ti-DLC films. Ti atoms existed as amorphous-phase Ti carbide when the Ti doping ratio was less than 2.8 at.%, while the nanocrystalline TiC phase was formed in DLC films when the Ti doping ratio was exceeded 4.0 at.%. The adhesion strength, electrical resistivity, electrochemical activity and reversibility of the DLC films were greatly improved by Ti doping. The influence of Ti doping ratio on the electrical and electrochemical properties of the DLC films were also investigated and the best performance was obtained at a Ti content of 2.8 at.%.

Method of preparing a positive electrode for an electrochemical cell

DOEpatents

Tomczuk, Zygmunt

1979-01-01

A method of preparing an electrochemical cell including a metal sulfide as the positive electrode reactant and lithium alloy as the negative electrochemical reactant with an alkali metal, molten salt electrolyte is disclosed which permits the assembly to be accomplished in air. The electrode reactants are introduced in the most part as a sulfide of lithium and the positive electrode metal in a single-phase compound. For instance, Li.sub.2 FeS.sub.2 is a single-phase compound that is produced by the reaction of Li.sub.2 S and FeS. This compound is an intermediate in the positive electrode cycle from FeS.sub.2 to Fe and Li.sub.2 S. Its use minimizes volumetric changes from the assembled to the charged and discharged conditions of the electrode and minimizes electrode material interaction with air and moisture during assembly.

Preparation of a porous Sn@C nanocomposite as a high-performance anode material for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Zhang, Yanjun; Jiang, Li; Wang, Chunru

2015-07-01

A porous Sn@C nanocomposite was prepared via a facile hydrothermal method combined with a simple post-calcination process, using stannous octoate as the Sn source and glucose as the C source. The as-prepared Sn@C nanocomposite exhibited excellent electrochemical behavior with a high reversible capacity, long cycle life and good rate capability when used as an anode material for lithium ion batteries.A porous Sn@C nanocomposite was prepared via a facile hydrothermal method combined with a simple post-calcination process, using stannous octoate as the Sn source and glucose as the C source. The as-prepared Sn@C nanocomposite exhibited excellent electrochemical behavior with a high reversible capacity, long cycle life and good rate capability when used as an anode material for lithium ion batteries. Electronic supplementary information (ESI) available: Detailed experimental procedure and additional characterization, including a Raman spectrum, TGA curve, N2 adsorption-desorption isotherm, TEM images and SEM images. See DOI: 10.1039/c5nr03093e

Layered double hydroxide materials coated carbon electrode: New challenge to future electrochemical power devices

NASA Astrophysics Data System (ADS)

Djebbi, Mohamed Amine; Braiek, Mohamed; Namour, Philippe; Ben Haj Amara, Abdesslem; Jaffrezic-Renault, Nicole

2016-11-01

Layered double hydroxides (LDHs) have been widely used in the past years due to their unique physicochemical properties and promising applications in electroanalytical chemistry. The present paper is going to focus exclusively on magnesium-aluminum and zinc-aluminum layered double hydroxides (MgAl & ZnAl LDHs) in order to investigate the property and structure of active cation sites located within the layer structure. The MgAl and ZnAl LDH nanosheets were prepared by the constant pH co-precipitation method and uniformly supported on carbon-based electrode materials to fabricate an LDH electrode. Characterization by powder x-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy and transmission electron microscopy revealed the LDH form and well-crystallized materials. Wetting surface properties (hydrophilicity and hydrophobicity) of both prepared LDHs were recorded by contact angle measurement show hydrophilic character and basic property. The electrochemical performance of these hybrid materials was investigated by mainly cyclic voltammetry, electrochemical impedance spectroscopy and chronoamperometry techniques to identify the oxidation/reduction processes at the electrode/electrolyte interface and the effect of the divalent metal cations in total reactivity. The hierarchy of the modified electrode proves that the electronic conductivity of the bulk material is considerably dependent on the divalent cation and affects the limiting parameter of the overall redox process. However, MgAl LDH shows better performance than ZnAl LDH, due to the presence of magnesium cations in the layers. Following the structural, morphological and electrochemical behavior studies of both synthesized LDHs, the prepared LDH modified electrodes were tested through microbial fuel cell configuration, revealing a remarkable, potential new pathway for high-performance and cost-effective electrode use in electrochemical power devices.

An Electrochemical Processing Strategy for Improving Tribological Performance of Aisi 316 Stainless Steel Under Grease Lubrication

NASA Astrophysics Data System (ADS)

Zou, Jiaojuan; Li, Maolin; Lin, Naiming; Zhang, Xiangyu; Qin, Lin; Tang, Bin

2014-12-01

In order to improve the tribological performance of AISI 316 stainless steel (316 SS) under grease lubrication, electrochemical processing was conducted on it to obtain a rough (surface texturing-like) surface by making use of the high sensitivity of austenitic stainless steel to pitting corrosion in Cl--rich environment. Numerous corrosion pits or micro-ditches acted as micro-reservoirs on the obtained surface. While the grease could offer consistent lubrication, and then improve the tribological performance of 316 SS. Tribological behaviors of raw 316 SS and the treated sample were measured using a reciprocating type tribometer sliding against GCr15 steel counterpart under dry and grease lubrication conditions. The results showed that the mass losses of the two samples were in the same order of magnitude, and the raw sample exhibited lower friction coefficient in dry sliding. When the tests were conducted under grease lubrication condition, the friction coefficients and mass losses of the treated sample were far lower than those of the raw 316 SS. The tribological performance of 316 SS under grease lubrication was drastically improved after electrochemical processing.

Enhanced Intrinsic Catalytic Activity of λ-MnO2 by Electrochemical Tuning and Oxygen Vacancy Generation.

PubMed

Lee, Sanghan; Nam, Gyutae; Sun, Jie; Lee, Jang-Soo; Lee, Hyun-Wook; Chen, Wei; Cho, Jaephil; Cui, Yi

2016-07-18

Chemically prepared λ-MnO2 has not been intensively studied as a material for metal-air batteries, fuel cells, or supercapacitors because of their relatively poor electrochemical properties compared to α- and δ-MnO2 . Herein, through the electrochemical removal of lithium from LiMn2 O4 , highly crystalline λ-MnO2 was prepared as an efficient electrocatalyst for the oxygen reduction reaction (ORR). The ORR activity of the material was further improved by introducing oxygen vacancies (OVs) that could be achieved by increasing the calcination temperature during LiMn2 O4 synthesis; a concentration of oxygen vacancies in LiMn2 O4 could be characterized by its voltage profile as the cathode in a lithiun-metal half-cell. λ-MnO2-z prepared with the highest OV exhibited the highest diffusion-limited ORR current (5.5 mA cm(-2) ) among a series of λ-MnO2-z electrocatalysts. Furthermore, the number of transferred electrons (n) involved in the ORR was >3.8, indicating a dominant quasi-4-electron pathway. Interestingly, the catalytic performances of the samples were not a function of their surface areas, and instead depended on the concentration of OVs, indicating enhancement in the intrinsic catalytic activity of λ-MnO2 by the generation of OVs. This study demonstrates that differences in the electrochemical behavior of λ-MnO2 depend on the preparation method and provides a mechanism for a unique catalytic behavior of cubic λ-MnO2 . © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparation and electrochemical properties of mesoporous NiCo2O4 double-hemisphere used as anode for lithium-ion battery.

PubMed

Yang, Yue; Huang, Guo Yong; Sun, Hongyu; Ahmad, Mashkoor; Mou, Qinyao; Zhang, Hongmei

2018-06-19

NiCo 2 O 4 is a potential anode material for lithium ion battery due to its many advantages, such as high theoretical capacitance, low cost, and good electrochemical activity. In this study, mesoporous NiCo 2 O 4 double-hemisphere (3-5 μm) with high surface area (270.68 m 2 ·g -1 ) and excellent electrochemical performances has been synthesized through a facile precipitation method followed with thermal treatment process. The prepared NiCo 2 O 4 is pure phase and can be indexed as a face-centered-cubic with a typical spinel structure. Electrochemical tests show the prepared material has high specific capacities (910 mAh·g -1 at 100 mA·g -1 ), excellent cyclicity (908  mAh·g -1 at 100 mA·g -1 after 60 cycles) and remarkable high rate performance (after 100 cycles, 585 mAh·g -1 at 400 mAh·g -1 , 415 mAh·g -1 at 800 mAh·g -1 and 320 mAh·g -1 at 1600 mAh·g -1 with coulombic efficiencies of almost 100%). The excellent performances of prepared NiCo 2 O 4 are mainly caused by the unique double-hemisphere structure, which has large surface area, gives material more opportunity to contact with electrolyte and facilitates lithium ion spreading into the material along the radical direction, resulting in a promising application for next-generation lithium-ion batteries. Copyright © 2018 Elsevier Inc. All rights reserved.

An electrochemical investigation of TMJ implant metal alloys in an artificial joint fluid environment: the influence of pH variation.

PubMed

Royhman, Dmitry; Radhakrishnan, Rashmi; Yuan, Judy Chia-Chun; Mathew, Mathew T; Mercuri, Louis G; Sukotjo, Cortino

2014-10-01

To investigate the corrosion behaviour of commonly used TMJ implants alloys (CoCrMo and Ti6Al4V) under simulated physiological conditions. Corrosion behaviour was evaluated using standard electrochemical corrosion techniques and galvanic corrosion techniques as per ASTM standards. Standard electrochemical tests (E(corr), I(corr), R(p) and C(f)) were conducted in bovine calf serum (BCS), as a function of alloys type and different pHs. Galvanic corrosion tests were conducted in BCS at a pH of 7.6. Alloy surfaces were characterized using white-light interferometry (WLI) and scanning electron microscopy (SEM). The potentiodynamic test results exhibited the enhanced passive layer growth and a better corrosion resistance of Ti6Al4V compared to CoCrMo. Electrochemical impedance spectroscopy measurements demonstrated the influence of protein as a function of pH on corrosion mechanisms/kinetics. Galvanic coupling was not a major contributor to corrosion. SEM and WLI images demonstrated a significantly higher in surface roughness in CoCrMo after corrosion. The results of this study suggest that Ti6Al4V shows superior corrosion behaviour to CoCrMo due to its strong passive layer, simulated joint fluid components can affect the electrochemical nature of the metal/electrolyte interface as a function of pH, and the galvanic effect of coupling CoCrMo and Ti6Al4V in a single joint is weak. Published by Elsevier Ltd.

Method of preparing porous, rigid ceramic separators for an electrochemical cell. [Patent application

DOEpatents

Bandyopadhyay, G.; Dusek, J.T.

Porous, rigid separators for electrochemical cells are prepared by first calcining particles of ceramic material at temperatures above about 1200/sup 0/C for a sufficient period of time to reduce the sinterability of the particles. A ceramic powder that has not been calcined is blended with the original powder to control the porosity of the completed separator. The ceramic blend is then pressed into a sheet of the desired shape and sintered at a temperature somewhat lower than the calcination temperature. Separator sheets of about 1 to 2.5 mm thickness and 30 to 70% porosity can be prepared by this technique. Ceramics such as yttria, magnesium oxide, and magnesium-aluminium oxide have advantageously been used to form separators by this method.

A doped activated carbon prepared from polyaniline for high performance supercapacitors

NASA Astrophysics Data System (ADS)

Li, Limin; Liu, Enhui; Li, Jian; Yang, Yanjing; Shen, Haijie; Huang, Zhengzheng; Xiang, Xiaoxia; Li, Wen

A novel doped activated carbon has been prepared from H 2SO 4-doped polyaniline which is prepared by the oxypolymerization of aniline. The morphology, surface chemical composition and surface area of the carbon have been investigated by scanning electron microscope, X-ray photoelectron spectroscopy and Brunaner-Emmett-Teller measurement, respectively. Electrochemical properties of the doped activated carbon have been studied by cyclic voltammograms, galvanostatic charge/discharge, and electrochemical impedance spectroscopy measurements in 6 mol l -1 KOH. The specific capacitance of the carbon is as high as 235 F g -1, the specific capacitance hardly decreases at a high current density 11 A g -1 after 10,000 cycles, which indicates that the carbon possesses excellent cycle durability and may be a promising candidate for supercapacitors.

A facile and green preparation of reduced graphene oxide using Eucalyptus leaf extract

NASA Astrophysics Data System (ADS)

Li, Chengyang; Zhuang, Zechao; Jin, Xiaoying; Chen, Zuliang

2017-11-01

In this paper, a green and facile synthesis of reduced graphene oxide (GO) by Eucalyptus leaf extract (EL-RGO) was investigated, which was characterized with ultraviolet-visible spectroscopy (UV), Raman spectroscopy, X-ray diffraction (XRD), scanning electron microscope (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and Thermal gravimetric analysis (TG). Eucalyptus leaf extract also play both reducing and capping stabilizing agents prepared EL-RGO as shown a good stability and electrochemical properties. This approach could provide an alternative method to prepare EL-RGO in large-scale production. Moreover, the good electrochemical property and biocompatibility can be used in various applications. In addition, the merit of this study is that both the oxidized products and the reducing agents are environmental friendly by green reduction.

Preparation and Electrochemical Properties of Graphene/Epoxy Resin Composite Coating

NASA Astrophysics Data System (ADS)

Liao, Zijun; Zhang, Tianchi; Qiao, Sen; Zhang, Luyihang

2017-11-01

The multilayer graphene powder as filler, epoxy modified silicone resin as film-forming agent, anticorrosion composite coating has been created using sand dispersion method, the electrochemical performance was compared with different content of graphene composite coating and pure epoxy resin coating. The open circuit potential (OCP), potentiodynamic polarization curves (Tafel Plot) and electrochemical impedance spectroscopy (EIS) were tested. The test results showed that the anti-corrosion performance of multilayer graphene added has improved greatly, and the content of the 5% best corrosion performance of graphene composite coating.

Surface immobilized azomethine for multiple component exchange.

PubMed

Lerond, Michael; Bélanger, Daniel; Skene, W G

2017-09-27

Diazonium chemistry concomitant with in situ electrochemical reduction was used to graft an aryl aldehyde to indium-tin oxide (ITO) coated glass substrates. This served as an anchor for preparing electroactive azomethines that were covalently bonded to the transparent electrode. The immobilized azomethines could undergo multiple step-wise component exchanges with different arylamines. The write-erase-write sequences were electrochemically confirmed. The azomethines could also be reversibly hydrolyzed. This was exploited for multiple azomethine-hydrolysis cycles resulting in discrete electroactive immobilized azomethines. The erase-rewrite sequences were also electrochemically confirmed.

Preparation of nickel oxide thin films at different annealing temperature by sol-gel spin coating method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Abdullah, M. A. R., E-mail: ameerridhwan89@gmail.com; Mamat, M. H., E-mail: hafiz-030@yahoo.com; Ismail, A. S., E-mail: kyrin-samaxi@yahoo.com

2016-07-06

Preparation of NiO thin films at different annealing temperature by sol-gel method was conducted to synthesize the quality of the surface thin films. The effects of annealing temperature on the surface topology were systematically investigated. Our studies confirmed that the surface roughness of the thin films was increased whenever annealing temperature was increase. NiO thin films morphology structure analysis was confirmed by field emission scanning electron microscope. Surface roughness of the thin films was investigated by atomic force microscopy.

Specimen preparation for x-ray fluorescence analysis of solutions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Eksperiandova, L.P.; Spolnik, Z.M.; Blank, A.B.

1995-12-31

Specimens for x-ray fluorescence analysis (XRFA) were prepared by adding dry gelatine (10%) to the analysis solution, homogenizing the mixture and cooling for 20 minutes. Thus, a compact resilient mass could be formed with the required shape and size; the roughness of the surface was determined by the roughness of the surface on which the specimen was formed, much the same as highly polished. Various calibration methods can be applied in the XRFA of a variety of materials if such specimens are used. 12 refs., 1 fig., 2 tabs.

Pulse electrodeposition of self-lubricating Ni-W/PTFE nanocomposite coatings on mild steel surface

NASA Astrophysics Data System (ADS)

Sangeetha, S.; Kalaignan, G. Paruthimal; Anthuvan, J. Tennis

2015-12-01

Ni-W/PTFE nanocomposite coatings with various contents of PTFE (polytetafluoroethylene) particles were prepared by pulse current (PC) electrodeposition from the Ni-W plating bath containing self lubricant PTFE particles to be co-deposited. Co-deposited PTFE particulates were uniformly distributed in the Ni-W alloy matrix. The coatings were characterized by Scanning Electron Microscopy (SEM), Energy Dispersive X-Ray Analysis (EDAX), X-ray Diffractometry (XRD) and Vicker's micro hardness tester. Tafel Polarization and electrochemical Impedance methods were used to evaluate the corrosion resistance behaviour of the nanocomposite coatings in 3.5% NaCl solution. It was found that, the Ni-W/PTFE nanocomposite coating has better corrosion resistance than the Ni-W alloy coating. Surface roughness and friction coefficient of the coated samples were assessed by Mitutoyo Surftest SJ-310 (ISO1997) and Scratch tester TR-101-M4 respectively. The contact angle (CA) of a water droplet on the surface of nanocomposite coating was measured by Optical Contact Goniometry (OCA 35). These results indicated that, the addition of PTFE in the Ni-W alloy matrix has resulted moderate microhardness, smooth surface, less friction coefficient, excellent water repellency and enhanced corrosion resistance of the nanocomposite coatings.

Electrochemical performances of graphene nanoribbons interlacing hollow NiCo oxide nanocages

NASA Astrophysics Data System (ADS)

Zhao, Xiyu; Li, Xinlu; Huang, Yanchun; Su, Zelong; Long, Junjun; Zhang, Shilei; Sha, Junwei; Wu, Tianli; Wang, Ronghua

2017-12-01

A hybrid of graphene nanoribbons (GNRs) interlacing hollow NiCoO2 (G-HNCO) nanocages in a size range of 300 500 nm with rough surface is synthesized by a chemical etching Cu2O templates and followed by GNR interlacing process. The G-HNCO showed high electrochemical performance of oxygen evolution reaction (OER), which exhibited small onset potential of 1.50 V and achieved current densities of 10 mA cm-2 at potentials of 1.62 V. Also, the hybrid delivered high capacitance of 937.8 F g-1 at 1 A g-1 in supercapacitor (SC) tests as well as stable cycling performance in both OER and SC measurements. The approach to synthesize the hybrid is simple and scalable for other graphene nanoribbon-based electrocatalysts. [Figure not available: see fulltext.

Smooth and selective photo-electrochemical etching of heavily doped GaN:Si using a mode-locked 355 nm microchip laser

NASA Astrophysics Data System (ADS)

Lee, SeungGeun; Mishkat-Ul-Masabih, Saadat; Leonard, John T.; Feezell, Daniel F.; Cohen, Daniel A.; Speck, James S.; Nakamura, Shuji; DenBaars, Steven P.

2017-01-01

We investigate the photo-electrochemical (PEC) etching of Si-doped GaN samples grown on nonpolar GaN substrates, using a KOH/K2S2O8 solution and illuminated by a Xe arc lamp or a Q-switched 355 nm laser. The etch rate with the arc lamp decreased as the doping concentration increased, and the etching stopped for concentrations above 7.7 × 1018 cm-3. The high peak intensity of the Q-switched laser extended the etchable concentration to 2.4 × 1019 cm-3, with an etch rate of 14 nm/min. Compositionally selective etching was demonstrated, with an RMS surface roughness of 1.6 nm after etching down to an n-Al0.20Ga0.80N etch stop layer.

Nano-structured manganese oxide as a cathodic catalyst for enhanced oxygen reduction in a microbial fuel cell fed with a synthetic wastewater.

PubMed

Liu, Xian-Wei; Sun, Xue-Fei; Huang, Yu-Xi; Sheng, Guo-Ping; Zhou, Kang; Zeng, Raymond J; Dong, Fang; Wang, Shu-Guang; Xu, An-Wu; Tong, Zhong-Hua; Yu, Han-Qing

2010-10-01

Microbial fuel cells (MFCs) provide new opportunities for the simultaneous wastewater treatment and electricity generation. Enhanced oxygen reduction capacity of cost-effective metal-based catalysts in an air cathode is essential for the scale-up and commercialization of MFCs in the field of wastewater treatment. We demonstrated that a nano-structured MnO(x) material, prepared by an electrochemically deposition method, could be an effective catalyst for oxygen reduction in an MFC to generate electricity with the maximum power density of 772.8 mW/m(3) and remove organics when the MFC was fed with an acetate-laden synthetic wastewater. The nano-structured MnO(x) with the controllable size and morphology could be readily obtained with the electrochemical deposition method. Both morphology and manganese oxidation state of the nano-scale catalyst were largely dependent on the electrochemical preparation process, and they governed its catalytic activity and the cathodic oxygen reduction performance of the MFC accordingly. Furthermore, cyclic voltammetry (CV) performed on each nano-structured material suggests that the MnO(x) nanorods had an electrochemical activity towards oxygen reduction reaction via a four-electron pathway in a neutral pH solution. This work provides useful information on the facile preparation of cost-effective cathodic catalysts in a controllable way for the single-chamber air-cathode MFC for wastewater treatment. Copyright © 2010 Elsevier Ltd. All rights reserved.

The Local Atomic Structure and Chemical Bonding in Sodium Tin Phases

DOE PAGES

Baggetto, Loic; Bridges, Craig A.; Jumas, Dr. Jean-Claude; ...

2014-09-25

To understand these electrochemically-derived materials we have reinvestigated the formation of Na-Sn alloys to identify all the phases which form when x ≥ 1 (NaxSn) and characterized the local bonding around the Sn atoms with X-ray diffraction, 119Sn M ssbauer spectroscopy, and X-ray absorption spectroscopies. The results from the well-defined crystallographic materials were compared to the spectroscopic measurements of the local Sn structures in the electrochemically prepared materials. The reinvestigation of the Na-Sn compounds yields a number of new results: (i) Na 7Sn 3 is a new thermodynamically-stable phase with a rhombohedral structure and R-3m space group; (ii) orthorhombic Namore » 9Sn 4 (Cmcm) has relatively slow formation kinetics suggesting why it does not form at room temperature during the electrochemical reaction; (iii) orthorhombic Na 14.78Sn 4 (Pnma), better described as Na 16-xSn 4, is Na-richer than cubic Na 15Sn 4 (I-43d). Characterization of electrochemically prepared Na-Sn alloys indicate that, at the exception of Na 7Sn 3 and Na 15Sn 4, different crystal structures than similar Na-Sn compositions prepared via classic solid state reactions are formed. These phases are composed of disordered structures characteristic of kinetic-driven solid-state amorphization reactions. In these structures, Sn coordinates in asymmetric environments, which differ significantly from the environments present in Na-Sn model compounds.« less

Ru-assisted synthesis of Pd/Ru nanodendrites with high activity for ethanol electrooxidation

NASA Astrophysics Data System (ADS)

Zhang, Ke; Bin, Duan; Yang, Beibei; Wang, Caiqin; Ren, Fangfang; Du, Yukou

2015-07-01

Due to the specific physical and chemical properties of a highly branched noble metal, the controllable synthesis has attracted much attention. This article reports the synthesis of Pd/Ru nanodendrites by a facile method using an oil bath in the presence of polyvinyl pyrrolidone, potassium bromide and ascorbic acid. The morphology, structure, and composition of the as-prepared catalysts were characterized by means of X-ray diffraction, X-ray photoelectron spectroscopy and transmission electron microscopy. In the electrochemical measurement, the as-prepared Pd7/Ru1 bimetallic nanodendrites provide a large electrochemically active surface area and exhibit high peak current density in the forward scan toward ethanol electrooxidation, which is nearly four times higher than those of a pure Pd catalyst. The as-prepared Pd7/Ru1 catalysts also exhibit significantly enhanced cycling stability toward ethanol oxidation in alkaline medium, which are mainly ascribed to the synergetic effect between Pd and Ru. This indicates that the Pd7/Ru1 catalysts should have great potential applications in direct ethanol fuel cells.Due to the specific physical and chemical properties of a highly branched noble metal, the controllable synthesis has attracted much attention. This article reports the synthesis of Pd/Ru nanodendrites by a facile method using an oil bath in the presence of polyvinyl pyrrolidone, potassium bromide and ascorbic acid. The morphology, structure, and composition of the as-prepared catalysts were characterized by means of X-ray diffraction, X-ray photoelectron spectroscopy and transmission electron microscopy. In the electrochemical measurement, the as-prepared Pd7/Ru1 bimetallic nanodendrites provide a large electrochemically active surface area and exhibit high peak current density in the forward scan toward ethanol electrooxidation, which is nearly four times higher than those of a pure Pd catalyst. The as-prepared Pd7/Ru1 catalysts also exhibit significantly enhanced cycling stability toward ethanol oxidation in alkaline medium, which are mainly ascribed to the synergetic effect between Pd and Ru. This indicates that the Pd7/Ru1 catalysts should have great potential applications in direct ethanol fuel cells. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr02713f

Synergetic enhancement of gold nanoparticles and 2-mercaptobenzothiazole as highly-sensitive sensing strategy for tetrabromobisphenol A

NASA Astrophysics Data System (ADS)

Chen, Xuerong; Ji, Liudi; Zhou, Yikai; Wu, Kangbing

2016-05-01

Various gold nanoparticles (AuNPs) were in-situ prepared on the electrode surface through electrochemical reduction under different potentials such as -0.60, -0.50, -0.40, -0.30 and -0.20 V. The reduction potentials heavily affect the surface morphology and electrochemical activity of AuNPs such as effective area and catalytic ability, as confirmed using atomic force microscopy and electrochemical impedance spectroscopy. The electrochemical behaviors of tetrabromobisphenol A (TBBPA), a widely-existed pollutant with severe adverse health effects, were studied. The oxidation activity of TBBPA enhances obviously on the surface of AuNPs, and the signal improvements of TBBPA show difference on the prepared AuNPs. Interestingly, the existence of 2-mercaptobenzothiazole (MBT) further improves the oxidation signals of TBBPA on AuNPs. The synergetic enhancement effects of AuNPs and MBT were studied using cyclic voltammetry and chronocoulometry. The numerous nano-scaled gold particles together with the strong hydrophobic interaction between TBBPA and the assembled MBT on AuNPs jointly provide highly-effective accumulation for TBBPA. As a result, a sensitive and simple electrochemical method was developed for the direct determination of TBBPA, with detection limit of 0.12 μg L-1 (0.22 nM). The practical applications in water samples manifest that this new sensing system is accurate and feasible.

Constructing the magnetic bifunctional graphene/titania nanosheet-based composite photocatalysts for enhanced visible-light photodegradation of MB and electrochemical ORR from polluted water.

PubMed

Zhang, Qian; Zhang, Yihe; Meng, Zilin; Tong, Wangshu; Yu, Xuelian; An, Qi

2017-09-25

Photocatalysis is a promising strategy to address the global environmental and energy challenges. However, the studies on the application of the photocatalytically degraded dye-polluted water and the multi-purpose use of one type of catalyst have remained sparse. In this report, we try to demonstrate a concept of multiple and cyclic application of materials and resources in environmentally relevant catalyst reactions. A magnetic composite catalyst prepared from exfoliated titania nanosheets, graphene, the magnetic iron oxide nanoparticles, and a polyelectrolyte enabled such a cyclic application. The composite catalyst decomposed a methylene blue-polluted water under visible light, and then the catalyst was collected and removed from the treated water using a magnet. The photocatalytically treated water was then used to prepare the electrolyte in electrochemical reductive reactions and presented superior electrochemical performance compared with the dye-polluted water. The composite catalyst was once again used as the cathode catalyst in the electrochemical reaction. Each component in the composite catalyst was indispensable in its catalytic activity, but each component played different roles in the photochemical, magnetic recycling, and electrochemical processes. We expect the report inspire the study on the multi-functional catalyst and cyclic use of the catalytically cleaned water, which should contribute for the environmental and energy remedy from a novel perspective.

Pt NPs and DNAzyme functionalized polymer nanospheres as triple signal amplification strategy for highly sensitive electrochemical immunosensor of tumour marker.

PubMed

Chang, Honghong; Zhang, Haochun; Lv, Jia; Zhang, Bing; Wei, Wenlong; Guo, Jingang

2016-12-15

Highly sensitive determination of tumour markers is the key for early diagnosis of cancer. Herein, triple signal amplification strategy resulting from polymer nanospheres, Pt NPs, and DNAzyme was proposed in the developed electrochemical immunosensor. First, electroactive polymer nanospheres were synthesized by infinite coordination polymerization of ferrocenedicarboxylic acid, which could generate strong electrochemical signals due to plentiful ferrocene molecules. Further, the polymer nanospheres were functionalized by Pt NPs and DNAzyme (hemin/G-quadruplex) with the ability of catalyzing H2O2, which contributes to enhance the electrochemical signals. The prepared conjugations were characterized by transmission electron microscope (TEM) and energy dispersive X-ray spectroscopy (EDX). And the process of preparation was monitored by zeta potential. Based on the sandwich-type immunoassay, the electrochemical immunosensor was constructed employing the conjugations as signal tags. Under optimal conditions, the DPV peak increased with the increasing of alpha fetal protein (AFP) concentration, and the linear range was from 0.1pgmL(-1) to 100ngmL(-1) with low detection limit of 0.086pgmL(-1). Meanwhile, the designed immunosensor exhibited excellent selectivity and anti-interference property, good reproducibility and stability. More importantly, there were no significant differences in analyzing real clinical samples between designed immunosensor and commercial ELISA. Copyright © 2016 Elsevier B.V. All rights reserved.

Electrodeposition of high-density lithium vanadate nanowires for lithium-ion battery

NASA Astrophysics Data System (ADS)

Hua, Kang; Li, Xiujuan; Fang, Dong; Yi, Jianhong; Bao, Rui; Luo, Zhiping

2018-07-01

Lithium vanadate nanowires have been electrodeposited onto a titanium (Ti) foil by a direct current electrodeposition without template. The morphology, crystal structure, and the effects of deposition voltage, temperature and time on the prepared samples were tested and presented. The as-prepared lithium vanadate nanowires/Ti composite can be used as electrode for lithium-ion battery. Electrochemical measurements showed that the electrode displayed a specific discharge capacitance as high as 235.1 mAh g-1 after 100 cycles at a current density of 30 mA g-1. This research provides a new pathway to explore high tap density vanadates nanowires on metals with enhanced electrochemical performance.

Highly Safe Ionic Liquid Electrolytes for Sodium-Ion Battery: Wide Electrochemical Window and Good Thermal Stability.

PubMed

Wu, Feng; Zhu, Na; Bai, Ying; Liu, Libin; Zhou, Hang; Wu, Chuan

2016-08-24

Novel ionic liquid (IL) electrolytes are prepared by mixing 1-ethyl-3-methylimidazolium-bis-tetrafluoroborate (EMIBF4) with different concentrations of sodium salt (NaBF4). The as-prepared IL electrolytes display wide electrochemical windows of ∼4 V (1-5 V), which are consistent with the quantum chemical theoretical calculation. The IL electrolyte with 0.1 M NaBF4 shows excellent ionic conductivity, namely, 9.833 × 10(-3) S cm(-1) at 20 °C. In addition, nonflammability and good thermal stability are exhibited by combustion test and thermogravimetric analysis (TGA), which indicate the high safety of the IL electrolyte.

Nanoelectrical investigation and electrochemical performance of nickel-oxide/carbon sphere hybrids through interface manipulation.

PubMed

Yang, Xiaogang; Zhang, Yan'ge; Wu, Guodong; Zhu, Congxu; Zou, Wei; Gao, Yuanhao; Tian, Jie; Zheng, Zhi

2016-05-01

Advanced hetero-nanostructured materials for electrochemical devices, such as Li-ion batteries (LiBs), dramatically depend on each functional component and their interfaces to transport and storage charges, where the bottleneck is the sluggish one in series. In this work, we prepare Ni(OH)2@C hybrids through a continuous feeding in reflux and followed by a hydrothermal treatment. The as-prepared Ni(OH)2@C can be further converted into NiO@C hybrids after thermal annealing. As a control, Ni(OH)2&C and NiO&C nanocomposites have also been prepared. Peakforce Tuna measurement shows the conductivity of the NiO@C hybrids is higher than that of NiO&C composites in nanoscale. To further investigate the quality of the interface, 100 charge/discharge cycles of the hybrids are performed in LiBs. The capacity retention of hybrid materials has significantly improved than the simple carbon composites. The enhancement of the electrochemical performance is attributed to the better electric conductivity and smaller charge transfer impedance and strong covalent interface between nickel species and carbon spheres obtained through the controlled seeded deposition. Copyright © 2016 Elsevier Inc. All rights reserved.

Enhancement of the electrochemical performance of hydrothermally prepared anatase nanoparticles for optimal use as high capacity anode materials in lithium ion batteries (LIBs)

NASA Astrophysics Data System (ADS)

Sanad, M. M. S.; Rashad, M. M.; Powers, K.

2015-02-01

Mesoporous TiO2 nanoparticles have been synthesized via facile hydrolytic hydrothermal technique without incorporation any template. The precious metallic nanoparticles; Ag, Pt and Pd have been embedded between the anatase particles using in situ reduction step. The structural properties of the as-synthesized samples were investigated by X-ray diffraction, transmission electron microscopic and N2 adsorption-desorption isotherm ( S BET). The electrochemical studies for the as-prepared anode materials including, cyclic voltammetry and electrochemical impedance spectroscopy indicated a significant improvement in the electronic conductivity of the lithium-TiO2 cells. Therefore, the charge-discharge rates were noticeably promoted as a result of the enhancement of Li-ion diffusion and charge transfer. The cycling results of Pd-TiO2 revealed a marvelous improvement in both charge and discharge capacities by 89.4 and 88 % after 10 cycles at C/5 rate. Generally, all the as-prepared TiO2 nanocomposites showed enhanced specific capacity, cycling stability and rate capability compared to the pure TiO2, providing a promising behavior for use as anodes in lithium ion batteries (LIBs).

Effect of S-doping on structural, optical and electrochemical properties of vanadium oxide thin films prepared by spray pyrolysis

NASA Astrophysics Data System (ADS)

Mousavi, M.; Kompany, A.; Shahtahmasebi, N.; Bagheri-Mohagheghi, M.-M.

2013-12-01

In this research, S-doped vanadium oxide thin films, with doping levels from 0 to 40 at.%, are prepared by spray pyrolysis technique on glass substrates. For electrochemical measurements, the films were deposited on florin-tin oxide coated glass substrates. The effect of S-doping on structural, electrical, optical and electrochemical properties of vanadium oxide thin films was studied. The x-ray diffractometer analysis indicated that most of the samples have cubic β-V2O5 phase structure with preferred orientation along [200]. With increase in the doping levels, the structure of the samples tends to be amorphous. The scanning electron microscopy images show that the structure of the samples is nanobelt-shaped and the width of the nanobelts decreases from nearly 100 to 40 nm with increase in the S concentration. With increase in the S-doping level, the sheet resistance and the optical band gap increase from 940 to 4015 kΩ/square and 2.41 to 2.7 eV, respectively. The cyclic voltammogram results obtained for different samples show that the undoped sample is expanded and the sample prepared at 20 at.% S-doping level has sharper anodic and cathodic peaks.

Flower-like NiO structures: Controlled hydrothermal synthesis and electrochemical characteristic

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chai, Hui; Chen, Xuan; Key Laboratory of Advanced Functional Materials, Institute of Applied Chemistry, Xinjiang University, Urumqi 830046, Xinjiang

Graphical abstract: Flower-like porous NiO was obtained via thermal decomposition of the precursor prepared by a hydrothermal process using hexamethylenetetramine and polyethylene glycol as hydrolysis-controlling agent and surfactant, respectively. The morphology and microstructure of as-synthesized NiO were characterized by X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results of electrochemical measurements demonstrated that the flower-like porous NiO has high capacity (340 F g{sup −1}) with excellent cycling performance as electrode materials of electrochemical capacitors (ECs), which may be attributed to the unique microstrcture of NiO. Data analyses indicated that NiO with novel porousmore » structure attractive for practical and large-scale applications in electrochemical capacitors. Display Omitted Highlights: ► Synthesis and characterization of NiO with novel porous structure is presented in this work. ► The electrochemical performance of product was examined. ► NiO with excellent performance as electrode materials may be due to the unique microstrcture. ► NiO with novel porous structure attractive for practical with high capacity (340 F g{sup −1}). -- Abstract: Flower-like porous NiO was obtained by thermal decomposition of the precursor prepared by a hydrothermal process with hexamethylenetetramine and polyethylene glycol as hydrolysis-controlling agent and surfactant, respectively. The morphology and microstructure of as-synthesized NiO were characterized by X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The resulting structures of NiO exhibited porous like petal building blocks. The electrochemical measurements’ results demonstrated that flower-like porous NiO has high capacity (340 F g{sup −1}) with excellent cycling performance as electrode materials for electrochemical capacitors, which may be attributed to the unique structure of NiO. The results indicated that NiO with novel porous structure has been attractive for practical and large-scale applications in electrochemical capacitors.« less

Electrochemical aptamer-based nanosensor fabricated on single Au nanowire electrodes for adenosine triphosphate assay.

PubMed

Wang, Dongmei; Xiao, Xiaoqing; Xu, Shen; Liu, Yong; Li, Yongxin

2018-01-15

In this work, single Au nanowire electrodes (AuNWEs) were fabricated by laser-assisted pulling/hydrofluoric acid (HF) etching process, which then were characterized by transmission electron microscopy (TEM), electrochemical method and finite-element simulation. The as-prepared single AuNWEs were used to construct electrochemical aptamer-based nanosensors (E-AB nanosensors) based on the formation of Au-S bond that duplex DNA tagged with methylene blue (MB) was modified on the surface of electrode. In the presence of adenosine triphosphate (ATP), the MB-labeled aptamer dissociated from the duplex DNA due to the strong specific affinity between aptamer and target, which lead to the reduction of MB electrochemical signals. Moreover, BSA was employed to further passivate electrode surface bonding sites for the stable of the sensor. The as-prepared E-AB nanosensor has been used for ATP assay with excellent sensitivity and selectivity, even in a complex system like cerebrospinal fluid of rat brain. Considering the unique properties of good stability, larger surface area and smaller overall dimensions, this E-AB nanosensor should be an ideal platform for widely sensing applications in living bio-system. Copyright © 2017 Elsevier B.V. All rights reserved.

Ultrasensitive thrombin detection based on direct electrochemistry of highly loaded hemoglobin spheres-encapsulated platinum nanoparticles as labels and electrocatalysts.

PubMed

Wu, Yongmei; Xu, Wenju; Bai, Lijuan; Yuan, Yali; Yi, Huayu; Chai, Yaqin; Yuan, Ruo

2013-12-15

For the first time, a sandwich-type electrochemical method was proposed for ultrasensitive thrombin (TB) detection based on direct electrochemistry of highly loaded hemoglobin spheres-encapsulated platinum nanoparticles (PtNPs@Hb) as labels and electrocatalysts. The prepared PtNPs@Hb not only exhibited good biocompatibility, excellent electrocatalytic activity, but also presented redox activity of Hb. Thus, it was employed for the fabrication of aptasensor without any extraneous redox mediators, leading to a simple preparation process for the aptasensor. The high loading of Hb spheres as redox mediators could enhance the electrochemical signal. Importantly, the synergetic electrocatalytic behavior of Hb and PtNPs toward H2O2 reduction greatly amplified the electrochemical signal, resulting in the high sensitivity of aptasensor. Consequently, under optimal conditions, the designed aptasensor exhibited a lower detection limit of 0.05 pM and wide dynamic linear range from 0.15 pM to 40 nM for TB detection. Additionally, the proposed mediator-free and signal-amplified electrochemical aptasensor showed great potential in portable and cost-effective TB sensing devices. Copyright © 2013 Elsevier B.V. All rights reserved.

Nanoporous carbon derived from agro-waste pineapple leaves for supercapacitor electrode

NASA Astrophysics Data System (ADS)

Sodtipinta, Jedsada; Amornsakchai, Taweechai; Pakawatpanurut, Pasit

2017-09-01

By using KOH as the chemical activating agent in the synthesis, the activated carbon derived from pineapple leaf fiber (PALF) was prepared. The structure, morphology, and the surface functional groups of the as-prepared activated carbon were investigated using x-ray diffraction, field emission scanning electron microscope equipped with energy dispersive x-ray spectroscopy, and x-ray photoelectron spectroscopy. The electrochemical behavior and performance of the as-synthesized activated carbon electrode were measured using the cyclic voltammetry and the electrochemical impedance spectroscopy in 1 M Na2SO4 electrolyte solution in three-electrode setup. The activated carbon electrode exhibited the specific capacitance of 131.3 F g-1 at a scan rate of 5 mV s-1 with excellent cycling stability. The capacitance retention after 1000 cycles was about 97% of the initial capacitance at a scan rate of 30 mV s-1. Given these good electrochemical properties along with the high abundance of PALF, this activated carbon electrode has the potential to be one of the materials for future large-scale production of the electrochemical capacitors. Invited talk at 5th Thailand International Nanotechnology Conference (Nano Thailand-2016), 27-29 November 2016, Nakhon Ratchasima, Thailand.

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

NASA Astrophysics Data System (ADS)

Zhang, Yan; Hao, Huilian; Wang, Linlin

2016-12-01

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 (k0) of GCE with different ERGOs was comparatively investigated. Owing to increased surface areas and decreased defect density, the k0 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. k0 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.

Nitrogen-doped graphene: effect of graphite oxide precursors and nitrogen content on the electrochemical sensing properties.

PubMed

Megawati, Monica; Chua, Chun Kiang; Sofer, Zdenek; Klímová, Kateřina; Pumera, Martin

2017-06-21

Graphene, produced via chemical methods, has been widely applied for electrochemical sensing due to its structural and electrochemical properties as well as its ease of production in large quantity. While nitrogen-doped graphenes are widely studied materials, the literature showing an effect of graphene oxide preparation methods on nitrogen quantity and chemical states as well as on defects and, in turn, on electrochemical sensing is non-existent. In this study, the properties of nitrogen-doped graphene materials, prepared via hydrothermal synthesis using graphite oxide produced by various classical methods using permanganate or chlorate oxidants Staudenmaier, Hummers, Hofmann and Brodie oxidation methods, were studied; the resulting nitrogen-doped graphene oxides were labeled as ST-GO, HU-GO, HO-GO and BR-GO, respectively. The electrochemical oxidation of biomolecules, such as ascorbic acid, uric acid, dopamine, nicotinamide adenine nucleotide and DNA free bases, was carried out using cyclic voltammetry and differential pulse voltammetry techniques. The nitrogen content in doped graphene oxides increased in the order ST-GO < BR-GO < HO-GO < HU-GO. In the same way, the pyridinic form of nitrogen increased and the electrocatalytic effect of N-doped graphene followed this trend, as shown in the cyclic voltammograms. This is a very important finding that provides insight into the electrocatalytic effect of N-doped graphene. The nitrogen-doped graphene materials exhibited improved sensitivity over bare glassy carbon for ascorbic acid, uric acid and dopamine detection. These studies will enhance our understanding of the effects of graphite oxide precursors on the electrochemical sensing properties of nitrogen-doped graphene materials.

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

PubMed

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

2017-07-15

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

Poly arginine-graphene quantum dots as a biocompatible and non-toxic nanocomposite: Layer-by-layer electrochemical preparation, characterization and non-invasive malondialdehyde sensory application in exhaled breath condensate.

PubMed

Hasanzadeh, Mohammad; Mokhtari, Fozieh; Shadjou, Nasrin; Eftekhari, Aziz; Mokhtarzadeh, Ahad; Jouyban-Gharamaleki, Vahid; Mahboob, Soltanali

2017-06-01

This study reports on the electropolymerization of a low toxic and biocompatible polymer with entitle poly arginine-graphene quantum dots (PARG-GQDs) as a novel strategy for surface modification of glassy carbon (GC) surface and preparation a new interface for biomedical application. The fabrication of PARG-GQDs on GCE was performed using Layer-by-layer regime. Scanning electron microscopy (SEM) was confirmed dispersion of GQDs on the surface of PARG which lead to increase of surface coverage of PARG. The redox behavior of prepared sensor was then characterized by cyclic voltammetry (CV), differential pulse voltammetry (DPV) and chronoamperometry (CHA), square wave voltammetry (SWV), linear sweep voltammetry (LSV). The electroactivity of PARG-GQDs coating towards detection and determination of malondialdehyde (MDA) as one of the most common biomarkers of oxidative stress, was then studied. Then, application of prepared sensor for the detection of MDA in exhaled breath condensate (EBC) is described. Electrochemical based sensor shows the lower limit of quantification (LLOQ) were 0.329nanomolar. This work is the first report on the integration of GQDs to poly amino acids. Further development can lead to monitoring of MDA or other exhaled breath biomarkers by GQDs functionalized poly amino acids in EBC using electrochemical methods. Copyright © 2017. Published by Elsevier B.V.

Designing of fluorescent and magnetic imprinted polymer for rapid, selective and sensitive detection of imidacloprid via activators regenerated by the electron transfer-atom transfer radical polymerization (ARGET-ATRP) technique

NASA Astrophysics Data System (ADS)

Kumar, Sunil; Karfa, Paramita; Madhuri, Rashmi; Sharma, Prashant K.

2018-05-01

In this work, we report on a dual-behavior electrochemical/optical sensor for sensitive determination of Imidacloprid by fluorescent dye (fluorescein, FL) and imprinted polymer modified europium doped superparamagnetic iron oxide nanoparticles (FL@SPIONs@MIP). The imidacloprid (IMD)-imprinted polymer was directly synthesized on the Eu-SPIONs surface via Activators regenerated by the electron transfer-atom transfer radical polymerization (ARGET-ATRP) technique. Preparation, characterization and application of the prepared FL@SPIONs@MIP were systematically investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), vibrating sample magnetometer (VSM), fluorescence spectroscopy and electrochemical techniques. The electrochemical experiments exhibited a remarkable selectivity of the prepared sensor towards IMD. Determination of IMD by the square wave stripping voltammetry method represented a wide linear range of 0.059-0.791 μg L-1 with a detection limit of 0.0125 μg L-1. In addition, the fluorescence method shows a linear range of 0.039-0.942 μg L-1 and LOD of 0.0108 μg L-1. The fluorescence property of prepared FL@SPIONs@MIP was used for rapid, on-spot but selective detection of IMD in real samples. The proposed electrode displayed excellent repeatability and long-term stability and was successfully applied for quantitative and trace level determination of IMD in several real samples.

Facile synthesis of NiAl-layered double hydroxide/graphene hybrid with enhanced electrochemical properties for detection of dopamine

NASA Astrophysics Data System (ADS)

Li, Meixia; Zhu, Jun E.; Zhang, Lili; Chen, Xu; Zhang, Huimin; Zhang, Fazhi; Xu, Sailong; Evans, David G.

2011-10-01

Layered double hydroxides (LDHs), also known as hydrotalcite-like anionic clays, have been investigated widely as promising electrochemical active materials. Due to the inherently weak conductivity, the electrochemical properties of LDHs were improved typically by utilization of either functional molecules intercalated between LDH interlayer galleries, or proteins confined between exfoliated LDH nanosheets. Here, we report a facile protocol to prepare NiAl-LDH/graphene (NiAl-LDH/G) nanocomposites using a conventional coprecipitation process under low-temperature conditions and subsequent reduction of the supporting graphene oxide. Electrochemical tests showed that the NiAl-LDH/G modified electrode exhibited highly enhanced electrochemical performance of dopamine electrooxidation in comparison with the pristine NiAl-LDH modified electrode. Results of high-resolution transmission electron microscopy and Raman spectra provide convincing information on the nanostructure and composition underlying the enhancement. Our results of the NiAl-LDH/G modified electrodes with the enhanced electrochemical performance may allow designing a variety of promising hybrid sensors via a simple and feasible approach.Layered double hydroxides (LDHs), also known as hydrotalcite-like anionic clays, have been investigated widely as promising electrochemical active materials. Due to the inherently weak conductivity, the electrochemical properties of LDHs were improved typically by utilization of either functional molecules intercalated between LDH interlayer galleries, or proteins confined between exfoliated LDH nanosheets. Here, we report a facile protocol to prepare NiAl-LDH/graphene (NiAl-LDH/G) nanocomposites using a conventional coprecipitation process under low-temperature conditions and subsequent reduction of the supporting graphene oxide. Electrochemical tests showed that the NiAl-LDH/G modified electrode exhibited highly enhanced electrochemical performance of dopamine electrooxidation in comparison with the pristine NiAl-LDH modified electrode. Results of high-resolution transmission electron microscopy and Raman spectra provide convincing information on the nanostructure and composition underlying the enhancement. Our results of the NiAl-LDH/G modified electrodes with the enhanced electrochemical performance may allow designing a variety of promising hybrid sensors via a simple and feasible approach. Electronic supplementary information (ESI) available: Fig. S1 showing 2D fast Fourier transform (FFT) image of NiAl-LDH phase in NiAl-LDH/G composites, and Fig. S2 showing CV curve of the pristine G modified electrode. See DOI: 10.1039/c1nr10592b.

Preparation of porous nitrogen-doped titanium dioxide microspheres and a study of their photocatalytic, antibacterial and electrochemical activities

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, S.; Chu, W., E-mail: chuwei65@yahoo.com.cn; Huang, Y.Y.

Graphical abstract: Porous N-doped TiO{sub 2} microspheres were prepared for the first time via plasma technique. The sample exhibited better photocatalytic activity, photoinduced inactivation activity and better electrochemical activity than those of TiO{sub 2} microspheres and P25. Display Omitted Highlights: ► Porous N-doped TiO{sub 2} microspheres were prepared via nitrogen plasma technique. ► Plasma treatment did not affect the porous structure of the TiO{sub 2} microspheres. ► With the plasma treatment, the N contents in the samples increased. ► Their photocatalytic, antibacterial and electrochemical activities were studied. -- Abstract: Nitrogen-doped titanium dioxide (N-doped TiO{sub 2}) microspheres with porous structure weremore » prepared via the nitrogen-assisted glow discharge plasma technique at room temperature for the first time. The samples were characterized by X-ray diffraction, scanning electron microscopy, nitrogen adsorption–desorption measurement, UV–Vis diffuse reflectance spectra, photoluminescence spectroscopy and X-ray photoelectron spectroscopy. The results indicated that the plasma treatment did not affect the porous structure of the TiO{sub 2} microspheres. With the plasma treatment, the N contents in the samples increased. During the photocatalytic degradation of methylene blue under simulative sunlight irradiation, the sample after plasma treatment for 60 min (N-TiO{sub 2}-60) exhibited higher photocatalytic activity than those of the TiO{sub 2} microspheres, P25 and other N-doped TiO{sub 2} microspheres. Furthermore, the N-TiO{sub 2}-60 showed excellent antibacterial activities towards Escherichia coli under visible irradiation. These should be attributed to the enhancement of the visible light region absorption for TiO{sub 2} after N-doping. Electrochemical data demonstrated that the N-doping not only enhanced the electrochemical activity of TiO{sub 2}, but also improved the reversibility of Li insertion/extraction reactions and the rate behavior of TiO{sub 2} during charge–discharge cycles.« less

Shape control VO2 nanorods prepared by soft chemistry and electrochemical method

NASA Astrophysics Data System (ADS)

Simo, A.; Sibanyoni, J.; Fuku, X.; Numan, N.; Omorogbe, S.; Maaza, M.

2018-07-01

"Bottom up" approach is of primary interest for chemistry and materials science because the fundamental building blocks are atoms. Thus colloidal chemical synthetic methods can be utilized to prepare uniform nanocrystals with controlled particle size. In the following work of study, thermochromic VO2 nanostructures were prepared by hydrothermal technique soft chemistry. We concentrate on solution phase synthetic methods that enable a proper shape and size control of metal oxide nanocrystals. Their structural properties were studied by Scanning Electron Microscopy (SEM), Fourier Transform IR (FTIR) and Differential Scanning Calorimetry (DSC). It is demonstrated that the surfactant assistance (NaOH) has great influence on the morphology-control of the material. Electrochemical properties of the nanospheres show good stability after 20 cycles and the surface diffusion coefficient was calculated to be 5 × 10-6 cm2 s-1.

Graphene-based electrochemical energy conversion and storage: fuel cells, supercapacitors and lithium ion batteries.

PubMed

Hou, Junbo; Shao, Yuyan; Ellis, Michael W; Moore, Robert B; Yi, Baolian

2011-09-14

Graphene has attracted extensive research interest due to its strictly 2-dimensional (2D) structure, which results in its unique electronic, thermal, mechanical, and chemical properties and potential technical applications. These remarkable characteristics of graphene, along with the inherent benefits of a carbon material, make it a promising candidate for application in electrochemical energy devices. This article reviews the methods of graphene preparation, introduces the unique electrochemical behavior of graphene, and summarizes the recent research and development on graphene-based fuel cells, supercapacitors and lithium ion batteries. In addition, promising areas are identified for the future development of graphene-based materials in electrochemical energy conversion and storage systems. This journal is © the Owner Societies 2011

Electrochemical analysis in a liposome suspension using lapachol as a hydrophobic electro active species.

PubMed

Okumura, Noriko; Wakamatsu, Shiori; Uno, Bunji

2014-01-01

This study demonstrated that the electro-chemical analysis of hydrophobic quinones can be performed in liposome suspension systems. We prepared and analyzed liposome suspensions containing lapachol, which is a quinone-based anti-tumor activity compound. In this suspension system, a simple one redox couple of lapachol is observed. These results are quite different from those obtained in organic solvents. In addition, the pH dependence of redox behaviors of lapachol could be observed in multilamellar vesicle (MLV) suspension system. This MLV suspension system method may approximate the electrochemical behavior of hydrophobic compounds in aqueous conditions. A benefit of this liposome suspension system for electrochemical analysis is that it enables to observe water-insoluble compounds without using organic solvents.

The influence of surface roughness and high pressure torsion on the growth of anodic titania nanotubes on pure titanium

NASA Astrophysics Data System (ADS)

Hu, Nan; Gao, Nong; Starink, Marco J.

2016-11-01

Anodic titanium dioxide nanotube (TNT) arrays have wide applications in photocatalytic, catalysis, electronics, solar cells and biomedical implants. When TNT coatings are combined with severe plastic deformation (SPD), metal processing techniques which efficiently improve the strength of metals, a new generation of biomedical implant is made possible with both improved bulk and surface properties. This work investigated the effect of processing by high pressure torsion (HPT) and different mechanical preparations on the substrate and subsequently on the morphology of TNT layers. HPT processing was applied to refine the grain size of commercially pure titanium samples and substantially improved their strength and hardness. Subsequent anodization at 30 V in 0.25 wt.% NH4F for 2 h to form TNT layers on sample surfaces prepared with different mechanical preparation methods was carried out. It appeared that the local roughness of the titanium surface on a microscopic level affected the TNT morphology more than the macroscopic surface roughness. For HPT-processed sample, the substrate has to be pre-treated by a mechanical preparation finer than 4000 grit for HPT to have a significant influence on TNTs. During the formation of TNT layers the oxide dissolution rate was increased for the ultrafine-grained microstructure formed due to HPT processing.

A Diamond in the Rough: Carat's Organizational and Administrative Leadership (COAL) Program

ERIC Educational Resources Information Center

Brown, Kathleen M.; Schainker, Stanley A.

2006-01-01

A diamond is a chunk of coal that stood up under pressure. Carat's Organizational and Administrative Leadership (COAL) program is a diamond in the rough--experiencing strong political pressure from multiple sides. As the state's premiere educational leadership preparation program, expectations are high. While striving to live up to its national…

Uniform manganese hexacyanoferrate hydrate nanocubes featuring superior performance for low-cost supercapacitors and nonenzymatic electrochemical sensors.

PubMed

Pang, Huan; Zhang, Yizhou; Cheng, Tao; Lai, Wen-Yong; Huang, Wei

2015-10-14

Uniform manganese hexacyanoferrate hydrate nanocubes are prepared via a simple chemical precipitation method at room temperature. Due to both micro/mesopores of the Prussian blue analogue and nanocubic structures, the manganese hexacyanoferrate hydrate nanocubes allow the efficient charge transfer and mass transport for electrolyte solution and chemical species. Thus, the manganese hexacyanoferrate hydrate nanocube electrode shows a good rate capability and cycling stability for electrochemical capacitors. Furthermore, electrodes modified with manganese hexacyanoferrate hydrate nanocubes demonstrate a sensitive electrochemical response to hydrogen peroxide (H2O2) in buffer solutions with a high selectivity.

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

NASA Astrophysics Data System (ADS)

Tao, Ying; Yi, Danqing; Zhu, Baojun

2013-04-01

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

Rapid microwave-assisted preparation of binary and ternary transition metal sulfide compounds

DOE Office of Scientific and Technical Information (OSTI.GOV)

Butala, Megan M.; Perez, Minue A.; Arnon, Shiri

Transition metal chalcogenides are of interest for energy applications, including energy generation in photoelectrochemical cells and as electrodes for next-generation electrochemical energy storage. Synthetic routes for such chalcogenides typically involve extended heating at elevated temperatures for multiple weeks. We demonstrate here the feasibility of rapidly preparing select sulfide compounds in a matter of minutes, rather than weeks, using microwave-assisted heating in domestic microwaves. We report the preparations of phase pure FeS2, CoS2, and solid solutions thereof from the elements with only 40 min of heating. Conventional furnace and rapid microwave preparations of CuTi2S4 both result in a majority of themore » targeted phase, even with the significantly shorter heating time of 40 min for microwave methods relative to 12 days using a conventional furnace. The preparations we describe for these compounds can be extended to related structures and chemistries and thus enable rapid screening of the properties and performance of various compositions of interest for electronic, optical, and electrochemical applications.« less

Fabrication of advanced electrochemical energy materials using sol-gel processing techniques

NASA Technical Reports Server (NTRS)

Chu, C. T.; Chu, Jay; Zheng, Haixing

1995-01-01

Advanced materials play an important role in electrochemical energy devices such as batteries, fuel cells, and electrochemical capacitors. They are being used as both electrodes and electrolytes. Sol-gel processing is a versatile solution technique used in fabrication of ceramic materials with tailored stoichiometry, microstructure, and properties. The application of sol-gel processing in the fabrication of advanced electrochemical energy materials will be presented. The potentials of sol-gel derived materials for electrochemical energy applications will be discussed along with some examples of successful applications. Sol-gel derived metal oxide electrode materials such as V2O5 cathodes have been demonstrated in solid-slate thin film batteries; solid electrolytes materials such as beta-alumina for advanced secondary batteries had been prepared by the sol-gel technique long time ago; and high surface area transition metal compounds for capacitive energy storage applications can also be synthesized with this method.

Electrochemical Analysis of Neurotransmitters

NASA Astrophysics Data System (ADS)

Bucher, Elizabeth S.; Wightman, R. Mark

2015-07-01

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

Fabrication of luminescent SrWO{sub 4} thin films by a novel electrochemical method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen Lianping; Gao Yuanhong

2007-10-02

Highly crystallized SrWO{sub 4} thin films with single scheelite structure were prepared within 60 min by a cell electrochemical method. X-ray diffraction analysis shows that SrWO{sub 4} thin films have a tetragonal structure. Scanning electron microscopy examinations reveal that SrWO{sub 4} grains grow well in tetragonal tapers and grains like flowers or bunches, which can usually form by using the electrolysis electrochemical method, have disappeared under cell electrochemical conditions. X-ray photoelectron spectra and energy dispersive X-ray microanalysis examinations demonstrate that the composition of the film is consistent with its stoichiometry. These SrWO{sub 4} films show a single blue emission peakmore » (located at 460 nm) using an excitation wave of 230 nm. The speed of cell electrochemical method can be controlled by changing temperature. The optimum treatment temperature is about 50-60 deg. C.« less

Electrochemical Analysis of Neurotransmitters

PubMed Central

Bucher, Elizabeth S.; Wightman, R. Mark

2016-01-01

Chemical signaling through the release of neurotransmitters into the extracellular space is the primary means of communication between neurons. More than four decades ago, Ralph Adams and his colleagues realized the utility of electrochemical methods for the study of easily oxidizable neurotransmitters, such as dopamine, norepinephrine, and serotonin and their metabolites. Today, electrochemical techniques are frequently coupled to microelectrodes to enable spatially resolved recordings of rapid neurotransmitter dynamics in a variety of biological preparations spanning from single cells to the intact brain of behaving animals. In this review, we provide a basic overview of the principles underlying constant-potential amperometry and fast-scan cyclic voltammetry, the most commonly employed electrochemical techniques, and the general application of these methods to the study of neurotransmission. We thereafter discuss several recent developments in sensor design and experimental methodology that are challenging the current limitations defining the application of electrochemical methods to neurotransmitter measurements. PMID:25939038

Synthesis, Optical and Electrochemical Properties of Y2O3 Nanoparticles Prepared by Co-Precipitation Method.

PubMed

Saravanan, Thulasingam; Raj, Srinivasan Gokul; Chandar, Nagamuthu Raja Krishna; Jayavel, Ramasamy

2015-06-01

Y2O3 nanoparticles were synthesized by co-precipitation route using yttrium nitrate hexahydrate and ammonium hydroxide as precursors. The prepared sample was calcined at 500 degrees C and subjected to various characterization studies like thermal analysis (TG/DTA), X-ray diffraction (XRD), transmission electron microscope (TEM), UV-visible (UV-Vis) and photoluminescence (PL) spectroscopy. The XRD pattern showed the cubic fluorite structure of Y2O3 without any impurity peaks, revealing high purity of the prepared sample. TEM images revealed that the calcined Y2O3 nanoparticles consist of spherical-like morphology with an average particle size of 12 nm. The absorption spectrum of calcined samples shows blue-shift compared to the as-prepared sample, which was further confirmed by PL studies. The possible formation mechanism of Y2O3 nanoparticles has been discussed based on the experimental results. Electrochemical behavior of Y2O3 nanoparticles was studied by cyclic voltammetry to assess their suitability for supercapacitor applications.

Hydroxyapatite with Permanent Electrical Polarization: Preparation, Characterization, and Response against Inorganic Adsorbates.

PubMed

Rivas, Manuel; Del Valle, Luis J; Armelin, Elaine; Bertran, Oscar; Turon, Pau; Puiggalí, Jordi; Alemán, Carlos

2018-04-16

Permanently polarized hydroxyapatite (HAp) particles have been prepared by applying a constant DC of 500 V at 1000 °C for 1 h to the sintered mineral. This process causes important chemical changes, as the formation of OH - defects (vacancies), the disappearance of hydrogenophosphate ions at the mineral surface layer, and structural variations reflected by the increment of the crystallinity. As a consequence, the electrochemical properties and electrical conductivity of the polarized mineral increase noticeably compared with as-prepared and sintered samples. Moreover, these increments remain practically unaltered after several months. In addition, permanent polarization favours significantly the ability of HAp to adsorb inorganic bioadsorbates in comparison with as-prepared and sintered samples. The adsorbates cause a significant increment of the electrochemical stability and electrical conductivity with respect to bare polarized HAp, which may have many implications for biomedical applications of permanently polarized HAp. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Chronoamperometric study of mild steel pitting in sodium sulfide aqueous solution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Otero, T.F.; Achucarro, C.

1994-08-01

Mild steel samples were studied by chronoamperometry in sodium sulfide (Na[sub 2]S) aqueous solution. Pit nucleation and growth also were monitored by optical microscopy. The influence of variables such as temperature, polarization potential, surface roughness, the presence of electrochemically generated oxide layers, and the simultaneous presence of potassium hydroxide (KOH) was studied. The influence of each parameter on pit shape and growth was reviewed. Different reactions and competitive processes were proposed based on the experimental results.

Hemispherical cavities on silicon substrates: an overview of micro fabrication techniques

NASA Astrophysics Data System (ADS)

Poncelet, O.; Rasson, J.; Tuyaerts, R.; Coulombier, M.; Kotipalli, R.; Raskin, J.-P.; Francis, L. A.

2018-04-01

Hemispherical photonic crystals found in species like Papilio blumei and Cicendella chinensis have inspired new applications like anti-counterfeiting devices and gas sensors. In this work, we investigate and compare four different ways to micro fabricate such hemispherical cavities: using colloids as template, by wet (HNA) or dry (XeF2) isotropic etching of silicon and by electrochemical etching of silicon. The shape and the roughness of the obtained cavities have been discussed and the pros/cons for each method are highlighted.

In vitro selection of electrochemical peptide probes using bioorthogonal tRNA for influenza virus detection.

PubMed

K C, Tara Bahadur; Tada, Seiichi; Zhu, Liping; Uzawa, Takanori; Minagawa, Noriko; Luo, Shyh-Chyang; Zhao, Haichao; Yu, Hsiao-Hua; Aigaki, Toshiro; Ito, Yoshihiro

2018-05-17

An electrosensitive peptide probe has been developed from an in vitro selection technique using biorthogonal tRNA prepared with an electroreactive non-natural amino acid, 3,4-ethylenedioxythiophene-conjugated aminophenylalanine. The selected probe quantitatively detected the influenza virus based on a signal "turn-on" mechanism. The developed strategy could be used to develop electrochemical biosensors toward a variety of targets.

Electrochemical preparation of tris(tert-butyldimethylsilyl)cyclopropene and its hydride abstraction to tris(tert-butyldimethylsilyl)cyclopropenium tetrafluoroborate

PubMed Central

Buchholz, Herwig A.; Prakash, G. K. Surya; Deffieux, Denis; Olah, George A.

1999-01-01

Electrochemical reductive tert-butyldimethylsilylation of tetrachlorocyclopropene to 1,2,3-tris(tert-butyldimethylsilyl)cyclopropene, a potential strained precursor for Diels–Alder and related cycloaddition reactions, is described. By hydride abstraction with nitrosonium tetrafluoroborate, 1,2,3-tris(tert-butyldimethylsilyl)cyclopropene is ionized quantitatively to Hückeloid 2π aromatic tris(tert-butyldimethylsilyl)cyclopropenium tetrafluoroborate. PMID:10468551

Measuring Skew in Average Surface Roughness as a Function of Surface Preparation

NASA Technical Reports Server (NTRS)

Stahl, Mark T.

2015-01-01

Characterizing surface roughness is important for predicting optical performance. Better measurement of surface roughness reduces grinding saving both time and money and allows the science requirements to be better defined. In this study various materials are polished from a fine grind to a fine polish. Each sample's RMS surface roughness is measured at 81 locations in a 9x9 square grid using a Zygo white light interferometer at regular intervals during the polishing process. Each data set is fit with various standard distributions and tested for goodness of fit. We show that the skew in the RMS data changes as a function of polishing time.

Rough SERS substrate based on gold coated porous silicon layer prepared on the silicon backside surface

NASA Astrophysics Data System (ADS)

Dridi, H.; Haji, L.; Moadhen, A.

2017-04-01

We report in this paper a novel method to elaborate rough Surface Enhanced Raman Scattering (SERS) substrate. A single layer of porous silicon was formed on the silicon backside surface. Morphological characteristics of the porous silicon layer before and after gold deposition were influenced by the rough character (gold size). The reflectance measurements showed a dependence of the gold nano-grains size on the surface nature, through the Localized Surface Plasmon (LSP) band properties. SERS signal of Rhodamine 6G used as a model analyte, adsorbed on the rough porous silicon layer revealed a marked enhancement of its vibrational modes intensities.

Formation of Sn-M (M=Fe, Al, Ni) alloy nanoparticles by DC arc-discharge and their electrochemical properties as anodes for Li-ion batteries

NASA Astrophysics Data System (ADS)

Gao, Song; Huang, Hao; Wu, Aimin; Yu, Jieyi; Gao, Jian; Dong, Xinglong; Liu, Chunjing; Cao, Guozhong

2016-10-01

A direct current arc-discharge method was applied to prepare the Sn-M (M=Fe, Al, Ni) bi-alloy nanoparticles. Thermodynamic is introduced to analyze the energy circumstances for the formation of the nanoparticles during the physical condensation process. The electrochemical properties of as-prepared Sn-M alloy nanoparticles are systematically investigated as anodes of Li-ion batteries. Among them, Sn-Fe nanoparticles electrode exhibits high Coulomb efficiency (about 71.2%) in the initial charge/discharge (257.9 mA h g-1/366.6 mA h g-1) and optimal cycle stability (a specific reversible capacity of 240 mA h g-1 maintained after 20 cycles) compared with others. Large differences in the electrochemical behaviors indicate that the chemical composition and microstructure of the nanoparticles determine the lithium-ion storage properties and the long-term cyclic stability during the charge/discharge process.

Raman structural studies of the nickel electrode

NASA Technical Reports Server (NTRS)

Cornilsen, B. C.

1985-01-01

Raman spectroscopy is sensitive to empirically controlled nickel electrode structural variations, and has unique potential for structural characterization of these materials. How the structure relates to electrochemical properties is examined so that the latter can be more completely understood, controlled, and optimized. Electrodes were impregnated and cycled, and cyclic voltammetry is being used for electrochemical characterization. Structural variation was observed which has escaped detection using other methods. Structural changes are induced by: (1) cobalt doping, (2) the state of change or discharge, (3) the preparation conditions and type of buffer used, and (4) the formation process. Charged active mass has an NiOOH-type structure, agreeing with X-ray diffraction results. Discharged active mass, however, is not isostructural with beta-Ni(OH)2. Chemically prepared alpha phases are not isostructural either. A disordered structural model, containing point defects, is proposed for the cycled materials. This model explains K(+) incorporation. Band assignments were made and spectra interpreted for beta-Ni(OH)2, electrochemical NiOOH and chemically precipitated NiOOH.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liang, Kun; Marcus, Kyle; Yang, Zhenzhong

In this work, a freestanding NiFe oxyfluoride (NiFeOF) holey film was prepared by electrochemical deposition and anodic treatments. With the combination of good electrical conductivity and holey structure, the NiFeOF holey film offers superior electrochemical performance, due to the following reasons: (i) The residual metal alloy framework can be used as the current collector to improve electrode conductivity. Moreover, the as-prepared freestanding NiFeOF holey film can be used as a supercapacitor electrode without reliance on binders and other additives. The residual metal alloy framework and binder-free electrode effectively reduces electrode resistance, thus improving electron transport. (ii) The highly interconnected holeymore » structure and hierarchical pore distribution provides a high specific surface area to improve electron transport, enhancing rapid ion transport and mitigating diffusion limitations throughout the holey film. (iii) The excellent mechanical characteristics facilitate flexibility and cyclability related performance. Additionally, the NiFeOF holey film presents exceptional electrochemical performance, showing that it is a promising alternative for small/micro-size electronic devices.« less

Novel secondary assembled micro/nano porous spheres ZnCo2O4 with superior electrochemical performances as lithium ion anode material.

PubMed

Liu, Haowen; Hu, Qihong

2018-08-10

In this work, novel secondary assembled micro/nano porous spheres ZnCo 2 O 4 were firstly prepared by combining the hydrothermal method with post-synthesis calcinations. The structure and morphology of the obtained powder were characterized by x-ray powder diffraction and field emission-scanning electron microscopy. As the anode material of lithium-ion half-cells, the as-prepared ZnCo 2 O 4 delivered a very high capacity, extra cycling stability and excellent rate capability. A discharge capacity of 950 mAh g -1 with up to 99.7% retention corresponding to the second cycle at 0.1 C was achieved after 90 cycles, which was an improved cyclability over previous reports. The higher current charge-discharge and electrochemical impedance spectroscopy data indicate that the material's integrity was maintained. Therefore constructing the secondary assembled 3D micro/nano structure is an effective strategy to obtain the superior electrochemical performances.

Facile preparation and enhanced capacitance of the polyaniline/sodium alginate nanofiber network for supercapacitors.

PubMed

Li, Yingzhi; Zhao, Xin; Xu, Qian; Zhang, Qinghua; Chen, Dajun

2011-05-17

A porous and mat-like polyaniline/sodium alginate (PANI/SA) composite with excellent electrochemical properties was polymerized in an aqueous solution with sodium sulfate as a template. Ultraviolet-visible spectra, X-ray diffraction pattern, and Fourier transform infrared spectra were employed to characterize the PANI/SA composite, indicating that the PANI/SA composite was successfully prepared. The PANI/SA nanofibers with uniform diameters from 50 to 100 nm can be observed on scanning electron microscopy. Cyclic voltammetry and galvanostatic charge/discharge tests were carried out to investigate the electrochemical properties. The PANI/SA nanostructure electrode exhibits an excellent specific capacitance as high as 2093 F g(-1), long cycle life, and fast reflect of oxidation/reduction on high current changes. The remarkable electrochemical characteristic is attributed to the nanostructured electrode materials, which generates a high electrode/electrolyte contact area and short path lengths for electronic transport and electrolyte ion. The approach is simple and can be easily extended to fabricate nanostructural composites for supercapacitor electrode materials.

Hydrothermal synthesis of flower-like MoS2 nanospheres for electrochemical supercapacitors.

PubMed

Zhou, Xiaoping; Xu, Bin; Lin, Zhengfeng; Shu, Dong; Ma, Lin

2014-09-01

Flower-like MoS2 nanospheres were synthesized by a hydrothermal route. The structure and surface morphology of the as-prepared MoS2 was characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The supercapacitive behavior of MoS2 in 1 M KCl electrolyte was studied by means of cyclic voltammetry (CV), constant current charge-discharge cycling (CD) and electrochemical impedance spectroscopy (EIS). The XRD results indicate that the as-prepared MoS2 has good crystallinity. SEM images show that the MoS2 nanospheres have uniform sizes with mean diameter about 300 nm. Many nanosheets growing on the surface make the MoS2 nanospheres to be a flower-like structure. The specific capacitance of MoS2 is 122 F x g(-1) at 1 A x g(-1) or 114 F x g(-1) at 2 mv s(-1). All the experimental results indicate that MoS2 is a promising electrode material for electrochemical supercapacitors.

Corrosion resistance of premodeled wires made of stainless steel used for heart electrotherapy leaders

NASA Astrophysics Data System (ADS)

Przondziono, J.; Walke, W.; Młynarski, R.; Szatka, W.

2012-05-01

The purpose of the study is to evaluate resistance to electrochemical corrosion of wire made of X10CrNi18-8 stainless steel designed for use in cardiology treatment. The influence of strain formed in the premodeling process and methods of wire surface preparation to corrosive resistance in artificial plasma solution were analysed. Wire corrosion tests were carried out in the solution of artificial plasma. Resistance to electrochemical corrosion was evaluated on the ground of recorded curves of anodic polarization by means of potentiodynamic method. Potentiodynamic tests carried out enabled to determine how the resistance to pitting corrosion of wire changes, depending on strain formed in the premodeling process as well as on the method of wire surface preparation. For evaluation of phenomena occurring on the surface of tested steel, electrochemical impedance spectroscopy (EIS) was applied. Deterioration of corrosive properties of wire along with the increase in the formed strain hardening was observed.

Influence of electrode preparation on the electrochemical performance of LiNi0.8Co0.15Al0.05O2 composite electrodes for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Tran, Hai Yen; Greco, Giorgia; Täubert, Corina; Wohlfahrt-Mehrens, Margret; Haselrieder, Wolfgang; Kwade, Arno

2012-07-01

The electrode manufacturing for lithium-ion batteries is based on a complex process chain with several influencing factors. A proper tailoring of the electrodes can greatly improve both the electrochemical performances and the energy density of the battery. In the present work, some significant parameters during the preparation of LiNi0.8Co0.15Al0.05O2-based cathodes were investigated. The active material was mixed with a PVDF-binder and two conductive additives in different ratios. The electrode thickness, the degree of compacting and the conductive agent type and mixing ratio have proven to have a strong impact on the electrochemical performances of the composite electrodes, especially on their behaviour at high C-rates. Further it has been shown that the compacting has an essential influence on the mechanical properties of NCA coatings, according to their total, ductile and elastic deformation behaviour.

Microwave plasma-assisted chemical vapor deposition of porous carbon film as supercapacitive electrodes

NASA Astrophysics Data System (ADS)

Wu, Ai-Min; Feng, Chen-Chen; Huang, Hao; Paredes Camacho, Ramon Alberto; Gao, Song; Lei, Ming-Kai; Cao, Guo-Zhong

2017-07-01

Highly porous carbon film (PCF) coated on nickel foam was prepared successfully by microwave plasma-assisted chemical vapor deposition (MPCVD) with C2H2 as carbon source and Ar as discharge gas. The PCF is uniform and dense with 3D-crosslinked nanoscale network structure possessing high degree of graphitization. When used as the electrode material in an electrochemical supercapacitor, the PCF samples verify their advantageous electrical conductivity, ion contact and electrochemical stability. The test results show that the sample prepared under 1000 W microwave power has good electrochemical performance. It displays the specific capacitance of 62.75 F/g at the current density of 2.0 A/g and retains 95% of its capacitance after 10,000 cycles at the current density of 2.0 A/g. Besides, its near-rectangular shape of the cyclic voltammograms (CV) curves exhibits typical character of an electric double-layer capacitor, which owns an enhanced ionic diffusion that can fit the requirements for energy storage applications.

Synthesis and electrochemical properties of olivine LiFePO 4 prepared by a carbothermal reduction method

NASA Astrophysics Data System (ADS)

Liu, Hui-ping; Wang, Zhi-xing; Li, Xin-hai; Guo, Hua-jun; Peng, Wen-jie; Zhang, Yun-he; Hu, Qi-yang

LiFePO 4/C composite cathode material was prepared by carbothermal reduction method, which uses NH 4H 2PO 4, Li 2CO 3 and cheap Fe 2O 3 as starting materials, acetylene black and glucose as carbon sources. The precursor of LiFePO 4/C was characterized by differential thermal analysis and thermogravimetry. X-ray diffraction (XRD), scanning electron microscopy (SEM) micrographs showed that the LiFePO 4/C is olivine-type phase, and the addition of the carbon reduced the LiFePO 4 grain size. The carbon is dispersed between the grains, ensuring a good electronic contact. The products sintered at 700 °C for 8 h with glucose as carbon source possessed excellent electrochemical performance. The synthesized LiFePO 4 composites showed a high electrochemical capacity of 159.3 mAh g -1 at 0.1 C rate, and the capacity fading is only 2.2% after 30 cycles.

Impedance nanopore biosensor: influence of pore dimensions on biosensing performance.

PubMed

Kant, Krishna; Yu, Jingxian; Priest, Craig; Shapter, Joe G; Losic, Dusan

2014-03-07

Knowledge about electrochemical and electrical properties of nanopore structures and the influence of pore dimensions on these properties is important for the development of nanopore biosensing devices. The aim of this study was to explore the influence of nanopore dimensions (diameter and length) on biosensing performance using non-faradic electrochemical impedance spectroscopy (EIS). Nanoporous alumina membranes (NPAMs) prepared by self-ordered electrochemical anodization of aluminium were used as model nanopore sensing platforms. NPAMs with different pore diameters (25-65 nm) and lengths (4-18 μm) were prepared and the internal pore surface chemistry was modified by covalently attaching streptavidin and biotin. The performance of this antibody nanopore biosensing platform was evaluated using various concentrations of biotin as a model analyte. EIS measurements of pore resistivity and conductivity were carried out for pores with different diameters and lengths. The results showed that smaller pore dimensions of 25 nm and pore lengths up to 10 μm provide better biosensing performance.

Chip-based generation of carbon nanodots via electrochemical oxidation of screen printed carbon electrodes and the applications for efficient cell imaging and electrochemiluminescence enhancement

NASA Astrophysics Data System (ADS)

Xu, Yuanhong; Liu, Jingquan; Zhang, Jizhen; Zong, Xidan; Jia, Xiaofang; Li, Dan; Wang, Erkang

2015-05-01

A portable lab-on-a-chip methodology to generate ionic liquid-functionalized carbon nanodots (CNDs) was developed via electrochemical oxidation of screen printed carbon electrodes. The CNDs can be successfully applied for efficient cell imaging and solid-state electrochemiluminescence sensor fabrication on the paper-based chips.A portable lab-on-a-chip methodology to generate ionic liquid-functionalized carbon nanodots (CNDs) was developed via electrochemical oxidation of screen printed carbon electrodes. The CNDs can be successfully applied for efficient cell imaging and solid-state electrochemiluminescence sensor fabrication on the paper-based chips. Electronic supplementary information (ESI) available: Experimental section; Fig. S1. XPS spectra of the as-prepared CNDs after being dialyzed for 72 hours; Fig. S2. LSCM images showing time-dependent fluorescence signals of HeLa cells treated by the as-prepared CNDs; Tripropylamine analysis using the Nafion/CNDs modified ECL sensor. See DOI: 10.1039/c5nr01765c

In-situ preparation and unique electrochemical behavior of pore-embedding CoO/Co3O4 intermixed composite for Li+ rechargeable battery electrodes

NASA Astrophysics Data System (ADS)

Kim, Jin Kyu; Ju, Ji Young; Choi, Seul Ki; Unithrattil, Sanjith; Lee, Sun Sook; Kang, Yongku; Kim, Yongseon; Im, Won Bin; Choi, Sungho

2018-02-01

Electrochemically active CoO/Co3O4 co-existing microspheres with morphology-inherited porous particles is successfully synthesized via a simple solvothermal method. The as-prepared intermixed composite undergoes a monoxide CoO-preferred conversion reaction with an extremely enhanced capacity retention, ∼905 mA h g-1 after 250 cycles for discharge state, which is 1.6 times higher than the conventional CoOx-based anodes. Moreover, stable catalytic behavior of the electrocatalysts in Li-air cathodes of the given composites is also demonstrated. We believe that the extraordinarily enhanced electrode performance might be due to the novel pore-tempered microspheres packed with double electrochemically active centers of the CoO/Co3O4 composite effectively confine the detrimental volume exchange during the reversible cyclic reactions as well as the preserved multiple reactive sites for a reversible Li+ ⇄ LiOx reaction, which is advantageous for advanced Li rechargeable battery.

Synthesis and characterization of Cu3Se2 nanofilms by an underpotential deposition based electrochemical codeposition technique

NASA Astrophysics Data System (ADS)

Aydın, Zehra Yazar; Abacı, Serdar

2017-12-01

The Cu3Se2 nanofilms were synthesized with underpotential deposition based electrochemical codeposition technique for the first time in the literature. The electrochemical behaviors of copper and selenium were investigated in 0.1 M H2SO4 on Au electrode. The effects of concentration and scan rate on the electrochemical behavior of selenium were studied. The electrochemical behaviors in underpotential deposition and bulk regions of the Cu-Se system were investigated in acidic solution by cyclic voltammetry and electrolysis techniques. X-ray photoelectron spectroscopy, scanning electron microscopy, atomic force microscopy, X-ray diffraction, Raman spectroscopy, and ultraviolet and visible absorption spectroscopy techniques were used for characterization of synthesized films. According to the X-ray photoelectron spectroscopy spectrum, Cu/Se ratio was determined to be approximately 3/2. Copper selenide nanofilms are two phases and polycrystalline according to X-ray diffraction. The films mainly formed tetragonal Cu3Se2 (umangite mineral structure) structure and the particle size was approximately 45.95 nm. Scanning electron microscopy images showed that Cu3Se2 nanofilms consisted of uniform, nano-sizes and two-dimensional. It was found through AFM that the surface roughness of the film was 6.173 nm, with a mean particle size of around 50 nm. Depending on the deposition time, the band gaps of the Cu3Se2 films were in the range of 2.86-3.20 eV. Three characteristic vibrational modes belonging to Cu3Se2 nanofilms were recorded in the Raman spectrum.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mistry, Hemma; Varela, Ana Sofia; Bonifacio, Cecile S.

There is an urgent need to develop technologies that use renewable energy to convert waste products such as carbon dioxide into hydrocarbon fuels. Carbon dioxide can be electrochemically reduced to hydrocarbons over copper catalysts, although higher efficiency is required. We have developed oxidized copper catalysts displaying lower overpotentials for carbon dioxide electroreduction and record selectivity towards ethylene (60%) through facile and tunable plasma treatments. Herein we provide insight into the improved performance of these catalysts by combining electrochemical measurements with microscopic and spectroscopic characterization techniques. Operando X-ray absorption spectroscopy and cross-sectional scanning transmission electron microscopy show that copper oxides aremore » surprisingly resistant to reduction and copper + species remain on the surface during the reaction. Furthermore, our results demonstrate that the roughness of oxide-derived copper catalysts plays only a partial role in determining the catalytic performance, while the presence of copper + is key for lowering the onset potential and enhancing ethylene selectivity.« less

Aluminium Electrodeposition from Ionic Liquid: Effect of Deposition Temperature and Sonication †

PubMed Central

Berretti, Enrico; Giaccherini, Andrea; Martinuzzi, Stefano M.; Innocenti, Massimo; Schubert, Thomas J.S.; Stiemke, Frank M.; Caporali, Stefano

2016-01-01

Since their discovery, ionic liquids (ILs) have attracted a wide interest for their potential use as a medium for many chemical processes, in particular electrochemistry. As electrochemical media they allow the electrodeposition of elements that are impossible to reduce in aqueous media. We have investigated the electrodeposition of aluminium from 1-butyl-3-methyl-imidazolium chloride ((Bmim)Cl)/AlCl3 (40/60 mol %) as concerns the effect of deposition parameters on the quality of the deposits. Thick (20 μm) aluminium coatings were electrodeposited on brass substrates at different temperatures and mixing conditions (mechanical stirring and sonication). These coatings were investigated by means of scanning electron microscope, roughness measurements, and X-ray diffraction to assess the morphology and the phase composition. Finally, electrochemical corrosion tests were carried out with the intent to correlate the deposition parameters to the anti-corrosion properties. PMID:28773839

Tuning the thickness of electrochemically grafted layers in large area molecular junctions

NASA Astrophysics Data System (ADS)

Fluteau, T.; Bessis, C.; Barraud, C.; Della Rocca, M. L.; Martin, P.; Lacroix, J.-C.; Lafarge, P.

2014-09-01

We have investigated the thickness, the surface roughness, and the transport properties of oligo(1-(2-bisthienyl)benzene) (BTB) thin films grafted on evaporated Au electrodes, thanks to a diazonium-based electro-reduction process. The thickness of the organic film is tuned by varying the number of electrochemical cycles during the growth process. Atomic force microscopy measurements reveal the evolution of the thickness in the range of 2-27 nm. Its variation displays a linear dependence with the number of cycles followed by a saturation attributed to the insulating behavior of the organic films. Both ultrathin (2 nm) and thin (12 and 27 nm) large area BTB-based junctions have then been fabricated using standard CMOS processes and finally electrically characterized. The electronic responses are fully consistent with a tunneling barrier in case of ultrathin BTB film whereas a pronounced rectifying behavior is reported for thicker molecular films.

Exploring electrolyte preference of vanadium nitride supercapacitor electrodes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Bo; Chen, Zhaohui; Lu, Gang

Highlights: • Hierarchical VN nanostructures were prepared on graphite foam. • Electrolyte preference of VN supercapacitor electrodes was explored. • VN showed better capacitive property in organic and alkaline electrolytes than LiCl. - Abstract: Vanadium nitride hierarchical nanostructures were prepared through an ammonia annealing procedure utilizing vanadium pentoxide nanostructures grown on graphite foam. The electrochemical properties of hierarchical vanadium nitride was tested in aqueous and organic electrolytes. As a result, the vanadium nitride showed better capacitive energy storage property in organic and alkaline electrolytes. This work provides insight into the charge storage process of vanadium nitride and our findings canmore » shed light on other transition metal nitride-based electrochemical energy storage systems.« less

Preparation and evaluation of advanced electrocatalysts for phosphoric acid fuel cells

NASA Technical Reports Server (NTRS)

Stonehart, P.; Baris, J.; Hochmuth, J.; Pagliaro, P.

1981-01-01

A number of electrocatalyst combinations were prepared and characterized. These electrocatalysts were formulated to contain platinum combined with transition metal carbide forming elements (W, Mo, V) for cathodes and platinum combined with palladium for anodes. High resolution electron microscopy was used to determine the crystallite size and dispersion of platinum-palladium alloy electrocatalysts in order to provide analytical support for the electrochemical determinations of the particle dispersions. An equation was derived which correlates palladium crystallite size with electrochemical hydrogen adsorption. Based on comparisons of electrocatalyst performances in the presence of pure hydrogen and hydrogen containing carbon monoxide, it was shown that the apparent poisoning of the electrocatalyst by carbon monoxide is influenced by the electrode structure.

Crystal structure and electrochemical characteristics of non-AB 5 type La-Ni system alloys

NASA Astrophysics Data System (ADS)

Shi, Siqi; Ouyang, Chuying; Lei, Minsheng

The La-Ni system compounds have been prepared by arc-melting method under Ar atmosphere. X-ray diffraction analysis reveals that the as-prepared alloys consist of different phases. The electrochemical properties, including activation, maximum discharge capacity, high rate chargeability (HRC), and high rate dischargeability (HRD) of these alloy electrodes have been studied through the charge-discharge recycle testing at different temperatures and charge (or discharge) currents. Among the La-Ni alloy electrodes studied, LaNi 2.28 alloy has the most excellent high rate charging performance, and La 2Ni 7 alloy exhibit the highest high rate dischargeability, while La 7Ni 3 alloy is capable of discharging at low temperature.

Corrosion of Nickel-Titanium Orthodontic Archwires in Saliva and Oral Probiotic Supplements

PubMed Central

Turco, Gianluca; Contardo, Luca; Serdarević, Nikolina Leona; Otmačić, Helena; Ćurković; Špalj, Stjepan

2017-01-01

Objectives The aim of the study was to examine how probiotic supplements affect the corrosion stability of orthodontic archwires made of nickel-titanium alloy (NiTi). Materials and Methods NiTi archwires (0.508x0.508 and having the length of 2.5 cm) were tested. The archwires (composition Ni=50.4%, Ti=49.6%) were uncoated, nitrified and rhodium coated. Surface microgeometry was observed by using scanning electron microscope and surface roughness was measured by profilometer through these variables: roughness average, maximum height and maximum roughness depth. Corrosion was examined by electrochemical method of cyclic polarisation. Results Rhodium coated alloy in saliva has significantly higher general corrosion in saliva than nitrified alloy and uncoated alloy, with large effect size (p=0.027; η2=0.700). In the presence of probiotics, the result was even more pronounced (p<0.001; η2=0.936). Probiotic supplement increases general and localised corrosion of rhodium coated archwire and slightly decreases general corrosion and increases localised corrosion in uncoated archwire, while in the case of nitrified archwire the probability of corrosion is very low. The differences in surface roughness between NiTi wires before corrosion are not significant. Exposure to saliva decreases roughness average in rhodium coated wire (p=0.015; η2=0.501). Media do not significantly influence surface microgeometry in nitrified and uncoated wires. Conclusion Probiotic supplement affects corrosion depending on the type of coating of the NiTi archwire. It increases general corrosion of rhodium coated wire and causes localised corrosion of uncoated and rhodium coated archwire. Probiotic supplement does not have greater influence on surface roughness compared to that of saliva. PMID:29872237

Dynamic evolution of interface roughness during friction and wear processes.

PubMed

Kubiak, K J; Bigerelle, M; Mathia, T G; Dubois, A; Dubar, L

2014-01-01

Dynamic evolution of surface roughness and influence of initial roughness (S(a) = 0.282-6.73 µm) during friction and wear processes has been analyzed experimentally. The mirror polished and rough surfaces (28 samples in total) have been prepared by surface polishing on Ti-6Al-4V and AISI 1045 samples. Friction and wear have been tested in classical sphere/plane configuration using linear reciprocating tribometer with very small displacement from 130 to 200 µm. After an initial period of rapid degradation, dynamic evolution of surface roughness converges to certain level specific to a given tribosystem. However, roughness at such dynamic interface is still increasing and analysis of initial roughness influence revealed that to certain extent, a rheology effect of interface can be observed and dynamic evolution of roughness will depend on initial condition and history of interface roughness evolution. Multiscale analysis shows that morphology created in wear process is composed from nano, micro, and macro scale roughness. Therefore, mechanical parts working under very severe contact conditions, like rotor/blade contact, screws, clutch, etc. with poor initial surface finishing are susceptible to have much shorter lifetime than a quality finished parts. © Wiley Periodicals, Inc.

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

NASA Astrophysics Data System (ADS)

Gobal, Fereydoon; Faraji, Masoud

2014-12-01

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

Electrochemical and microstructural characterization of magnetron-sputtered ATO thin films as Li–ion storage materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ouyang, Pan; Zhang, Hong; Chen, Wenhao

2015-01-15

Highlights: • Nano-structured ATO thin films prepared by RF magnetron sputtering at 25 °C, 100 °C and 200 °C, respectively. • ATO thin films show a high reversible capacity and high rate performance. • Electrochemical reaction mechanism of the ATO thin film was revealed by transmission electron microscopy. - Abstract: Sb-doped SnO{sub 2} (ATO) nanostructured thin films were prepared by using radio frequency magnetron sputtering at the substrate temperatures of 25 °C, 100 °C and 200 °C, respectively. All the ATO thin films have the similar redox characteristics in the cyclic voltammetry measurements. The ATO thin film sputtered at 200more » °C shows the lowest charge transfer resistance and best electrochemical performance, and has a high reversible capacity of 679 mA h g{sup −1} at 100 mA g{sup −1} after 200 charge–discharge cycles and high rate performance of 483 mA h g{sup −1} at 800 mA g{sup −1}. The electrochemical mechanisms were investigated by analyzing the phase evolution of the ATO electrodes that had been electrochemically induced at various stages. The results reveal that the ATO underwent reversible lithiation/delithiation processes during the electrochemical cycles, i.e., the SnO{sub 2} reacted with Li{sup +} to produce metallic Sn and followed by the formation of the Li{sub x}Sn alloys during discharge process, and then Li{sub x}Sn alloys de-alloyed, Sn reacted with Li{sub 2}O, and even partially formed SnO{sub 2} during charge process.« less

Effect of sandblasting on surface roughness of zirconia-based ceramics and shear bond strength of veneering porcelain.

PubMed

He, Min; Zhang, Zutai; Zheng, Dongxiang; Ding, Ning; Liu, Yan

2014-01-01

This study aims to investigate the effect of sandblasting on the surface roughness of zirconia and the shear bond strength of the veneering porcelain. Pre-sintered zirconia plates were prepared and divided into four groups. Group A were not treated at all; group B were first sandblasted under 0.2 MPa pressure and then densely sintered; group C and D were sintered first, and then sandblasted under 0.2 MPa and 0.4 MPa pressures respectively. Surface roughness was measured and 3D roughness was reconstructed for the specimens, which were also analyzed with X-ray diffractometry. Finally after veneering porcelain sintering, shear bond tests were conducted. Sandblasting zirconia before sintering significantly increased surface roughness and the shear bond strength between zirconia and veneering porcelain (p<0.05). Sandblasting zirconia before sintering is a useful method to increase surface roughness and could successfully improve the bonding strength of veneering porcelain.

Nanometric MgFe2O4: Synthesis, characterization and its application towards supercapacitor and electrochemical uric acid sensor

NASA Astrophysics Data System (ADS)

Majumder, S.; Kumar, S.; Banerjee, S.

2017-05-01

In this paper, we have synthesized nanocrystalline MgFe2O4 (S1) by auto-combustion assisted sol-gel method. The structure and morphology and elemental study of S1 are examined by powder X-ray diffraction (PXRD), field emission scanning electron microscopic (FESEM) and energy dispersive X-ray spectroscopic (EDS) techniques. The FESEM images reveal that the morphology of the sample is rough and average particle size is 50 nm. The PXRD study indicates that the samples are well crystalline and single phase in nature. Moreover, we have performed supercapacitor study by electrochemical galvanostatic charge-discharge (GCD) measurement, which shows pseudo capacitive behavior. S1 contains a high specific capacitance of 428.9 Fg-1 at the current density 0.0625 Ag-1 and can deliver high energy and power density of 18.01 Wh kg-1 and 21468 Wkg-1 respectively. Moreover, uric acid (UA) sensing study has also been performed by cyclic voltmetry (CV) and electrochemical impedance spectroscopy measurement (EIS) of S1. We can use nanocrystalline MgFe2O4 as supercapacitor and UA sensor applications purpose.

Effect of polyvinyl alcohol on electrochemically deposited ZnO thin films for DSSC applications

NASA Astrophysics Data System (ADS)

Marimuthu, T.; Anandhan, N.

2017-05-01

Nanostructures of zinc oxide (ZnO) thin film are electrochemically deposited in the absence and presence of polyvinyl alcohol (PVA) on fluorine doped tin oxide (FTO) substrate. X-ray diffraction (XRD) patterns and Raman spectroscopy confirmed the formation of hexagonal structure of ZnO. The film prepared in the presence of PVA showed a better crystallinity and its crystalline growth along the (002) plane orientation. Field emission scanning electron microscope (FE-SEM) images display nanowire arrays (NWAs) and sponge like morphology for films prepared in the absence and presence of PVA, respectively. Photoluminescence (PL) spectra depict the film prepared in the presence PVA having less atomic defects with good crystal quality compared with other film. Dye sensitized solar cell (DSSC) is constructed using low cost eosin yellow dye and current-voltage (J-V) curve is recorded for optimized sponge like morphology based solar cell.

Carbon-Nanotube-Based Electrochemical Double-Layer Capacitor Technologies for Spaceflight Applications

NASA Technical Reports Server (NTRS)

Arepalli, S.; Fireman, H.; Huffman, C.; Maloney, P.; Nikolaev, P.; Yowell, L.; Kim, K.; Kohl, P. A.; Higgins, C. D.; Turano, S. P.

2005-01-01

Electrochemical double-layer capacitors, or supercapacitors, have tremendous potential as high-power energy sources for use in low-weight hybrid systems for space exploration. Electrodes based on single-wall carbon nanotubes (SWCNTs) offer exceptional power and energy performance due to the high surface area, high conductivity, and the ability to functionalize the SWCNTs to optimize capacitor properties. This paper will report on the preparation of electrochemical capacitors incorporating SWCNT electrodes and their performance compared with existing commercial technology. Preliminary results indicate that substantial increases in power and energy density are possible. The effects of nanotube growth and processing methods on electrochemical capacitor performance is also presented. The compatibility of different SWCNTs and electrolytes was studied by varying the type of electrolyte ions that accumulate on the high-surface-area electrodes.

Effect of engraving speeds of CO₂ laser irradiation on In-Ceram Alumina roughness: a pilot study.

PubMed

Ersu, Bahadır; Ersoy, Orkun; Yuzugullu, Bulem; Canay, Senay

2015-05-01

The aim of the study was to determine the effect of CO₂ laser on surface roughness of In-Ceram-Alumina-ceramic. Four aluminum-oxide ceramic disc specimens were prepared of In-Ceram Alumina. Discs received CO₂ laser irradiation with different engraving speeds (100, 400, 600 and 800 mm/min) as a surface treatment. The roughness of the surfaces was measured on digital elevation models reconstructed from stereoscopic images acquired by scanning-electron-microscope. Surface roughness data were analyzed with One-Way-Analysis-of-Variance at a significance level of p<0.05. There was no significant difference between the roughness values (p=0.82). Due to higher laser durations, partial melting signs were observed on the surfaces. Tearing, smearing and swelling occurred on melted surfaces. Swelling accompanying melting increased the surface roughness, while laser power was fixed and different laser engraving speeds were applied. Although different laser irradiation speeds did not affect the roughness of ceramic surfaces, swelling was observed which led to changes on surfaces.

Preparation and characterization of hierarchical porous carbons derived from solid leather waste for supercapacitor applications.

PubMed

Konikkara, Niketha; Kennedy, L John; Vijaya, J Judith

2016-11-15

Utilization of crust leather waste (CLW) as precursors for the preparation of hierarchical porous carbons (HPC) were investigated. HPCs were prepared from CLW by pre-carbonization followed by chemical activation using KOH at relatively high temperatures. Textural properties of HPC's showed an extent of micro-and mesoporosity with maximum BET surface area of 716m(2)/g. Inducements of graphitic planes in leather waste derived carbons were observed from X-ray diffraction and HR-TEM analysis. Microstructure, thermal behavior and surface functional groups were identified using FT-Raman, thermo gravimetric analysis and FT-IR techniques. HPCs were evaluated for electrochemical properties by cyclic voltammetry (CV), galvanostatic charge/discharge (GCD) and electrochemical impedance spectroscopy (EIS) by three electrode system. CLC9 sample showed a maximum capacitance of 1960F/g in 1M KCl electrolyte. Results achieved from rectangular curves of CV, GCD symmetric curves and Nyquist plots show that the leather waste carbon is suitable to fabricate supercapacitors as it possess high specific capacitance and electrochemical cycle stability. The present study proposes an effective method for solid waste management in leather industry by the way of converting toxic leather waste to new graphitic porous carbonaceous materials as a potential candidate for energy storage devices. Copyright © 2016 Elsevier B.V. All rights reserved.

Electrochemical properties of Sn-based nanopowders synthesized by a pulsed wire evaporation method and effect of binder coating

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ha, Jong-Keun; Song, Ju-Seok; Cho, Gyu-Bong

Highlights: • Sn-based nanoparticles are fabricated by using the pulsed wire evaporation method. • The electrodes are prepared by mixing the graphene and coating the surface. • Coating the surface of electrode is used with brushing of simple and facile method. • The electrochemical measurements are performed with galvanostatic experiments. • The coating electrode maintains capacity nearly of 501 mAh g{sup −1} up to 100 cycles. - Abstract: Sn-based nanoparticles are prepared with the O{sub 2} concentrations in chamber of Ar atmosphere (by v/v) by using the pulsed wire evaporation (PWE) method. The prepared electrodes are only Sn-based powder electrode,more » its binder coating electrode and Sn-based powder/graphene nanocomposite electrode. Morphology and structure of the synthesized powders and electrodes are investigated with a field emission scanning electron microscope (FE-SEM) and an X-ray diffraction (XRD) analysis. The electrochemical measurements were performed with galvanostatic cycling experiments using a coin type cell of CR2032 (Ø20, T3.2 mm). The binder coating electrode is superior to others and maintains delithiation capacity nearly of 501 mAh g{sup −1} as 58.3% of first delithiation capacity at 0.2 C-rate up to 100 cycles.« less

Enhancing Electrochemical Performance of Graphene Fiber-Based Supercapacitors by Plasma Treatment.

PubMed

Meng, Jie; Nie, Wenqi; Zhang, Kun; Xu, Fujun; Ding, Xin; Wang, Shiren; Qiu, Yiping

2018-04-25

Graphene fiber-based supercapacitors (GFSCs) hold high power density, fast charge-discharge rate, ultralong cycling life, exceptional mechanical/electrical properties, and safe operation conditions, making them very promising to power small wearable electronics. However, the electrochemical performance is still limited by the severe stacking of graphene sheets, hydrophobicity of graphene fibers, and complex preparation process. In this work, we develop a facile but robust strategy to easily enhance electrochemical properties of all-solid-state GFSCs by simple plasma treatment. We find that 1 min plasma treatment under an ambient condition results in 33.1% enhancement of areal specific capacitance (36.25 mF/cm 2 ) in comparison to the as-prepared GFSC. The energy density reaches 0.80 μW h/cm 2 in polyvinyl alcohol/H 2 SO 4 gel electrolyte and 18.12 μW h/cm 2 in poly(vinylidene difluoride)/ethyl-3-methylimidazolium tetrafluoroborate electrolyte, which are 22 times of that of as-prepared ones. The plasma-treated GFSCs also exhibit ultrahigh rate capability (69.13% for 40 s plasma-treated ones) and superior cycle stability (96.14% capacitance retention after 20 000 cycles for 1 min plasma-treated ones). This plasma strategy can be extended to mass-manufacture high-performance carbonaceous fiber-based supercapacitors, such as graphene and carbon nanotube-based ones.

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

NASA Astrophysics Data System (ADS)

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

2014-10-01

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

Reduced graphene oxide hydrogels deposited in nickel foam for supercapacitor applications: Toward high volumetric capacitance

DOE PAGES

Pham, Viet Hung; Dickerson, James H.

2016-02-21

Graphene hydrogels have been considered as ideal materials for high-performance supercapacitors. However, their low volumetric capacitance significantly limits its real application. In this study, we report an environment-friendly and scalable method to prepare high packing density, electrochemically reduced graphene oxide hydrogels (ERGO) for supercapacitor application by the electrophoretic deposition of graphene oxide onto nickel foam, followed by the electrochemical reduction and hydraulic compression of the deposited materials. The as-prepared ERGO on nickel foam was hydraulic compressed up to 20 tons, resulting in an increase of the packing density of ERGO from 0.0098 to 1.32 g cm –3. Consequently, the volumetricmore » capacitance and volumetric energy density of ERGOs greatly increased from 1.58 F cm –3 and 0.053 Wh cm –3 (as-prepared ERGO) to 176.5 F cm –3 and 6.02 Wh cm –3 (ERGO compressed at 20 tons), respectively. The ERGOs also exhibited long-term electrochemical stability with a capacitance retention in the range of approximately 79–90% after 10 000 cycles. Lastly, we believe that these high packing density ERGOs are promising for real-world energy storage devices for which scalable, cost-effective manufacturing is of significance and for which space constraints are paramount.« less

Symmetric Supercapacitor Electrodes from KOH Activation of Pristine, Carbonized, and Hydrothermally Treated Melia azedarach Stones.

PubMed

Moreno-Castilla, Carlos; García-Rosero, Helena; Carrasco-Marín, Francisco

2017-07-04

Waste biomass-derived activated carbons (ACs) are promising materials for supercapacitor electrodes due to their abundance and low cost. In this study, we investigated the potential use of Melia azedarach (MA) stones to prepare ACs for supercapacitors. The ash content was considerably lower in MA stones (0.7% ash) than that found in other lignocellulosic wastes. ACs were prepared by KOH activation of pristine, carbonized, and hydrothermally-treated MA stones. The morphology, composition, surface area, porosity, and surface chemistry of the ACs were determined. Electrochemical measurements were carried out in three- and two-electrode cells, 3EC and 2EC, respectively, using 1 M H₂SO₄ as the electrolyte. The highest capacitance from galvanostatic charge-discharge (GCD) in 2EC ranged between 232 and 240 F·g -1 at 1 A·g -1 . The maximum energy density reached was 27.4 Wh·kg -1 at a power density of 110 W·kg -1 . Electrochemical impedance spectroscopy (EIS) revealed an increase in equivalent series resistance (ESR) and charge transfer resistance (R CT ) with greater ash content. Electrochemical performance of MA stone-derived ACs was compared with that of other ACs described in the recent literature that were prepared from different biomass wastes and results showed that they are among the best ACs for supercapacitor applications.

Reduced graphene oxide hydrogels deposited in nickel foam for supercapacitor applications: Toward high volumetric capacitance

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pham, Viet Hung; Dickerson, James H.

Graphene hydrogels have been considered as ideal materials for high-performance supercapacitors. However, their low volumetric capacitance significantly limits its real application. In this study, we report an environment-friendly and scalable method to prepare high packing density, electrochemically reduced graphene oxide hydrogels (ERGO) for supercapacitor application by the electrophoretic deposition of graphene oxide onto nickel foam, followed by the electrochemical reduction and hydraulic compression of the deposited materials. The as-prepared ERGO on nickel foam was hydraulic compressed up to 20 tons, resulting in an increase of the packing density of ERGO from 0.0098 to 1.32 g cm –3. Consequently, the volumetricmore » capacitance and volumetric energy density of ERGOs greatly increased from 1.58 F cm –3 and 0.053 Wh cm –3 (as-prepared ERGO) to 176.5 F cm –3 and 6.02 Wh cm –3 (ERGO compressed at 20 tons), respectively. The ERGOs also exhibited long-term electrochemical stability with a capacitance retention in the range of approximately 79–90% after 10 000 cycles. Lastly, we believe that these high packing density ERGOs are promising for real-world energy storage devices for which scalable, cost-effective manufacturing is of significance and for which space constraints are paramount.« less

Ionic liquid-assisted solvothermal synthesis of hollow Mn2O3 anode and LiMn2O4 cathode materials for Li-ion batteries

NASA Astrophysics Data System (ADS)

He, Xin; Wang, Jun; Jia, Haiping; Kloepsch, Richard; Liu, Haidong; Beltrop, Kolja; Li, Jie

2015-10-01

Mn-based Mn2O3 anode and LiMn2O4 cathode materials are prepared by a solvothermal method combined with post annealing process. Environmentally friendly ionic liquid 1-Butyl-3-methylimidazolium tetrafluoroborate as both structure-directing agent and fluorine source is used to prepare hollow polyhedron MnF2 precursor. Both target materials Mn2O3 anode and LiMn2O4 cathode have the morphology of the MnF2 precursor. The Mn2O3 anode using carboxymethyl cellulose as binder could deliver slight better electrochemical performance than the one using poly (vinyldifluoride) as binder. The former has an initial charge capacity of 800 mAh g-1 at a current density of 101.8 mA g-1, and exhibits no obvious capacity decay for 150 cycles at 101.8 mA g-1. The LiMn2O4 cathode material prepared with molten salt assistant could display much better electrochemical performance than the one prepared without molten salt assistance. In particular, it has an initial discharge capacity of 117.5 mAh g-1 at a current density of 0.5C and good rate capability. In the field of lithium ion batteries, both the Mn2O3 anode and LiMn2O4 cathode materials could exhibit enhanced electrochemical performance due to the well formed morphology based on the ionic liquid-assisted solvothermal method.

Electrochemically exfoliated graphene as a novel microwave susceptor: the ultrafast microwave-assisted synthesis of carbon-coated silicon-graphene film as a lithium-ion battery anode.

PubMed

Kim, Jong Min; Ko, Dongjin; Oh, Jiseop; Lee, Jeongyeon; Hwang, Taejin; Jeon, Youngmoo; Hooch Antink, Wytse; Piao, Yuanzhe

2017-10-19

Graphene nanocomposites have attracted much attention in many applications due to their superior properties. However, preparing graphene nanocomposites requires a time-consuming thermal treatment to reduce the graphene or synthesize nanomaterials, in most cases. We present an ultrafast synthesis of a carbon-coated silicon-graphene nanocomposite using a commercial microwave system. Electrochemically exfoliated graphene is used as a novel microwave susceptor to deliver efficient microwave energy conversion. Unlike graphene oxide, it does not require a time-consuming pre-thermal reduction or toxic chemical reduction to absorb microwave radiation efficiently. A carbon-coated silicon nanoparticle-electrochemically exfoliated graphene nanocomposite film was prepared by a few seconds' microwave irradiation. The sp 2 domains of graphene absorb microwave radiation and generate heat to simultaneously reduce the graphene and carbonize the polydopamine carbon precursor. The as-prepared N-doped carbon-coated silicon-graphene film was used as a lithium-ion battery anode. The N-doped carbon coating decreases the contact resistance between silicon nanoparticles and graphene provides a wide range conductive network. Consequently, it exhibited a reversible capacity of 1744 mA h g -1 at a current density of 0.1 A g -1 and 662 mA h g -1 at 1.0 A g -1 after 200 cycles. This method can potentially be a general approach to prepare various graphene nanocomposites in an extremely short time.

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.

PubMed

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.

By-products of electrochemical synthesis of suberic acid

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shirobokova, O.I.; Adamov, A.A.; Freidlin, G.N.

By-products of the electrochemical synthesis of dimethyl suberate from glutaric anhydride were studied. This is isolated by thermal dehydration of a mixture of lower dicarboxylic acids that are wastes from the production of adipic acid. To isolate the by-products, they used the methods of vacuum rectification and preparative gas-liquid chromatography, and for their identification, PMR, IR spectroscopy, gas-liquid chromatography, and other known physicochemical methods of investigation.

Rough Gold Electrodes for Decreasing Impedance at the Electrolyte/Electrode Interface

PubMed Central

Koklu, Anil; Sabuncu, Ahmet C.; Beskok, Ali

2016-01-01

Electrode polarization at the electrolyte/electrode interface is often undesirable for bio-sensing applications, where charge accumulated over an electrode at constant potential causes large potential drop at the interface and low measurement sensitivity. In this study, novel rough electrodes were developed for decreasing electrical impedance at the interface. The electrodes were fabricated using electrochemical deposition of gold and sintering of gold nanoparticles. The performances of the gold electrodes were compared with platinum black electrodes. A constant phase element model was used to describe the interfacial impedance. Hundred folds of decrease in interfacial impedance were observed for fractal gold electrodes and platinum black. Biotoxicity, contact angle, and surface morphology of the electrodes were investigated. Relatively low toxicity and hydrophilic nature of the fractal and granulated gold electrodes make them suitable for bioimpedance and cell electromanipulation studies compared to platinum black electrodes which are both hydrophobic and toxic. PMID:27695132

Electron-beam patterned self-assembled monolayers as templates for Cu electrodeposition and lift-off.

PubMed

She, Zhe; Difalco, Andrea; Hähner, Georg; Buck, Manfred

2012-01-01

Self-assembled monolayers (SAMs) of 4'-methylbiphenyl-4-thiol (MBP0) adsorbed on polycrystalline gold substrates served as templates to control electrochemical deposition of Cu structures from acidic solution, and enabled the subsequent lift-off of the metal structures by attachment to epoxy glue. By exploiting the negative-resist behaviour of MBP0, the SAM was patterned by means of electron-beam lithography. For high deposition contrast a two-step procedure was employed involving a nucleation phase around -0.7 V versus Cu(2+)/Cu and a growth phase at around -0.35 V versus Cu(2+)/Cu. Structures with features down to 100 nm were deposited and transferred with high fidelity. By using substrates with different surface morphologies, AFM measurements revealed that the roughness of the substrate is a crucial factor but not the only one determining the roughness of the copper surface that is exposed after lift-off.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rahmani, N.; Dariani, R. S., E-mail: dariani@alzahra.ac.ir

Porous silicon films with porosity ranging from 42% to 77% were fabricated by electrochemical anodization under different current density. We used atomic force microscopy and dynamic scaling theory for deriving the surface roughness profile and processing the topography of the porous silicon layers, respectively. We first compared the topography of bare silicon surface with porous silicon and then studied the effect of the porosity of porous silicon films on their scaling behavior by using their self-affinity nature. Our work demonstrated that silicon compared to the porous silicon films has the highest Hurst parameter, indicating that the formation of porous layermore » due to the anodization etching of silicon surface leads to an increase of its roughness. Fractal analysis revealed that the evolution of the nanocrystallites’ fractal dimension along with porosity. Also, we found that both interface width and Hurst parameter are affected by the increase of porosity.« less

Natural sisal fibers derived hierarchical porous activated carbon as capacitive material in lithium ion capacitor

NASA Astrophysics Data System (ADS)

Yang, Zhewei; Guo, Huajun; Li, Xinhai; Wang, Zhixing; Yan, Zhiliang; Wang, Yansen

2016-10-01

Lithium-ion capacitor (LIC) is a novel advanced electrochemical energy storage (EES) system bridging gap between lithium ion battery (LIB) and electrochemical capacitor (ECC). In this work, we report that sisal fiber activated carbon (SFAC) was synthesized by hydrothermal treatment followed by KOH activation and served as capacitive material in LIC for the first time. Different particle structure, morphology, specific surface area and heteroatoms affected the electrochemical performance of as-prepared materials and corresponding LICs. When the mass ratio of KOH to char precursor was 2, hierarchical porous structured SFAC-2 was prepared and exhibited moderate specific capacitance (103 F g-1 at 0.1 A g-1), superior rate capability and cyclic stability (88% capacity retention after 5000 cycles at 1 A g-1). The corresponding assembled LIC (LIC-SC2) with optimal comprehensive electrochemical performance, displayed the energy density of 83 Wh kg-1, the power density of 5718 W kg-1 and superior cyclic stability (92% energy density retention after 1000 cycles at 0.5 A g-1). It is worthwhile that the source for activated carbon is a natural and renewable one and the synthesis method is eco-friendly, which facilitate that hierarchical porous activated carbon has potential applications in the field of LIC and other energy storage systems.

Preparation of Carbon-Chitosan-Polyvinyl Chloride (CC-PVC) Material and its Application to Electrochemical Degradation of Methylene Blue in Sodium Chloride Solution

NASA Astrophysics Data System (ADS)

Riyanto; Prawidha, A. D.

2018-01-01

Electrochemical degradation of methylene blue using Carbon-Chitosan-Polyvinyl Chloride (CC-PVC) electrode in sodium chloride have been done. The aim of this work was to degradation of methylene blue using Carbon-Chitosan-Polyvinyl Chloride (CC-PVC). Carbon chitosan composite electrode was preparing by Carbon and Chitosan powder and PVC in 4 mL tetrahydrofuran (THF) solvent and swirled flatly to homogeneous followed by drying in an oven at 100 °C for 3 h. The mixture was placed in stainless steel mould and pressed at 10 ton/cm2. Sodium chloride was used electrolyte solution. The effects of the current and electrolysis time were investigated using spectrophotometer UV-Visible. The experimental results showed that the carbon-chitosan composite electrode have higher effect in the electrochemical degradation of methylene blue in sodium chloride. Based on UV-visible spectra analysis shows current and electrolysis time has high effect to degradation of methylene blue in sodium chloride. Chitosan and polyvinyl chloride can strengthen the bond between the carbons so that the material has the high stability and conductivity. As conclusions is Carbon-Chitosan-Polyvinyl Chloride (CC-PVC) electrode have a high electrochemical activity for degradation of methylene blue in sodium chloride.

Immobilization and direct electrochemistry of glucose oxidase on a tetragonal pyramid-shaped porous ZnO nanostructure for a glucose biosensor.

PubMed

Dai, Zhihui; Shao, Guojian; Hong, Jianmin; Bao, Jianchun; Shen, Jian

2009-01-01

A tetragonal pyramid-shaped porous ZnO (TPSP-ZnO) nanostructure is used for the immobilization, direct electrochemistry and biosensing of proteins. The prepared ZnO has a large surface area and good biocompatibility. Using glucose oxidase (GOD) as a model, this shaped ZnO is tested for immobilization of proteins and the construction of electrochemical biosensors with good electrochemical performances. The interaction between GOD and TPSP-ZnO is examined by using AFM, N(2) adsorption isotherms and electrochemical methods. The immobilized GOD at a TPSP-ZnO-modified glassy carbon electrode shows a good direct electrochemical behavior, which depends on the properties of the TPSP-ZnO. Based on a decrease of the electrocatalytic response of the reduced form of GOD to dissolved oxygen, the proposed biosensor exhibits a linear response to glucose concentrations ranging from 0.05 to 8.2mM with a detection limit of 0.01mM at an applied potential of -0.50V which has better biosensing properties than those from other morphological ZnO nanoparticles. The biosensor shows good stability, reproducibility, low interferences and can diagnose diabetes very fast and sensitively. Such the TPSP-ZnO nanostructure provides a good matrix for protein immobilization and biosensor preparation.

One-step synthesis of large-scale graphene film doped with gold nanoparticles at liquid-air interface for electrochemistry and Raman detection applications.

PubMed

Zhang, Panpan; Huang, Ying; Lu, Xin; Zhang, Siyu; Li, Jingfeng; Wei, Gang; Su, Zhiqiang

2014-07-29

We demonstrated a facile one-step synthesis strategy for the preparation of a large-scale reduced graphene oxide multilayered film doped with gold nanoparticles (RGO/AuNP film) and applied this film as functional nanomaterials for electrochemistry and Raman detection applications. The related applications of the fabricated RGO/AuNP film in electrochemical nonenzymatic H2O2 biosensor, electrochemical oxygen reduction reaction (ORR), and surface-enhanced Raman scattering (SERS) detection were investigated. Electrochemical data indicate that the H2O2 biosensor fabricated by RGO/AuNP film shows a wide linear range, low limitation of detection, high selectivity, and long-term stability. In addition, it was proved that the created RGO/AuNP film also exhibits excellent ORR electrochemical catalysis performance. The created RGO/AuNP film, when serving as SERS biodetection platform, presents outstanding performances in detecting 4-aminothiophenol with an enhancement factor of approximately 5.6 × 10(5) as well as 2-thiouracil sensing with a low concentration to 1 μM. It is expected that this facile strategy for fabricating large-scale graphene film doped with metallic nanoparticles will spark inspirations in preparing functional nanomaterials and further extend their applications in drug delivery, wastewater purification, and bioenergy.

Electrochemical Formation of Mg-Li-Sm Alloys by Codeposition from LiCl-KCl-MgCl2-SmCl3 Molten Salts

NASA Astrophysics Data System (ADS)

Han, Wei; Wang, Fengli; Tian, Yang; Zhang, Milin; Yan, Yongde

2011-12-01

In this article, the electrochemical method of preparing Mg-Li-Sm alloys by codeposition in LiCl-KCl-MgCl2-SmCl3 melts was investigated. Transient electrochemical techniques, such as cyclic voltammetry, chronopotentiometry, and chronoamperometry were used to explore the electrochemical formation of Mg-Li-Sm alloys. Chronopotentiograms demonstrated that the codepositon of Mg, Li, and Sm occurred when current densities were more negative than -0.31 A cm-2. Chronoamperograms indicated that the onset potential for the codeposition of Mg, Li, and Sm was -2.40 V, and the codeposition of Mg, Li, and Sm was formed when the applied potentials were more negative than -2.40 V. The different phases of Mg-Li-Sm alloys were prepared by galvanostatic electrolysis and characterized by X-ray diffraction (XRD), optical microscope (OM), and scanning electron microscopy (SEM). An inductively coupled plasma (ICP) analysis showed that the lithium and samarium contents in Mg-Li-Sm alloys could be controlled by the concentrations of MgCl2 and SmCl3. The results demonstrated that Sm could refine the grains dramatically. When the Sm content was 0.8 wt pct, the grain size was the finest.

An Inexpensive Device for Studying Electrochromism

ERIC Educational Resources Information Center

Ibanez, Jorge G.; Puente-Caballero, Rodrigo; Torres-Perez, Jonatan; Bustos, Daniel; Carmona-Orbezo, Aranzazu; Sevilla, Fortunato B., III

2012-01-01

A novel procedure for the preparation of electrochromic WO[subscript 3] films from readily available materials is presented. It is based on the electrochemical preparation of potassium tungstate from tungsten filaments of incandescent light bulbs in a potassium hydroxide solution. Tungstic acid is then produced by proton exchange using a…

Preparation of Semiconducting Materials in the Laboratory, Part 3: The One-Penny Photovoltaic Cell

ERIC Educational Resources Information Center

Ibanez, Jorge G.; Finck-Pastrana, Adolfo; Mugica-Barrera, Alejandra; Balderas-Hernandez, Patricia; Ibarguengoitia-Cervantes, Martha E.; Garcia-Pintor, Elizabeth; Hartasanchez-Frenk, Jose Miguel; Bonilla-Jaurez, Cesar E.; Maldonado-Cordero, Casandra; Struck-Garza, Adelwart; Suberbie-Rocha, Felipe

2011-01-01

Copper(I) oxide photoresponsive layers are prepared on copper surfaces (e.g., U.S. pre-1982 pennies) by simple thermal, chemical, and electrochemical procedures. An easily measurable photovoltage (up to 100 mV) is obtained in each case under visible light illumination. (Contains 2 figures.)

Chitosan-58S bioactive glass nanocomposite coatings on TiO2 nanotube: Structural and biological properties

NASA Astrophysics Data System (ADS)

Mokhtari, H.; Ghasemi, Z.; Kharaziha, M.; Karimzadeh, F.; Alihosseini, F.

2018-05-01

Bacterial infection and insignificant osseointegration have been recognized as the main reasons of the failures of titanium based implants. The aim of this study was to apply titanium oxide nanotube (TNT) array on titanium using electrochemical anodization process as a more appropriate substrate for chitosan and chitosan-58S bioactive glass (BG) (58S-BG-Chitosan) nanocomposite coatings covered TNTs (TNT/Chiosan, TNT/58S-BG-Chitosan, respectively) through a conventional dip-coating process. Results showed that a TNT layer with average inner diameter of 82 ± 19 nm and wall's thickness of 23 ± 9 nm was developed on titanium surface using electrochemical anodization process. Roughness and contact angle measurement showed that TNT with Ra = 449 nm had highest roughness and hydrophilicity which then reduced to 86 nm and 143 nm for TNT/Chitosan and TNT/58S-BG-Chitosan, respectively. In vitro bioactivity evaluation in simulated buffer fluid (SBF) solution and antibacterial activity assay predicted that TNT/58S-BG-Chitosan was superior in bone like apatite formation and antibacterial activity against both gram-positive and gram-negative bacteria compared to Ti, TNT and TNT/Chitosan samples, respectively. Results revealed the noticeable MG63 cell attachment and proliferation on TNT/58S-BG-Chitosan coating compared to those of uncoated TNTs. These results confirmed the positive effect of using TNT substrate for natural polymer coating on improved bioactivity of implant.

3D surface topography study of the biofunctionalized nanocrystalline Ti-6Zr-4Nb/Ca-P

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jakubowicz, J., E-mail: jaroslaw.jakubowicz@put.poznan.pl; Adamek, G.; Jurczyk, M.U.

2012-08-15

In this work surface of the sintered Ti-6Zr-4Nb nanocrystalline alloy was electrochemically biofunctionalized. The porous surface was produced by anodic oxidation in 1 M H{sub 3}PO{sub 4} + 2%HF electrolyte at 10 V for 30 min. Next the calcium-phosphate (Ca-P) layer was deposited, onto the formed porous surface, using cathodic potential - 5 V kept for 60 min in 0.042 M Ca(NO{sub 3}){sub 2} + 0.025 M (NH{sub 4}){sub 2}HPO{sub 4} + 0.1 M HCl electrolyte. The deposited Ca-P layer anchored in the pores. The biofunctionalized surface was studied by XRD, SEM and EDS. In vitro tests culture of normalmore » human osteoblast (NHOst) cells showed very good cells proliferation, colonization and multilayering. Using optical profiler, roughness and hybrid 3D surface topography parameters were estimated. Correlation between surface composition, morphology, roughness and biocompatibility results was done. It has been shown by us that surface with appropriate chemical composition and topography, after combined electrochemical anodic and cathodic surface treatment, supports osteoblast adhesion and proliferation. 3D topography measurements using optical profiler play a key role in the biomaterials surface analysis. - Highlights: Black-Right-Pointing-Pointer Nanocrystalline Ti-6Zr-4Nb/Ca-P material was produced for hard tissue implant applications. Black-Right-Pointing-Pointer Calcium-phosphate results in surface biofunctionalization. Black-Right-Pointing-Pointer The biofunctionalized surface shows good in-vitro behavior.« less

Vanadium based materials as electrode materials for high performance supercapacitors

NASA Astrophysics Data System (ADS)

Yan, Yan; Li, Bing; Guo, Wei; Pang, Huan; Xue, Huaiguo

2016-10-01

As a kind of supercapacitors, pseudocapacitors have attracted wide attention in recent years. The capacitance of the electrochemical capacitors based on pseudocapacitance arises mainly from redox reactions between electrolytes and active materials. These materials usually have several oxidation states for oxidation and reduction. Many research teams have focused on the development of an alternative material for electrochemical capacitors. Many transition metal oxides have been shown to be suitable as electrode materials of electrochemical capacitors. Among them, vanadium based materials are being developed for this purpose. Vanadium based materials are known as one of the best active materials for high power/energy density electrochemical capacitors due to its outstanding specific capacitance and long cycle life, high conductivity and good electrochemical reversibility. There are different kinds of synthetic methods such as sol-gel hydrothermal/solvothermal method, template method, electrospinning method, atomic layer deposition, and electrodeposition method that have been successfully applied to prepare vanadium based electrode materials. In our review, we give an overall summary and evaluation of the recent progress in the research of vanadium based materials for electrochemical capacitors that include synthesis methods, the electrochemical performances of the electrode materials and the devices.

Surface and Electrochemical Properties of Polymer Brush-Based Redox Poly(Ionic Liquid).

PubMed

Bui-Thi-Tuyet, Van; Trippé-Allard, Gaëlle; Ghilane, Jalal; Randriamahazaka, Hyacinthe

2016-10-26

Redox-active poly(ionic liquid) poly(3-(2-methacryloyloxy ethyl)-1-(N-(ferrocenylmethyl) imidazolium bis(trifluoromethylsulfonyl)imide deposited onto electrode surfaces has been prepared using surface-initiated atom transfer radical polymerization SI-ATRP. The process starts by electrochemical immobilization of initiator layer, and then methacrylate monomer carrying ferrocene and imidazolium units is polymerized in ionic liquid media via SI-ATRP process. The surfaces analyses of the polymer exhibit a well-defined polymer brushlike structure and confirm the presence of ferrocene and ionic moieties within the film. Furthermore, the electrochemical investigations of poly(redox-active ionic liquid) in different media demonstrate that the electron transfer is not restricted by the rate of counterion migration into/out of the polymer. The attractive electrochemical performance of these materials is further demonstrated by performing electrochemical measurement, of poly(ferrocene ionic liquid), in solvent-free electrolyte. The facile synthesis of such highly ordered electroactive materials based ionic liquid could be useful for the fabrication of nanostructured electrode suitable for performing electrochemistry in solvent free electrolyte. We also demonstrate possible applications of the poly(FcIL) as electrochemically reversible surface wettability system and as electrochemical sensor for the catalytic activity toward the oxidation of tyrosine.

Polymer-directed synthesis of metal oxide-containing nanomaterials for electrochemical energy storage

NASA Astrophysics Data System (ADS)

Mai, Yiyong; Zhang, Fan; Feng, Xinliang

2013-12-01

Metal oxide-containing nanomaterials (MOCNMs) of controllable structures at the nano-scale have attracted considerable interest because of their great potential applications in electrochemical energy storage devices, such as lithium-ion batteries (LIBs) and supercapacitors. Among many structure-directing agents, polymers and macromolecules, including block copolymers (BCPs) and graphene, exhibit distinct advantages in the template-assisted synthesis of MOCNMs. In this feature article, we introduce the controlled preparation of MOCNMs employing BCPs and graphene as structure-directing agents. Typical synthetic strategies are presented for the control of structures and sizes as well as the improvement of physical properties and electrochemical performance of MOCNMs in LIBs and supercapacitors.

Polymer-directed synthesis of metal oxide-containing nanomaterials for electrochemical energy storage.

PubMed

Mai, Yiyong; Zhang, Fan; Feng, Xinliang

2014-01-07

Metal oxide-containing nanomaterials (MOCNMs) of controllable structures at the nano-scale have attracted considerable interest because of their great potential applications in electrochemical energy storage devices, such as lithium-ion batteries (LIBs) and supercapacitors. Among many structure-directing agents, polymers and macromolecules, including block copolymers (BCPs) and graphene, exhibit distinct advantages in the template-assisted synthesis of MOCNMs. In this feature article, we introduce the controlled preparation of MOCNMs employing BCPs and graphene as structure-directing agents. Typical synthetic strategies are presented for the control of structures and sizes as well as the improvement of physical properties and electrochemical performance of MOCNMs in LIBs and supercapacitors.

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

PubMed

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.

Non-Kinetic Losses Caused by Electrochemical Carbon Corrosion in PEM Fuel Cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Park, Seh Kyu; Shao, Yuyan; Viswanathan, Vilayanur V.

2012-05-01

This paper presented non-kinetic losses in PEM fuel cells under an accelerated stress test of catalyst support. The cathode with carbon-supported Pt catalyst was prepared and characterized with potential hold at 1.2 V vs. SHE in PEM fuel cells. Irreversible losses caused by carbon corrosion were evaluated using a variety of electrochemical characterizations including cyclic voltammetry, linear sweep voltammetry, electrochemical impedance spectroscopy, and polarization technique. Ohmic losses at the cathode with potential hold were determined using its capacitive responses. Concentration losses in PEM fuel cells were analyzed in terms of Tafel behavior and thin film/flooded-agglomerate dynamics.

Role of carbon nanotubes in electroanalytical chemistry: a review.

PubMed

Agüí, Lourdes; Yáñez-Sedeño, Paloma; Pingarrón, José M

2008-08-01

This review covers recent advances in the development of new designs of electrochemical sensors and biosensors that make use of electrode surfaces modification with carbon nanotubes. Applications based on carbon nanotubes-driven electrocatalytic effects, and the construction and analytical usefulness of new hybrid materials with polymers or other nanomaterials will be treated. Moreover, electrochemical detection using carbon nanotubes-modified electrodes as detecting systems in separation techniques such as high performance liquid chromatography (HPLC) or capillary electrophoresis (CE) will be also considered. Finally, the preparation of electrochemical biosensors, including enzyme electrodes, immunosensors and DNA biosensors, in which carbon nanotubes play a significant role in their sensing performance will be separately considered.

Graphite intercalation with fluoroanions by chemical and electrochemical methods

NASA Astrophysics Data System (ADS)

Ozmen-Monkul, Bahar

New acceptor-type graphite intercalation compounds (GICs) containing perfluoroalkyl anions have been synthesized by using both chemical and electrochemical methods and characterized by elemental and thermogravimetric analyses. Investigation into these graphite intercalation compounds can provide novel materials and a detailed understanding of their properties. GICs of composition Cx[FB(C2F 5)3]·deltaF are prepared for the first time by the intercalation of fluoro-tris(pentafluoroethyl)borate anion, [FB(C2F 5)3]-, under ambient conditions in aqueous (48%) hydrofluoric acid containing the oxidant K2[MnF6]. Powder-XRD data indicate that products are pure stage 2 and physical mixture of stage 2 and stage 3 after 1 h to 20 h reaction times. The calculated basal repeat distance, Ic, is 1.20 nm for stage 2 and 1.54-1.56 nm for stage 3 GICs, corresponding to gallery heights of di = 0.86-0.89 nm. In addition, stage 2 GIC of C x[FB(C2F5)3]·deltaCH 3NO2 having di = 0.84 nm is prepared by electrochemical oxidation of graphite in a nitromethane electrolyte. The elemental analyses of these complex GICs required that a new sample digestion protocol be developed. After digestion, the fluoride amounts in these GIC samples were analyzed by using ion-selective fluoride combination electrode. The method developed is able to provide fluoride anion content in GICs without interference from the decomposition products of [FB(C 2F5)3]- anion. For the boron analyses the same digestion procedure above is used and the B contents were determined by ICP-AES. For Cx[FB(C2F 5)3]·deltaF, both compositional parameters x and delta are obtained from the results of elemental B and F analyses. For the chemically prepared GICs at 1 h to 20 h, calculated x values were in the range of 51-56 and the calculated delta values increased with reaction time from approx. 0-2. Combining B analysis and TGA mass loss gives a composition of x = 44 and delta = 0.37 for the electrochemically prepared GIC of Cx[FB(C2F5)3]·deltaCH 3NO2. Energy minimized structure for the isolated borate anion and powder XRD data show that the borate anions adopt a "lying-down" orientation where the long axes of [FB(C2F5)3] - intercalate anions are parallel to the encasing graphene sheets. The same electrochemical synthesis strategy is also used for the preparation of a new acceptor-type GIC containing the cyclo-hexafluoropropane-1,3-bis(sulfonyl)amide anion, [CF2(CF2SO2)2N] -. The gallery heights of 0.85-0.86 nm are determined by powder X-ray diffraction for stage 2 and 3 products. These GICs are obtained by electrochemical oxidation of graphite in a nitromethane electrolyte. GICs containing the linear anion, [(CF3SO2)2N]- are also prepared in order to compare the gallery heights and the electron charge distributions that helps to understand the GIC stabilities within the graphene sheets. The compositions of GICs containing [CF2(CF 2SO2)2N]- are determined by thermogravimetric, fluorine and nitrogen elemental analyses. GICs of composition Cx[(C2F 5)3PF3] are prepared for the first time by the intercalation of tris(pentafluoroethyl)trifluorophosphate (FAP) anion, [(C 2F5)3PF3]- by electrochemical oxidation of graphite. Powder-XRD data indicate that products are of stages 2-4 with gallery heights of 0.82-0.86 nm. These GICs are characterized by the same methods using TGA and F ion-selective probe analyses.

Nanostructured core-shell electrode materials for electrochemical capacitors

NASA Astrophysics Data System (ADS)

Jiang, Long-bo; Yuan, Xing-zhong; Liang, Jie; Zhang, Jin; Wang, Hou; Zeng, Guang-ming

2016-11-01

Core-shell nanostructure represents a unique system for applications in electrochemical energy storage devices. Owing to the unique characteristics featuring high power delivery and long-term cycling stability, electrochemical capacitors (ECs) have emerged as one of the most attractive electrochemical storage systems since they can complement or even replace batteries in the energy storage field, especially when high power delivery or uptake is needed. This review aims to summarize recent progress on core-shell nanostructures for advanced supercapacitor applications in view of their hierarchical architecture which not only create the desired hierarchical porous channels, but also possess higher electrical conductivity and better structural mechanical stability. The core-shell nanostructures include carbon/carbon, carbon/metal oxide, carbon/conducting polymer, metal oxide/metal oxide, metal oxide/conducting polymer, conducting polymer/conducting polymer, and even more complex ternary core-shell nanoparticles. The preparation strategies, electrochemical performances, and structural stabilities of core-shell materials for ECs are summarized. The relationship between core-shell nanostructure and electrochemical performance is discussed in detail. In addition, the challenges and new trends in core-shell nanomaterials development have also been proposed.

Tested Demonstrations.

ERIC Educational Resources Information Center

Gilbert, George L., Ed.

1988-01-01

Describes two demonstrations for college level chemistry courses including: "Electrochemical Cells Using Sodium Silicate" and "A Simple, Vivid Demonstration of Selective Precipitation." Lists materials, preparation, procedures, and precautions. (CW)

Burnishing rolling process of the surface prepared in the turning process

NASA Astrophysics Data System (ADS)

Kulakowska, Agnieszka; Kukielka, Leon; Kaldunski, Pawel; Bohdal, Lukasz; Patyk, Radoslaw; Chodor, Jaroslaw; Kukielka, Krzysztof

2018-05-01

The aim of this article is to demonstrate the possibility of using burnishing rolling process as the technology of product development. The experimental researches were carried out, showing the ability to form the surface layer of the product with the desired properties. First, during turning rolling the surfaces of the samples were prepared. Then, the surfaces were burnished. The influence of turning process on the state of the surface layer parameters of C45 steel shafts are shown. Among the examined aspects the surface roughness, nano-roughness, material bearing, surface microstructure, metallographic structure were considered. Numerical simulation were conducted. Conclusions from the experiments and simulation were given.

Chemically modified electrodes by nucleophilic substitution of chlorosilylated platinum oxide surfaces

NASA Astrophysics Data System (ADS)

Chen, Chun-Hsien; Hutchison, James H.; Postlethwaite, Timothy A.; Richardson, John N.; Murray, R. W.

1994-07-01

Chlorosilylated platinum oxide electrode surfaces can be generated by reaction of SiCl4 vapor with an electrochemically prepared monolayer of platinum oxide. A variety of nucleophilic agents (such as alcohols, amines, thiols, and Grignard reagents) can be used to displace chloride and thereby functionalize the metal surface. Electroactive surfaces prepared with ferrocene methanol as the nucleophile show that derivatization by small molecules can achieve coverages on the order of a full monolayer. Surfaces modified with long-chain alkyl groups efficiently block electrode reactions of redox probes dissolved in the contacting solution, but other electrochemical (double layer capacitance and surface coverage) and contact angle measurements suggest that these molecule films are not highly ordered, self-assembled monolayers.

Preparation and Electrochemical Performance of Li4Mn5O12 Nanorods using β-MnO2 Nanorods as Precursor

NASA Astrophysics Data System (ADS)

Zhao, Yan; Wang, Li; Mu, Yanlin; Zhang, Chongwei; Zhu, Fan; Liu, Mengjiao; Lai, Qiongyu; Bi, Jian; Gao, Daojiang

2018-03-01

Li4Mn5O12 nanorods were successfully prepared by using β-MnO2 nanorod precursors as self-templates. The obtained Li4Mn5O12 nanorods were approximately 0.8-1.5 μm in length and 0.15 μm in width, and were employed as electrode materials and applied in supercapacitors. The results show that Li4Mn5O12 nanorods can deliver 211 F g-1 within the potential range of 0-1.4 V at a scan rate of 5 mV s-1 in 1 mol L-1 Li2SO4 solution, which presents a good electrochemical performance.

Synthesis and electrochemical performances of amorphous carbon-coated Sn Sb particles as anode material for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Wang, Zhong; Tian, Wenhuai; Liu, Xiaohe; Yang, Rong; Li, Xingguo

2007-12-01

The amorphous carbon coating on the Sn-Sb particles was prepared from aqueous glucose solutions using a hydrothermal method. Because the outer layer carbon of composite materials is loose cotton-like and porous-like, it can accommodate the expansion and contraction of active materials to maintain the stability of the structure, and hinder effectively the aggregation of nano-sized alloy particles. The as-prepared composite materials show much improved electrochemical performances as anode materials for lithium-ion batteries compared with Sn-Sb alloy and carbon alone. This amorphous carbon-coated Sn-Sb particle is extremely promising anode materials for lithium secondary batteries and has a high potentiality in the future use.

Enhanced supercapacitor performances using C-doped porous TiO2 electrodes

NASA Astrophysics Data System (ADS)

Chen, Juanrong; Qiu, Fengxian; Zhang, Ying; Liang, Jianzheng; Zhu, Huijun; Cao, Shunsheng

2015-11-01

Considerable efforts have been paid to develop electrochemical capacitors with energy storage capability in order to meet the demands of multifunctional electronics. Here we report a facile method to fabricate C-doped porous anatase TiO2. This technique involves the preparation of monodisperse cationic polystyrene nanoparticles (CPN), following sequential deposition of tetrabutylorthotitanate (TBT), and directly carbonizing of CPN. Interestingly, during the process of carbonizing CPN, a phase transition of TiO2 will be happened and whist C-doped porous anatase TiO2 is in situ formed. When this porous C-doped TiO2 is used as electrode material to prepare electrochemical capacitor, it manifests a higher capacitance than the commercial P25, effectively broadening it potential for many practical applications.

Calibrating the Truax Rough Rider seed drill for restoration plantings

Treesearch

Loren St. John; Brent Cornforth; Boyd Simonson; Dan Ogle; Derek Tilley

2008-01-01

The purpose of this technical note is to provide a step-by-step approach to calibrating the Truax Rough Rider range drill, a relatively new, state-of-the-art rangeland drill. To achieve the desired outcome of a seeding project, an important step following proper weed control and seedbed preparation is the calibration of the seeding equipment to ensure the recommended...

Superficial physicochemical properties of polyurethane biomaterials as osteogenic regulators in human mesenchymal stem cells fates.

PubMed

Shahrousvand, Mohsen; Sadeghi, Gity Mir Mohamad; Shahrousvand, Ehsan; Ghollasi, Marzieh; Salimi, Ali

2017-08-01

All of the cells' interactions are done through their surfaces. Evaluation of surface physicochemical scaffolds along with other factors is important and determines the fate of stem cells. In this work, biodegradable and biocompatible polyester/polyether based polyurethanes (PUs) were synthesized by polycaprolactone diol (PCL) and poly (tetra methylene ether) glycol (PTMEG) as the soft segment. To assess better the impact of surface parameters such as stiffness and roughness effects on osteogenic differentiation of the human mesenchymal stem cell (hMSC), the dimension effect of substrates was eliminated and two-dimensional membranes were produced by synthesized polyurethane. Surface and bulk properties of prepared 2D membranes such as surface chemistry, roughness, stiffness and tensile behavior were evaluated by Attenuated total reflectance Fourier transform infrared (ATR-FTIR), atomic force microscopy (AFM) and tensile behavior. The prepared 2D PU films had suitable hydrophilicity, biodegradability, water absorption, surface roughness and bulk strength. The hMSCs showed greater osteogenesis expression in PU substrates with more roughness and stiffness than others. The results demonstrated that surface parameters along with other differentiation cues have a synergistic effect on stem cells fates. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation of redox polymer cathodes for thin film rechargeable batteries

DOEpatents

Skotheim, T.A.; Lee, H.S.; Okamoto, Yoshiyuki.

1994-11-08

The present invention relates to the manufacture of thin film solid state electrochemical devices using composite cathodes comprising a redox polymer capable of undergoing oxidation and reduction, a polymer solid electrolyte and conducting carbon. The polymeric cathode material is formed as a composite of radiation crosslinked polymer electrolytes and radiation crosslinked redox polymers based on polysiloxane backbones with attached organosulfur side groups capable of forming sulfur-sulfur bonds during electrochemical oxidation.

Li-cycling properties of molten salt method prepared nano/submicrometer and micrometer-sized CuO for lithium batteries.

PubMed

Reddy, M V; Yu, Cai; Jiahuan, Fan; Loh, Kian Ping; Chowdari, B V R

2013-05-22

We report the synthesis of CuO material by molten salt method at a temperature range, 280 to 950 °C for 3 h in air. This report includes studies on the effect of morphology, crystal structure and electrochemical properties of CuO prepared at different temperatures. Obtained CuO was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and Brunauer-Emmett-Teller (BET) surface area methods. Samples prepared at ≥410 °C showed a single-phase material with a lattice parameter value of a = 4.69 Å, b = 3.43 Å, c = 5.13 Å and surface area values are in the range 1.0-17.0 m(2) g(-1). Electrochemical properties were evaluated via cyclic voltammetry (CV) and galvanostatic cycling studies. CV studies showed a minor difference in the peak potentials depending on preparation temperature and all compounds exhibit a main anodic peak at ~2.45 V and cathodic peaks at ~0.85 V and ~1.25 V vs Li. CuO prepared at 750 °C showed high and stable capacity of ~620 mA h g(-1) at the end of 40th cycle.

The Effects of Fresh Detox Juices on Color Stability and Roughness of Resin-Based Composites.

PubMed

Yikilgan, İhsan; Akgul, Sinem; Hazar, Ahmet; Kedıcı Alp, Cemile; Baglar, Serdar; Bala, Oya

2018-02-27

To evaluate the effects of three fresh detox juices, including an orange, green, and red beverage, on the color stability and surface roughness of three anterior esthetic resin-based composites (RBCs). Disk-shaped specimens were prepared with three different esthetic RBCs (Amaris, G-aenial Anterior, Clearfil Majesty ES-2) according to the manufacturers' instructions. Forty specimens were prepared for each RBC, and all specimens were stored in artificial saliva at 37°C for 24 hours. The initial color values and surface roughness measurements of the specimens were taken using a spectrophotometer and a profilometer. The specimens were then divided into 4 subgroups (n = 10). All specimens except the control specimens were immersed in their designated fresh detox juices (green, red, or orange) for 10 minutes twice a day. Color and surface roughness measurements were taken on day 15 and day 30, and the results were analyzed by one-way ANOVA and Tukey HSD test. The association between color change and surface roughness was evaluated by Spearman's Rank Correlation analysis. Color changes and surface roughness increased upon exposure to fresh detox juices for 15 and 30 days for all of the RBCs. All of the G-aenial and Amaris groups displayed color changes above the threshold of acceptability, whereas Clearfil Majesty ES-2 displayed a color change above the threshold of acceptability only after exposure to the red beverage for 30 days (ΔE > 3.7). With regard to surface roughness, Clearfil Majesty ES-2 outperformed the other RBCs (p < 0.001). According to Spearman's Rank Correlation analysis, there was no correlation between color change and surface roughness (p > 0.001). Exposure to the fresh detox juices used in this study led to similar color changes in the RBCs used in this study. © 2018 by the American College of Prosthodontists.

Synthesis of porous NiO/CeO2 hybrid nanoflake arrays as a platform for electrochemical biosensing

NASA Astrophysics Data System (ADS)

Cui, Jiewu; Luo, Jinbao; Peng, Bangguo; Zhang, Xinyi; Zhang, Yong; Wang, Yan; Qin, Yongqiang; Zheng, Hongmei; Shu, Xia; Wu, Yucheng

2015-12-01

Porous NiO/CeO2 hybrid nanoflake arrays fabricated by a facile hydrothermal method were employed as substrates for electrochemical biosensors. The resulting NiO/CeO2 hybrid nanoflake arrays with a large specific surface area and good biocompatibility presented an excellent platform for electrochemical biosensing.Porous NiO/CeO2 hybrid nanoflake arrays fabricated by a facile hydrothermal method were employed as substrates for electrochemical biosensors. The resulting NiO/CeO2 hybrid nanoflake arrays with a large specific surface area and good biocompatibility presented an excellent platform for electrochemical biosensing. Electronic supplementary information (ESI) available: Optical photographs of the as-prepared samples, SEM, TEM, EDS, XRD and BET data of the samples are presented, I-t curves of glucose biosensors based on NiO and NiO/CeO2 NFAs, EIS results of different electrodes. See DOI: 10.1039/c5nr05924k

One-Step Electrochemical Preparation of Multilayer Graphene Functionalized with Nitrogen

NASA Astrophysics Data System (ADS)

Ustavytska, Olena; Kurys, Yaroslav; Koshechko, Vyacheslav; Pokhodenko, Vitaly

2017-03-01

A new environmentally friendly one-step method for producing multilayer (preferably 7-9 layers) nitrogen-doped graphene (N-MLG) with a slight amount of oxygen-containing defects was developed. The approach is based on the electrochemical exfoliation of graphite electrode in the presence of azide ions under the conditions of electrolysis with pulse changing of the electrode polarization potential. It was found that usage of azide anions lead not only to the exfoliation of graphite but also to the simultaneous functionalization of graphene sheets by nitrogen atoms (as a result of electrochemical decomposition of azide anions with ammonia evolution). Composition, morphology, structure, and electrochemical properties of N-MLG were characterized by C,H,N analysis, transmission electron microscopy, atomic force microscopy, FTIR, UV-Vis, and Raman spectroscopy, as well as cyclic voltammetry. The perspective of using N-MLG as oxygen reduction reaction electrocatalyst and for the electrochemical analysis of biomarkers (dopamine, ascorbic acid, and uric acid) in their mixtures was shown.

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

PubMed

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.

Contribution of tin in electrochemical properties of zinc antimonate nanostructures: An electrode material for supercapacitors

NASA Astrophysics Data System (ADS)

Balasubramaniam, M.; Balakumar, S.

2018-04-01

Tin (Sn) doped ZnSb2O6 nanostructures was synthesized by chemical precipitation method and was used as an electrode material for supercapacitors to explore its electrochemical stability and potentiality as energy storage materials. Their characteristic structural, morphological and compositional features were investigated through XRD, FESEM and XPS analysis. Results showed that the nanostructures have well ordered crystalline features with spherical particle morphology. As the size and morphology are the vital parameters in exhibiting better electrochemical properties, the prepared nanostructures exhibited a significant specific capacitance of 222 F/g at a current density of 0.5 A/g respectively. While charging and discharging for 1000 cycles, the capacitance retention was enhanced to 105.0% which depicts the stability and activeness of electrochemical sites present in the Sn doped ZnSb2O6 nanostructures even after cycling. Hence, the inclusion of Sn into ZnSb2O6 has contributed in improving the electrochemical properties thereby it represents itself as a potential electrode material for supercapacitors.

Amperometric sensing of hydrogen peroxide using glassy carbon electrode modified with copper nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sophia, J.; Muralidharan, G., E-mail: muraligru@gmail.com

2015-10-15

In this paper, fabrication of glassy carbon electrode (GCE) modified with nano copper particles is discussed. The modified electrode has been tested for the non-enzymatic electrochemical detection of hydrogen peroxide (H{sub 2}O{sub 2}). The copper nanoparticles (Cu NPs) were prepared employing a simple chemical reduction method. The presence of Cu NPs was confirmed through UV–visible (UV–vis) absorption spectroscopy and X-ray diffraction (XRD) analysis. The size and morphology of the particles were investigated using transmission electron microscopy (TEM). The electrochemical properties of the fabricated sensor were studied via cyclic voltammetry (CV), chronoamperometry and electrochemical impedance spectroscopy (EIS). The electrochemical sensor displayedmore » excellent performance features towards H{sub 2}O{sub 2} detection exhibiting wide linear range, low detection limit, swift response time, good reproducibility and stability.« less

Application of N-doped graphene modified carbon ionic liquid electrode for direct electrochemistry of hemoglobin.

PubMed

Sun, Wei; Dong, Lifeng; Deng, Ying; Yu, Jianhua; Wang, Wencheng; Zhu, Qianqian

2014-06-01

Nitrogen-doped graphene (NG) was synthesized and used for the investigation on direct electrochemistry of hemoglobin (Hb) with a carbon ionic liquid electrode as the substrate electrode. Due to specific characteristics of NG such as excellent electrocatalytic property and large surface area, direct electron transfer of Hb was realized with enhanced electrochemical responses appearing. Electrochemical behaviors of Hb on the NG modified electrode were carefully investigated with the electrochemical parameters calculated. The Hb modified electrode exhibited excellent electrocatalytic reduction activity toward different substrates, such as trichloroacetic acid and H2O2, with wider dynamic range and lower detection limit. These findings show that NG can be used for the preparation of chemically modified electrodes with improved performance and has potential applications in electrochemical sensing. Copyright © 2014 Elsevier B.V. All rights reserved.

Electrochemical impedimetric sensor based on molecularly imprinted polymers/sol-gel chemistry for methidathion organophosphorous insecticide recognition.

PubMed

Bakas, Idriss; Hayat, Akhtar; Piletsky, Sergey; Piletska, Elena; Chehimi, Mohamed M; Noguer, Thierry; Rouillon, Régis

2014-12-01

We report here a novel method to detect methidathion organophosphorous insecticides. The sensing platform was architected by the combination of molecularly imprinted polymers and sol-gel technique on inexpensive, portable and disposable screen printed carbon electrodes. Electrochemical impedimetric detection technique was employed to perform the label free detection of the target analyte on the designed MIP/sol-gel integrated platform. The selection of the target specific monomer by electrochemical impedimetric methods was consistent with the results obtained by the computational modelling method. The prepared electrochemical MIP/sol-gel based sensor exhibited a high recognition capability toward methidathion, as well as a broad linear range and a low detection limit under the optimized conditions. Satisfactory results were also obtained for the methidathion determination in waste water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Evaluation of a QuECHERS-like extraction approach for the determination of PBDEs in mussels by immuno-assay-based screening methods

USDA-ARS?s Scientific Manuscript database

A sample preparation method was evaluated for the determination of polybrominated diphenyl ethers (PBDEs) in mussel samples, by using colorimetric and electrochemical immunoassay-based screening methods. A simple sample preparation in conjunction with a rapid screening method possesses the desired c...

Synthesis and electrochemical performance of Ti3C2Tx with hydrothermal process

NASA Astrophysics Data System (ADS)

Wang, Libo; Zhang, Heng; Wang, Bo; Shen, Changjie; Zhang, Chuanxiang; Hu, Qianku; Zhou, Aiguo; Liu, Baozhong

2016-09-01

In this study, a simple hydrothermal method has been developed to prepare Ti3C2Tx from Ti3AlC2 as a high-performance electrode material for supercapacitors. This method is environmentally friendly and has a low level of danger. The morphology and structure of the Ti3C2Tx can be controlled by hydrothermal reaction time, temperature and NH4F amounts. The prepared Ti3C2Tx was characterized by X-ray diffraction, field emission scanning electron microscopy, Raman spectroscopy, X-ray photoelectron spectroscopy and Brunauer-Emmet-Teller. The results show that the prepared Ti3C2Tx is terminated by O, OH, and F groups. The electrochemical properties of the Ti3C2Tx sample exhibit specific capacitance up to 141 Fcm-3 in 3 M KOH aqueous electrolyte, and even after 1000 cycles, no significant degradation of the volumetric capacitance was observed. These results indicate that the Ti3C2Tx material prepared by this hydrothermal method can be used in high performance supercapacitors.

Biocorrosion of TiO2 nanoparticle coating of Ti-6Al-4V in DMEM under specific in vitro conditions

NASA Astrophysics Data System (ADS)

Höhn, Sarah; Virtanen, Sannakaisa

2015-02-01

A TiO2 nanoparticle coating was prepared on a biomedical Ti-6Al-4V alloy using "spin-coating" technique with a colloidal suspension of TiO2 nanopowders with the aim to optimize the surface morphology (e.g., roughness) for improved biocompatibility. The influence of a TiO2 nanoparticle (NP) coating on the corrosion behavior, metal ion release, and biomimetic apatite formation was studied in DMEM, at 37.5 °C with a continuous supply of 5% CO2. Electrochemical impedance spectroscopy measurements indicate a formation of a new layer on the surface of the NP-coated sample upon 28 days immersion in DMEM. Scanning electron microscopy (SEM) and X-ray spectroscopy confirm that the surface of the NP-coated Ti-6Al-4V shows a complete coverage by a Ca-phosphate layer in contrast to the non-coated Ti-6Al-4V alloy. Hence, the TiO2-NP coating strongly enhances biomimetic apatite formation on the alloy surface. In addition, the TiO2-NP coating can efficiently reduce Al-release from the alloy, for which the bare Ti-6Al-4V alloy is significant for at least 28 days of immersion in DMEM.

New thin films of NiO doped with V2O5 for electrochromic applications

NASA Astrophysics Data System (ADS)

Azevedo, Cristiane F.; Balboni, Raphael D. C.; Cholant, Camila M.; Moura, Elton A.; Lemos, Rafaela M. J.; Pawlicka, Agnieszka; Gündel, Andre; Flores, Wladimir H.; Pereira, Marcelo; Avellaneda, César O.

2017-11-01

This paper reports on synthesis and characterization of new electrochromic thin films of NiO doped with V2O5 that were prepared by the sol-gel method and deposited by the spin coating technique. The confirmation of the presence of the dopant in the structure of the films was given by energy-dispersive X-ray spectroscopy (EDX). The effect of the addition of vanadium to the films of NiO was evaluated by electrochemical techniques such as cyclic voltammetry, chronocoulometry, and chronoamperometry in 0.5 mol/L KOH electrolyte. The morphology and the structure of the films, determined by microscopies (SEM and AFM), reveal smooth and slightly rough surfaces. The addition of vanadium as a dopant does not produce changes in the host NiO matrix as evidenced by X-ray diffractometry (XRD). However, the addition of the dopant causes a significant improvement in a charge density values of the films that increase more than twice from 25.5 mC/cm2 for NiO to 52.8 mC/cm2 for NiO with 10 mol% of V2O5. V2O5 doping of NiO films also improved their optical properties as well as kinetics of insertion and extraction processes.

Electrochemical properties of thin films of V2O5 doped with TiO2

NASA Astrophysics Data System (ADS)

Moura, E. A.; Cholant, C. M.; Balboni, R. D. C.; Westphal, T. M.; Lemos, R. M. J.; Azevedo, C. F.; Gündel, A.; Flores, W. H.; Gomez, J. A.; Ely, F.; Pawlicka, A.; Avellaneda, C. O.

2018-08-01

The paper presents a systematic study of the electrochromic properties of thin films of V2O5:TiO2 for a possible utilization as counter-electrode in electrochromic devices. The V2O5:TiO2 thin films were prepared by the sol-gel process and deposited on a substrate of fluorine-tin oxide transparent electrode (FTO) using the dip coating technique and heat treatment at 350 °C for 30 min. The films were characterized by chronocoulometry, cyclic voltammetry (CV), UV-Vis, scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), atomic force microscopy (AFM), profilometry, and X-ray diffraction (XRD). The best results were obtained for the film of V2O5 with 7.5 mol% of TiO2, which presented highest ion storage capacity of ∼106 mC cm-2 and redox reversibility of 1. The diffusion of the Li+ ions into the thin films was modeled by solving Fick equations with appropriate boundary conditions for a plane sheet geometry. Besides that, these films showed optical modulation of 35% at 633 nm after coloration and bleaching. The XRD patterns revealed that the films have an orthorhombic crystal structure; the AFM and the profilometry confirmed roughness and thickness of 16.76 and 617 nm, respectively.

Facile incorporation of hydroxyapatite onto an anodized Ti surface via a mussel inspired polydopamine coating

NASA Astrophysics Data System (ADS)

Zhe, Wang; Dong, Chaofang; Sefei, Yang; Dawei, Zhang; Kui, Xiao; Xiaogang, Li

2016-08-01

Inspired by the porous morphology of anodized Ti and the adhesive versatility of polydopamine (PDA), which can induce apatite mineralization, we fabricated a novel interface by coating a porous anodized TiO2 layer with PDA to rapidly immobilize HA on Ti-based substrates. It was found that the as-prepared PDA/anodized (HD) surface exhibited nanoscale roughness, which possessed an excellent ability to form apatite when immersed in 1.5× simulated body fluid (SBF), as observed by AFM and FE-SEM. The morphology and composition of each layer were further confirmed by XPS, XRD and FTIR. The corrosion resistance of the multilayer was investigated using potentiodynamic polarization curve and electrochemical impedance spectra (EIS) measurements in a 0.9 wt% NaCl solution, the results suggested that the HA/PDA/anodized (HDA) layer increased the corrosion resistance of pure Ti with higher corrosion potential and lower passive current, the surface wettability was also enhanced with the incorporation of HA. In vitro cellular assays showed that the HDA layer stimulated cell attachment and improved the alkaline phosphate (ALP) activity. Overall, the PDA/anodized treatment provided a viable method to quickly integrate HA, and the obtained HDA layer improved both corrosion resistance and biocompatibility of the Ti surface.

Electrochemical Study of Hydrocarbon-Derived Electrolytes for Supercapacitors

NASA Astrophysics Data System (ADS)

Noorden, Zulkarnain A.; Matsumoto, Satoshi

2013-10-01

In this paper, we evaluate the essential electrochemical properties - capacitive and resistive behaviors - of hydrocarbon-derived electrolytes for supercapacitor application using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The electrolytes were systematically prepared from three hydrocarbon-derived compounds, which have different molecular structures and functional groups, by treatment with high-concentration sulfuric acid (H2SO4) at room temperature. Two-electrode cells were assembled by sandwiching an electrolyte-containing glass wool separator with two active electrodes of activated carbon sheets. The dc electrical properties of the tested cells in terms of their capacitive behavior were investigated by CV, and in order to observe the frequency characteristics of the constructed cells, EIS was carried out. Compared with the tested cell with only high-concentration H2SO4 as the electrolyte, the cell with the derived electrolytes exhibit a capacitance as high as 135 F/g with an improved overall internal resistance of 2.5 Ω. Through the use of a simple preparation method and low-cost precursors, hydrocarbon-derived electrolytes could potentially find large-scale and higher-rating supercapacitor applications.

Electrochemical characteristics of discrete, uniform, and monodispersed hollow mesoporous carbon spheres in double-layered supercapacitors.

PubMed

Chen, Xuecheng; Kierzek, Krzysztof; Wenelska, Karolina; Cendrowski, Krzystof; Gong, Jiang; Wen, Xin; Tang, Tao; Chu, Paul K; Mijowska, Ewa

2013-11-01

Core-shell-structured mesoporous silica spheres were prepared by using n-octadecyltrimethoxysilane (C18TMS) as the surfactant. Hollow mesoporous carbon spheres with controllable diameters were fabricated from core-shell-structured mesoporous silica sphere templates by chemical vapor deposition (CVD). By controlling the thickness of the silica shell, hollow carbon spheres (HCSs) with different diameters can be obtained. The use of ethylene as the carbon precursor in the CVD process produces the materials in a single step without the need to remove the surfactant. The mechanism of formation and the role played by the surfactant, C18TMS, are investigated. The materials have large potential in double-layer supercapacitors, and their electrochemical properties were determined. HCSs with thicker mesoporous shells possess a larger surface area, which in turn increases their electrochemical capacitance. The samples prepared at a lower temperature also exhibit increased capacitance as a result of the Brunauer-Emmett-Teller (BET) area and larger pore size. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Enhanced electrochemical performance of amorphous carbon nanotube-manganese-di-oxide-poly-pyrrole ternary nanohybrid

NASA Astrophysics Data System (ADS)

Pahari, D.; Das, N. S.; Das, B.; Howli, P.; Chattopadhyay, K. K.; Banerjee, D.

2017-12-01

Amorphous carbon nanotubes (a-CNTs) manganese di oxide (MnO2)-poly pyrrole (PPy) ternary nanocomposites have been synthesized by a simple chemical route. The as prepared samples have been characterized with different characterization tools that include field emission scanning and high resolution transmission electron microscopy, Raman, Fourier transformed infrared as well as UV-Vis spectroscopy. The electrochemical performance of all the as prepared pure and hybrid samples have been studied in detail. It has been seen that the ternary hybrid shows efficient electrochemical performance with high value of specific capacitance with good stability even up to 2000 cycles. The superior performance of the hybrid samples can be attributed to the strong synergistic effect between the components resulting electron shuttling along PPy main chains and inter-chain raising built-in continuous conductive network. The ternary composite approach offers an effective solution to enhance the device performance of metal-oxide based supercapacitors for long cycling applications. These studies can well speculate the existence of another supercapacitor hybrid for the use in environment friendly electrode and thus a pollution free nature.

Preparation of IrO2-Ta2O5|Ti electrodes by immersion, painting and electrophoretic deposition for the electrochemical removal of hydrocarbons from water.

PubMed

Herrada, Rosa Alhelí; Medel, Alejandro; Manríquez, Federico; Sirés, Ignasi; Bustos, Erika

2016-12-05

After intense years of great development, the electrochemical technologies have become very suitable alternatives in niche markets like industrial wastewater reclamation and soil remediation. A key role to achieve a high efficiency in such treatments is played by the characteristics of the coating of the electrodes employed. This paper compares three techniques, namely immersion, painting and electrophoresis, for the preparation of IrO2-Ta2O5ǀTi, so-called dimensionally stable anodes (DSA(®)). The quality of the coatings has been investigated by means of surface and electrochemical analysis. Their ability to generate hydroxyl radicals and degrade aqueous solutions of hydrocarbons like phenanthrene, naphthalene and fluoranthene has been thoroughly assessed. Among the synthesis techniques, electrophoretic deposition yielded the best results, with DSA(®) electrodes exhibiting a homogeneous surface coverage that led to a good distribution of active sites, thus producing hydroxyl radicals that were able to accelerate the degradation of hydrocarbons. Copyright © 2016 Elsevier B.V. All rights reserved.

A novel fullerene lipoic acid derivative: Synthesis and preparation of self-assembled monolayers on gold

NASA Astrophysics Data System (ADS)

Viana, A. S.; Leupold, S.; Eberle, C.; Shokati, T.; Montforts, F.-P.; Abrantes, L. M.

2007-11-01

Synthesis and preparation of self-assembled monolayers of a novel fullerene lipoic acid derivative on gold are reported. The presence of densely packed SAMs was confirmed by ellipsometry and cyclic voltammetry. The electrochemical response of the modified electrode in organic media exhibits the first two redox peaks characteristic of the extended π-electron system of fullerene. C 60 surface coverage (1.4 × 10 -10 mol cm -2) has been electrochemically determined by the redox process of the adsorbed fullerene moiety and by reductive desorption of the SAM in strong alkaline solution. Electrochemical data indicate that all four sulphur atoms are involved in the self-assembly process, providing an increase of SAM stability in comparison to mono or di-thiolated appended molecules. Visualisation of discrete fullerene molecules by scanning tunnelling microscopy supplied further evidence for gold modification and molecular distribution on the surface. Mixed monolayers of hexanethiol and fullerene derivatives in a proportion of 1:2 have been also studied with the purpose of controlling the amount and distribution of fullerene units on the gold surface.

Efficient photo-catalytic degradation of malachite green using nickel tungstate material as photo-catalyst.

PubMed

Helaïli, N; Boudjamaa, A; Kebir, M; Bachari, K

2017-03-01

The present study focused on the evaluation of photo-catalytic and photo-electrochemical properties of the photo-catalyst based on nickel tungstate material prepared by a nitrate method through the degradation of malachite green (MG) dye's. The effect of catalyst loading and dye concentration was examined. Physico-chemical, optical, electrical, electrochemical, and photo-electrochemical properties of the prepared material were analyzed by X-ray diffraction (XRD), fourier transform-infrared spectroscopy (FTIR), BET analysis, optical reflectance diffuse (DR), scanning electron microscopy (SEM/EDX), electrical conductivity, cyclic voltammetry (CV), current intensity, mott-shottky, and nyquist. XRD revealed the formation of monoclinic structure with a small particle size. BET surface area of the sample was around 10 m 2 /g. The results show that the degradation of MG was more than 80%, achieved after 3 h of irradiation at pH 4.6 and with a catalyst loading of 75 mg. Also, it was found that the dye photo-degradation obeyed the pseudo-first order kinetic via Langmuir Hinshelwood model.

Corrosion Protection Performance of Nano-SiO2/Epoxy Composite Coatings in Acidic Desulfurized Flue Gas Condensates

NASA Astrophysics Data System (ADS)

Wang, Z. B.; Wang, Z. Y.; Hu, H. X.; Liu, C. B.; Zheng, Y. G.

2016-09-01

Five kinds of nano-SiO2/epoxy composite coatings were prepared on mild steels, and their corrosion protection performance was evaluated at room temperature (RT) and 50 °C (HT) using electrochemical methods combined with scanning electron microscopy (SEM). The effects of preparation and sealing processes on the corrosion protection performance of epoxy coatings were specially focused on. The results showed that it was favorable for the corrosion protection and durable performance to add the modified nano-SiO2 during rather than after the synthesis of epoxy coatings. Furthermore, the employment of sealer varnish also had beneficial effects. The two better coatings still exhibited higher impedance values even after immersion tests for up to 1000 h at RT and 500 h at HT. SEM revealed that the improvement of corrosion protection performance mainly resulted from the enhancement of coating density. Moreover, the evolution of electrochemical behavior of the two better coatings with immersion time was also discussed by means of fitting the electrochemical impedance spectroscopy results using equivalent circuits with different physical meanings.

A Facile Electrochemical Preparation of Reduced Graphene Oxide@Polydopamine Composite: A Novel Electrochemical Sensing Platform for Amperometric Detection of Chlorpromazine

NASA Astrophysics Data System (ADS)

Palanisamy, Selvakumar; Thirumalraj, Balamurugan; Chen, Shen-Ming; Wang, Yi-Ting; Velusamy, Vijayalakshmi; Ramaraj, Sayee Kannan

2016-09-01

We report a novel and sensitive amperometric sensor for chlorpromazine (CPZ) based on reduced graphene oxide (RGO) and polydopamine (PDA) composite modified glassy carbon electrode. The RGO@PDA composite was prepared by electrochemical reduction of graphene oxide (GO) with PDA. The RGO@PDA composite modified electrode shows an excellent electro-oxidation behavior to CPZ when compared with other modified electrodes such as GO, RGO and GO@PDA. Amperometric i-t method was used for the determination of CPZ. Amperometry result shows that the RGO@PDA composite detects CPZ in a linear range from 0.03 to 967.6 μM. The sensor exhibits a low detection limit of 0.0018 μM with the analytical sensitivity of 3.63 ± 0.3 μAμM-1 cm-2. The RGO@PDA composite shows its high selectivity towards CPZ in the presence of potentially interfering drugs such as metronidazole, phenobarbital, chlorpheniramine maleate, pyridoxine and riboflavin. In addition, the fabricated RGO@PDA modified electrode showed an appropriate recovery towards CPZ in the pharmaceutical tablets.

Experimental characterization of electrochemically polymerized polycarbazole film and study of its behavior with different metals contacts

NASA Astrophysics Data System (ADS)

Srivastava, Aditi; Chakrabarti, P.

2017-12-01

In this paper, we present the method of fabrication, experimental characterization, and comparison of electrical parameters of semiconducting polycarbazole film with different rectifying metals contacts. Electrochemical polymerization and deposition of organic semiconductor, i.e., polycarbazole on ITO-coated glass substrate, were performed using an electrochemical workstation. Experimental characterization of the prepared polymer film was done in respect of morphology, absorption, bandgap, and thickness. The stability and electro-activity of polycarbazole film were verified by the cyclic voltammetric method. Study of the behavior of prepared polycarbazole film with the different metals contacts such as Aluminum, Copper, Tungsten, and Tin has been done using semiconductor device analyzer. Various electrical parameters such as barrier height, ideality factor, and reverse saturation current have been extracted with different metal contacts, and the values were compared and contrasted. The nature of I- V characteristic of polycarbazole film in non-contact mode has also been analyzed using scanning tunneling microscope. The rectifying I- V characteristics obtained with different metals contacts have also been validated by the simulation on Deckbuild platform of the of ATLAS® software tool from Silvaco Inc.

Electrochemical investigation of MoTe2/rGO composite materials for sodium-ion battery application

NASA Astrophysics Data System (ADS)

Panda, Manas Ranjan; Anish Raj, K.; Sarkar, Ananta; Bao, Qiaoliang; Mitra, Sagar

2018-05-01

2D layered materials are found to be promising anode materials for renewable energy storage devices like sodium and Li-ion batteries and have become attractive options due to their high specific capacity, abundance and low cost. In this work, we synthesized 2D MoTe2 layers embedded in reduced graphene oxide (rGO) anode material for sodium-ion battery applications. 2D MoTe2 was prepared by a solid-state reaction in vacuum at a temperature of 800 °C. The prepared composite material MoTe2/rGO showed excellent electrochemical performance against the sodium metal. The discharge capacity of MoTe2/rGO was observed to be 280 mAh g-1 at a current rate of 1.0 A g-1 for 100 cycles. rGO plays an important role in embedding the MoTe2 structure, thus improving the electrical and mechanical properties, leading to a superior cycling stability and excellent electrochemical performances of MoTe2 for sodium-ion battery applications.

Design of a Battery Intermediate Storage System for Rep-Rated Pulsed Power Loads

DTIC Science & Technology

2013-04-01

will be charged with a bank of LiFePO4 batteries in conjunction with a DC-DC converter. During discharge, the batteries will generate heat from the...able to use typical wall power. High power electrochemical cells will be used as the prime power source and emerging technologies such as LiFePO4 ...LFP26650 LiFePO4 cells connected in series [1]. Each cell has a capacity of roughly 2.6Ah, has an approximate internal resistance of 9mΩ, and a

Aluminum doped nickel oxide thin film with improved electrochromic performance from layered double hydroxides precursor in situ pyrolytic route

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shi, Jingjing; Lai, Lincong; Zhang, Ping

Electrochromic materials with unique performance arouse great interest on account of potential application values in smart window, low-power display, automobile anti-glare rearview mirror, and e-papers. In this paper, high-performing Al-doped NiO porous electrochromic film grown on ITO substrate has been prepared via a layered double hydroxides(LDHs) precursor in situ pyrolytic route. The Al{sup 3+} ions distributed homogenously within the NiO matrix can significantly influence the crystallinity of Ni-Al LDH and NiO:Al{sup 3+} films. The electrochromic performance of the films were evaluated by means of UV–vis absorption spectroscopy, cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and chronoamperometry(CA) measurements. In addition, themore » ratio of Ni{sup 3+}/Ni{sup 2+} also varies with Al content which can lead to different electrochemical performances. Among the as-prepared films, NiO film prepared from Ni-Al (19:1) LDH show the best electrochromic performance with a high transparency of 96%, large optical modulation range (58.4%), fast switching speed (bleaching/coloration times are 1.8/4.2 s, respectively) and excellent durability (30% decrease after 2000 cycles). The improved performance was owed to the synergy of large NiO film specific surface area and porous morphology, as well as Al doping stifled the formation of Ni{sup 3+} making bleached state more pure. This LDHs precursor pyrolytic method is simple, low-cost and environmental benign and is feasible for the preparation of NiO:Al and other Al-doped oxide thin film. - Graphical abstract: The ratio of Ni{sup 3+}/Ni{sup 2+} varies with Al content which can lead to different electrochemical performances. Among the as-prepared films, NiO film prepared from Ni-Al (19:1) LDH show the best electrochromic performance with a high transparency of 96%, large optical modulation range, fast switching speed and excellent durability. Display Omitted.« less

Integrated electrochemical microsystems for genetic detection of pathogens at the point of care.

PubMed

Hsieh, Kuangwen; Ferguson, B Scott; Eisenstein, Michael; Plaxco, Kevin W; Soh, H Tom

2015-04-21

The capacity to achieve rapid, sensitive, specific, quantitative, and multiplexed genetic detection of pathogens via a robust, portable, point-of-care platform could transform many diagnostic applications. And while contemporary technologies have yet to effectively achieve this goal, the advent of microfluidics provides a potentially viable approach to this end by enabling the integration of sophisticated multistep biochemical assays (e.g., sample preparation, genetic amplification, and quantitative detection) in a monolithic, portable device from relatively small biological samples. Integrated electrochemical sensors offer a particularly promising solution to genetic detection because they do not require optical instrumentation and are readily compatible with both integrated circuit and microfluidic technologies. Nevertheless, the development of generalizable microfluidic electrochemical platforms that integrate sample preparation and amplification as well as quantitative and multiplexed detection remains a challenging and unsolved technical problem. Recognizing this unmet need, we have developed a series of microfluidic electrochemical DNA sensors that have progressively evolved to encompass each of these critical functionalities. For DNA detection, our platforms employ label-free, single-step, and sequence-specific electrochemical DNA (E-DNA) sensors, in which an electrode-bound, redox-reporter-modified DNA "probe" generates a current change after undergoing a hybridization-induced conformational change. After successfully integrating E-DNA sensors into a microfluidic chip format, we subsequently incorporated on-chip genetic amplification techniques including polymerase chain reaction (PCR) and loop-mediated isothermal amplification (LAMP) to enable genetic detection at clinically relevant target concentrations. To maximize the potential point-of-care utility of our platforms, we have further integrated sample preparation via immunomagnetic separation, which allowed the detection of influenza virus directly from throat swabs and developed strategies for the multiplexed detection of related bacterial strains from the blood of septic mice. Finally, we developed an alternative electrochemical detection platform based on real-time LAMP, which not is only capable of detecting across a broad dynamic range of target concentrations, but also greatly simplifies quantitative measurement of nucleic acids. These efforts represent considerable progress toward the development of a true sample-in-answer-out platform for genetic detection of pathogens at the point of care. Given the many advantages of these systems, and the growing interest and innovative contributions from researchers in this field, we are optimistic that iterations of these systems will arrive in clinical settings in the foreseeable future.

Lunar terrain mapping and relative-roughness analysis

NASA Technical Reports Server (NTRS)

Rowan, L. C.; Mccauley, J. F.; Holm, E. A.

1971-01-01

Terrain maps of the equatorial zone were prepared at scales of 1:2,000,000 and 1:1,000,000 to classify lunar terrain with respect to roughness and to provide a basis for selecting sites for Surveyor and Apollo landings, as well as for Ranger and Lunar Orbiter photographs. Lunar terrain was described by qualitative and quantitative methods and divided into four fundamental classes: maria, terrae, craters, and linear features. Some 35 subdivisions were defined and mapped throughout the equatorial zone, and, in addition, most of the map units were illustrated by photographs. The terrain types were analyzed quantitatively to characterize and order their relative roughness characteristics. For some morphologically homogeneous mare areas, relative roughness can be extrapolated to the large scales from measurements at small scales.

Time-dependent behavior of rough discontinuities under shearing conditions

NASA Astrophysics Data System (ADS)

Wang, Zhen; Shen, Mingrong; Ding, Wenqi; Jang, Boan; Zhang, Qingzhao

2018-02-01

The mechanical properties of rocks are generally controlled by their discontinuities. In this study, the time-dependent behavior of rough artificial joints under shearing conditions was investigated. Based on Barton’s standard profile lines, samples with artificial joint surfaces were prepared and used to conduct the shear and creep tests. The test results showed that the shear strength of discontinuity was linearly related to roughness, and subsequently an empirical equation was established. The long-term strength of discontinuity can be identified using the inflection point of the isocreep-rate curve, and it was linearly related to roughness. Furthermore, the ratio of long-term and instantaneous strength decreased with the increase of roughness. The shear-stiffness coefficient increased with the increase of shear rate, and the influence of shear rate on the shear stiffness coefficient decreased with the decrease of roughness. Further study of the mechanism revealed that these results could be attributed to the different time-dependent behavior of intact and joint rocks.

Powder, paper and foam of few-layer graphene prepared in high yield by electrochemical intercalation exfoliation of expanded graphite.

PubMed

Wu, Liqiong; Li, Weiwei; Li, Peng; Liao, Shutian; Qiu, Shengqiang; Chen, Mingliang; Guo, Yufen; Li, Qi; Zhu, Chao; Liu, Liwei

2014-04-09

A facile and high-yield approach to the preparation of few-layer graphene (FLG) by electrochemical intercalation exfoliation (EIE) of expanded graphite in sulfuric acid electrolyte is reported. Stage-1 H2SO4-graphite intercalation compound is used as a key intermediate in EIE to realize the efficient exfoliation. The yield of the FLG sheets (<7 layers) with large lateral sizes (tens of microns) is more than 75% relative to the total amount of starting expanded graphite. A low degree of oxygen functionalization existing in the prepared FLG flakes enables them to disperse effectively, which contributes to the film-forming characteristics of the FLG flakes. These electrochemically exfoliated FLG flakes are integrated into several kinds of macroscopic graphene structures. Flexible and freestanding graphene papers made of the FLG flakes retain excellent conductivity (≈24,500 S m(-1)). Three-dimensional (3D) graphene foams with light weight are fabricated from the FLG flakes by the use of Ni foams as self-sacrifice templates. Furthermore, 3D graphene/Ni foams without any binders, which are used as supercapacitor electrodes in aqueous electrolyte, provide the specific capacitance of 113.2 F g(-1) at a current density of 0.5 A g(-1), retaining 90% capacitance after 1000 cycles. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effect of lithium and sodium salt on the performance of Nb2O5/rGO nanocomposite based supercapacitor

NASA Astrophysics Data System (ADS)

Ahmed, Sultan; Rafat, M.

2018-03-01

The present work reports the synthesis of Nb2O5/rGO composite using hydrothermal method and thermal annealing process. The prepared composite was found to have suitable characteristics necessary to be used as electrode material in supercapacitors. These characteristics were ascertained employing the techniques of scanning electron microscopy (SEM), x-ray diffraction (XRD), Raman spectroscopy and N2 adsorption-desorption isotherm. Further, the electrochemical performance of the prepared composite was compared in two different organic electrolytes, of lithium and sodium salt using the techniques of electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV) and charge-discharge measurements. The organic electrolyte solutions were prepared by dispersing 1 M LiClO4/NaClO4 in a mixture of ethylene carbonate/propylene carbonate (1:1 by volume). The observed results indicate that the composite of Nb2O5/rGO offers higher value of specific capacitance in sodium salt electrolyte and higher cyclic stability in lithium salt electrolyte. This is probably due to ion properties of electrolyte. Specific capacitance is observed according to efficient ion/charge diffusion/exchange and relaxation time (Li+ < Na+), while the cyclic stability is observed according to cation size (Na+ > Li+). Thus, the present study reveals the significant effect of electrolyte ions on electrochemical performance of Nb2O5/rGO composite.

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

NASA Astrophysics Data System (ADS)

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.

Sulfur-doped nanoporous carbon spheres with ultrahigh specific surface area and high electrochemical activity for supercapacitor

NASA Astrophysics Data System (ADS)

Liu, Simin; Cai, Yijin; Zhao, Xiao; Liang, Yeru; Zheng, Mingtao; Hu, Hang; Dong, Hanwu; Jiang, Sanping; Liu, Yingliang; Xiao, Yong

2017-08-01

Development of facile and scalable synthesis process for the fabrication of nanoporous carbon materials with large specific surface areas, well-defined nanostructure, and high electrochemical activity is critical for the high performance energy storage applications. The key issue is the dedicated balance between the ultrahigh surface area and highly porous but interconnected nanostructure. Here, we demonstrate the fabrication of new sulfur doped nanoporous carbon sphere (S-NCS) with the ultrahigh surface area up to 3357 m2 g-1 via a high-temperature hydrothermal carbonization and subsequent KOH activation process. The as-prepared S-NCS which integrates the advantages of ultrahigh porous structure, well-defined nanospherical and modification of heteroatom displays excellent electrochemical performance. The best performance is obtained on S-NCS prepared by the hydrothermal carbonization of sublimed sulfur and glucose, S-NCS-4, reaching a high specific capacitance (405 F g-1 at a current density of 0.5 A g-1) and outstanding cycle stability. Moreover, the symmetric supercapacitor is assembled by S-NCS-4 displays a superior energy density of 53.5 Wh kg-1 at the power density of 74.2 W kg-1 in 1.0 M LiPF6 EC/DEC. The synthesis method is simple and scalable, providing a new route to prepare highly porous and heteroatom-doped nanoporous carbon spheres for high performance energy storage applications.

Direct Electrochemical Preparation of Cobalt, Tungsten, and Tungsten Carbide from Cemented Carbide Scrap

NASA Astrophysics Data System (ADS)

Xiao, Xiangjun; Xi, Xiaoli; Nie, Zuoren; Zhang, Liwen; Ma, Liwen

2017-02-01

A novel process of preparing cobalt, tungsten, and tungsten carbide powders from cemented carbide scrap by molten salt electrolysis has been investigated in this paper. In this experiment, WC-6Co and NaCl-KCl salt were used as sacrificial anode and electrolyte, respectively. The dissolution potential of cobalt and WC was determined by linear sweep voltammetry to be 0 and 0.6 V ( vs Ag/AgCl), respectively. Furthermore, the electrochemical behavior of cobalt and tungsten ions was investigated by a variety of electrochemical techniques. Results of cyclic voltammetry (CV) and square-wave voltammetry show that the cobalt and tungsten ions existed as Co2+ and W2+ on melts, respectively. The effect of applied voltage, electrolysis current, and electrolysis times on the composition of the product was studied. Results showed that pure cobalt powder can be obtained when the electrolysis potential is lower than 0.6 V or during low current and short times. Double-cathode and two-stage electrolysis was utilized for the preparation of cobalt, tungsten carbide, and tungsten powders. Additionally, X-ray diffraction results confirm that the product collected at cathodes 1 and 2 is pure Co and WC, respectively. Pure tungsten powder was obtained after electrolysis of the second part. Scanning electron microscope results show that the diameters of tungsten, tungsten carbide, and cobalt powder are smaller than 100, 200, and 200 nm, respectively.

La0.8Sr0.2Fe0.8Cu0.2O3-δ as “cobalt-free” cathode for La0.8Sr0.2Ga0.8Mg0.2O3-δ electrolyte

NASA Astrophysics Data System (ADS)

Zurlo, Francesca; Di Bartolomeo, Elisabetta; D'Epifanio, Alessandra; Felice, Valeria; Natali Sora, Isabella; Tortora, Luca; Licoccia, Silvia

2014-12-01

A "cobalt-free" cathode material with stoichiometric composition La0.8Sr0.2Fe0.8Cu0.2O3-δ (LSFCu) was specifically developed for use with La0.8Sr0.2Ga0.8Mg0.2O3-δ (LSGM) electrolyte in intermediate temperature solid oxide fuel cell (IT-SOFC) systems. The chemical stability of LSFCu in contact with LSGM electrolyte was investigated by structural and morphological analysis. The electrochemical properties of LSFCu dense pellets were investigated in the temperature range 600-750 °C by electrochemical impedance spectroscopy (EIS). LSFCu|LSGM|LSFCu symmetrical cells were prepared and area specific resistance (ASR) values, directly depending on the rate limiting step of the oxygen reduction reaction, were evaluated. Fuel cells were prepared using LSFCu as cathode material on a LSGM pellet and electrochemical tests were performed in the 700-800 °C temperature range and compared to similar fuel cells prepared by using commercial La0.6Sr0.4Fe0.8Co0.2O3-δ (LSFCo) as a cathode. The maximum current density and power density recorded for LSFCu and LSFCo were similar. This fact demonstrates that Cu can be used as Co substitute in perovskite cathode materials.

High-Temperature Stable Anatase Titanium Oxide Nanofibers for Lithium-Ion Battery Anodes.

PubMed

Lee, Sangkyu; Eom, Wonsik; Park, Hun; Han, Tae Hee

2017-08-02

Control of the crystal structure of electrochemically active materials is an important approach to fabricating high-performance electrodes for lithium-ion batteries (LIBs). Here, we report a methodology for controlling the crystal structure of TiO 2 nanofibers by adding aluminum isopropoxide to a common sol-gel precursor solution utilized to create TiO 2 nanofibers. The introduction of aluminum cations impedes the phase transformation of electrospun TiO 2 nanofibers from the anatase to the rutile phase, which inevitably occurs in the typical annealing process utilized for the formation of TiO 2 crystals. As a result, high-temperature stable anatase TiO 2 nanofibers were created in which the crystal structure was well-maintained even at high annealing temperatures of up to 700 °C. Finally, the resulting anatase TiO 2 nanofibers were utilized to prepare LIB anodes, and their electrochemical performance was compared to pristine TiO 2 nanofibers that contain both anatase and rutile phases. Compared to the electrode prepared with pristine TiO 2 nanofibers, the electrode prepared with anatase TiO 2 nanofibers exhibited excellent electrochemical performances such as an initial Coulombic efficiency of 83.9%, a capacity retention of 89.5% after 100 cycles, and a rate capability of 48.5% at a current density of 10 C (1 C = 200 mA g -1 ).

Electrochemical aptasensor for detecting tetracycline in milk

NASA Astrophysics Data System (ADS)

Hanh Le, Thi; Phuc Pham, Van; Huyen La, Thi; Binh Phan, Thi; Huan Le, Quang

2016-03-01

A rapid, simple and sensitive biosensor system for tetracycline detection is very important in food safety. In this paper we developed a label-free aptasensor for electrochemical detection of tetracycline. According to the electrochemical impendence spectroscopy (EIS) analysis, there was a linear relationship between the concentration of tetracycline and the electron transfer resistance from 10 to 3000 ng ml-1 of the tetracycline concentration. The detection limit was 10 ng ml-1 in 15 min detection duration. The prepared aptasensor showed a good reproducibility with an acceptable stability in tetracycline detection. The recoveries of tetracycline in spiked milk samples were in the range of 88.1%-94.2%. The aptasensor has sensitivity 98% and specificity of 100%.

Enhanced lithium storage performance of hierarchical CuO nanomaterials with surface fractal characteristics

NASA Astrophysics Data System (ADS)

Li, Ang; He, Renyue; Bian, Zhuo; Song, Huaihe; Chen, Xiaohong; Zhou, Jisheng

2018-06-01

Self-assembled hierarchical CuO nanostructures with fractal structures were prepared by a mild method and exhibited excellent lithium storage properties, certain of which even demonstrated a high reversible capacity of 827 mAh g-1 at a rate of 0.1 C. An interesting phenomenon was observed that the electrochemical performance varies along with the structure complexity, and the products with higher surface factal dimensions exhibited larger capability and better cyclability. Structural and electrochemical analysis methods were used to explore the lithiation kinetics of the samples and the reasons for the outstanding electrochemical performances related to the complexities of hierarchical nanostructures and the irregularities of surface and mass distribution.

In-situ microwave irradiation synthesis of ZnO-graphene nanocomposite for high-performance supercapacitor applications

NASA Astrophysics Data System (ADS)

Gunaseelan, R.; Venkatachalam, V.; Raj, A. Antony

2018-04-01

In this paper, the ZnO/G nanocomposite was synthesized by facile in-situ microwave irradiation method. The as-prepared ZnO/G composite has been characterized with X-ray powder diffraction. The electrochemical properties of the obtained composite electrode for supercapacitor have been studied by cyclic voltammetry and electrochemical impedance spectra analyses. The ZnO/G nanocomposites showed a good capacitive behavior with a higher specific capacitance of 140.4 F/g at a scan rate of 5 mV/s scan rate in 1M KOH electrolyte. Based on the electrochemical results revealed that the composite electrode is a suitable candidate for supercapacitor applications.

Effect of counterface roughness on the friction of bionic wall-shaped microstructures for gecko-like attachments.

PubMed

Kasem, Haytam; Cohen, Yossi

2017-08-04

Hairy adhesive systems involved in gecko locomotion have drawn the interest of many researchers regarding the development of bionic solutions for fast and reversible adhesive technologies. To date, despite extensive efforts to design gecko-inspired adhesive surfaces, adhesion and friction capacities are often evaluated using smooth and rigid counterfaces, in general glass, whereas most natural and artificial surfaces inevitably have a certain level of roughness. For that reason, in this study experiments tested the effects of the substrate roughness on the friction of bionic wale-shaped microstructures for gecko-like attachments. To this end, 12 substrates with different isotropic roughness were prepared using the same Epoxy material. Friction force was measured under various normal loads. It was concluded that classical roughness parameters, considered separately, are not appropriate to explain roughness-related variations in friction force. This has led us to develop a new integrative roughness parameter that combines characteristics of the surface. The parameter is capable of classifying the obtained experimental results in a readable way. An analytical model based on the experimental results has been developed to predict the variation of the friction force as a function of counterface roughness and applied normal load.

Electrochemical potassium-ion intercalation in NaxCoO2: a novel cathode material for potassium-ion batteries.

PubMed

Sada, Krishnakanth; Senthilkumar, Baskar; Barpanda, Prabeer

2017-07-27

Reversible electrochemical potassium-ion intercalation in P2-type Na x CoO 2 was examined for the first time. Hexagonal Na 0.84 CoO 2 platelets prepared by a solution combustion synthesis technique were found to work as an efficient host for K + intercalation. They deliver a high reversible capacity of 82 mA h g -1 , good rate capability and excellent cycling performance up to 50 cycles.

Electrophoretic nanotechnology of graphene-carbon nanotube and graphene-polypyrrole nanofiber composites for electrochemical supercapacitors.

PubMed

Shi, Kaiyuan; Zhitomirsky, Igor

2013-10-01

Thin films of multiwalled carbon nanotubes (MWCNT), graphene and polypyrrole (PPy) nanofibers were prepared by cathodic electrophoretic deposition (EPD) from aqueous suspensions, containing safranin (SAF) as a new dispersant. The results of Fourier transform infrared spectroscopy, UV-Vis spectroscopy studies and sedimentation tests, coupled with deposition yield and electron microscopy data showed that SAF adsorbed on MWCNT, graphene and PPy, provided their dispersion and charging in the suspensions and allowed efficient EPD. The deposition yield can be controlled by the variation of SAF concentration in the suspensions and deposition time. The use of SAF as a co-dispersant for MWCNT, graphene and PPy, allowed controlled EPD of composite graphene-MWCNT and graphene-PPy films. The proposed approach for the deposition of PPy paves the way for EPD of neutral polymers using organic dyes as dispersing and charging agents. The composite films were investigated for application in electrochemical supercapacitors (ES). The graphene-MWCNT and graphene-PPy films showed significant increase in capacitance, decrease in resistance and increase in capacitance retention at high charge-discharge rates compared to the films of individual components. The analysis of electrochemical testing results and electron microscopy data provided an insight into the influence of composite microstructure on electrochemical performance. The composites, prepared by EPD are promising materials for electrodes of ES. Copyright © 2013 Elsevier Inc. All rights reserved.

Sulfur nanocrystals anchored graphene composite with highly improved electrochemical performance for lithium-sulfur batteries

NASA Astrophysics Data System (ADS)

Zhang, Jun; Dong, Zimin; Wang, Xiuli; Zhao, Xuyang; Tu, Jiangping; Su, Qingmei; Du, Gaohui

2014-12-01

Two kinds of graphene-sulfur composites with 50 wt% of sulfur are prepared using hydrothermal method and thermal mixing, respectively. Transmission Electron Microscopy (TEM) and Energy Dispersive X-ray Spectra mapping show that sulfur nanocrystals with size of ∼5 nm dispersed on graphene sheets homogeneously for the sample prepared by hydrothermal method (NanoS@G). While for the thermal mixed graphene-sulfur composite (S-G mixture), sulfur shows larger and uneven size (50-200 nm). X-ray Photoelectron Spectra (XPS) reveals the strong chemical bonding between the sulfur nanocrystals and graphene. Comparing with the S-G mixture, the NanoS@G composite shows highly improved electrochemical performance as cathode for lithium-sulfur (Li-S) battery. The NanoS@G composite delivers an initial capacity of 1400 mAh g-1 with the sulfur utilization of 83.7% at a current density of 335 mA g-1. The capacity keeps above 720 mAh g-1 over 100 cycles. The strong adherence of the sulfur nanocrystals on graphene immobilizes sulfur and polysulfides species and suppressed the "shuttle effect", resulting higher coulombic efficiency and better capacity retention. Electrochemical impedance also suggests that the strong bonding enabled rapid electronic/ionic transport and improved electrochemical kinetics, therefore good rate capability is obtained. These results demonstrate that the NanoS@G composite is a very promising candidate for high-performance Li-S batteries.

Ultrafast electrochemical preparation of graphene/CoS nanosheet counter electrodes for efficient dye-sensitized solar cells

DOE PAGES

Zhu, Chongyang; Zhu, Yimei; Min, Huihua; ...

2015-10-05

Utilizing inexpensive, high-efficiency counter electrodes (CEs) to replace the traditional platinum counterparts in dye-sensitized solar cells (DSSCs) is worthwhile. In this paper, we detail how we synchronously prepared composite CEs of CoS nanosheet arrays and reduced graphene oxide (rGO) layers for the first time via a low temperature, ultrafast one-step electrochemical strategy. With this approach, the whole fabrication process of the composite CEs was only a small percentage of the average time (~15 hours) using other methods. The DSSC assembled with the rGO–CoS composite CE achieved an enhanced power conversion efficiency (PCE) of 8.34%, which is dramatically higher than 6.27%more » of pure CoS CE-based DSSC and even exceeds 7.50% of Pt CE-based DSSC. The outstanding PCE breakthrough is undoubtedly attributed to the enhancement in electrocatalytic ability of the rGO–CoS composite CE due to the incorporation of highly conducting rGO layers and the GO layers-induced growth of CoS nanosheet arrays with higher density and larger surface area. Therefore, lower charge-transfer resistance and higher exchange current density can be achieved as corroborated by the electrochemical impedance spectra (EIS) and Tafel polarization curves (TPCs). As a result, further experiments also proved that the electrochemical strategy exhibited its universality of fabricating other graphene-enhanced chalcogenide functional composite films.« less

Carbon dots-decorated multiwalled carbon nanotubes nanocomposites as a high-performance electrochemical sensor for detection of H2O2 in living cells.

PubMed

Bai, Jing; Sun, Chunhe; Jiang, Xiue

2016-07-01

A novel enzyme-free hydrogen peroxide sensor composed of carbon dots (CDs) and multi-walled carbon nanotubes (MWCNTs) was prepared. It was found that the carbon dots-decorated multi-walled carbon nanotubes nanocomposites (CDs/MWCNTs) modified glassy carbon (GC) electrode (CDs/MWCNTs/GCE) exhibited a significant synergistic electrocatalytic activity towards hydrogen peroxide reduction as compared to carbon dots or multi-walled carbon nanotubes alone, and the CDs/MWCNTs/GCE has shown a low detection limit as well as excellent stability, selectivity, and reproducibility. These remarkable analytical advantages enable the practical application of CDs/MWCNTs/GCE for the real-time tracking of hydrogen peroxide (H2O2) released from human cervical cancer cells with satisfactory results. The enhanced electrochemical activity can be assigned to the edge plane-like defective sites and lattice oxygen in the CDs/MWCNTs nanocomposites due to the small amount of decoration of carbon dots on the multi-walled carbon nanotubes. Based on a facile preparation method and with good electrochemical properties, the CDs/MWCNTs nanocomposites represent a new class of carbon electrode for electrochemical sensor applications. Graphical Abstract CDs/MWCNTs exhibited good electrocatalytic activity and stability to H2O2 reduction and can be used for real-time detection of H2O2 released from living cells.

Synthesis of chemical vapor deposition graphene on tantalum wire for supercapacitor applications

NASA Astrophysics Data System (ADS)

Li, Mingji; Guo, Wenlong; Li, Hongji; Xu, Sheng; Qu, Changqing; Yang, Baohe

2014-10-01

This paper studies the synthesis and electrochemical characterization of graphene/tantalum (Ta) wires as high-performance electrode material for supercapacitors. Graphene on Ta wires is prepared by the thermal decomposition of methane under various conditions. The graphene nanosheets on the Ta wire surface have an average thickness of 1.3-3.4 nm and consist typically of a few graphene monolayers, and TaC buffer layers form between the graphene and Ta wire. A capacitor structure is fabricated using graphene/Ta wire with a length of 10 mm and a diameter of 0.6 mm as the anode and Pt wire of the same size as the cathode. The electrochemical behavior of the graphene/Ta wires as supercapacitor electrodes is characterized by cyclic voltammetry, galvanostatic charge/discharge, and electrochemical impedance spectroscopy in 1 M Na2SO4 aqueous electrolyte. The as-prepared graphene/Ta electrode has highest capacitance of 345.5 F g-1 at current density of 0.5 A g-1. The capacitance remains at about 84% after 1000 cycles at 10 A g-1. The good electrochemical performance of the graphene/Ta wire electrode is attributed to the unique nanostructural configuration, high electrical conductivity, and large specific surface area of the graphene layer. This suggests that graphene/Ta wire electrode materials have potential applications in high-performance energy storage devices.

Skin-Attachable, Stretchable Electrochemical Sweat Sensor for Glucose and pH Detection.

PubMed

Oh, Seung Yun; Hong, Soo Yeong; Jeong, Yu Ra; Yun, Junyeong; Park, Heun; Jin, Sang Woo; Lee, Geumbee; Oh, Ju Hyun; Lee, Hanchan; Lee, Sang-Soo; Ha, Jeong Sook

2018-04-25

As part of increased efforts to develop wearable healthcare devices for monitoring and managing physiological and metabolic information, stretchable electrochemical sweat sensors have been investigated. In this study, we report on the fabrication of a stretchable and skin-attachable electrochemical sensor for detecting glucose and pH in sweat. A patterned stretchable electrode was fabricated via layer-by-layer deposition of carbon nanotubes (CNTs) on top of patterned Au nanosheets (AuNS) prepared by filtration onto stretchable substrate. For the detection of glucose and pH, CoWO 4 /CNT and polyaniline/CNT nanocomposites were coated onto the CNT-AuNS electrodes, respectively. A reference electrode was prepared via chlorination of silver nanowires. Encapsulation of the stretchable sensor with sticky silbione led to a skin-attachable sweat sensor. Our sensor showed high performance with sensitivities of 10.89 μA mM -1 cm -2 and 71.44 mV pH -1 for glucose and pH, respectively, with mechanical stability up to 30% stretching and air stability for 10 days. The sensor also showed good adhesion even to wet skin, allowing the detection of glucose and pH in sweat from running while being attached onto the skin. This work suggests the application of our stretchable and skin-attachable electrochemical sensor to health management as a high-performance healthcare wearable device.

A general approach for MFe2O4 (M = Zn, Co, Ni) nanorods and their high performance as anode materials for lithium ion batteries

NASA Astrophysics Data System (ADS)

Wang, Nana; Xu, Huayun; Chen, Liang; Gu, Xin; Yang, Jian; Qian, Yitai

2014-02-01

MFe2O4 (M = Zn, Co, Ni) nanorods are synthesized by a template-engaged reaction, with β-FeOOH nanorods as precursors which are prepared by a hydrothermal method. The final products are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and high-resolution transmission electron microscopy (HRTEM). The electrochemical properties of the MFe2O4 (M = Zn, Co, Ni) nanorods are tested as the anode materials for lithium ion batteries. The reversible capacities of 800, 625 and 520 mAh g-1 are obtained for CoFe2O4, ZnFe2O4 and NiFe2O4, respectively, at the high current density of 1000 mA g-1 even after 300 cycles. The superior lithium-storage performances of MFe2O4 (M = Zn, Co, Ni) nanorods can be attributed to the one-dimensional (1D) nanostructure, which can shorten the diffusion paths of lithium ions and relax the strain generated during electrochemical cycling. These results indicate that this method is an effective, simple and general way to prepare good electrochemical properties of 1D spinel Fe-based binary transition metal oxides. In addition, the impact of different reaction temperatures on the electrochemical properties of MFe2O4 nanorods is also investigated.

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

PubMed

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

2018-02-06

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

Investigation of performance and durability of polymer electrolytes for electrochemical energy storage and conversion technologies

NASA Astrophysics Data System (ADS)

Jung, Min-Suk

Polymeric ion exchange membranes are integral components of electrochemical conversion/storage devices such as fuel cells, water electrolyzers, and redox flow batteries. There has been dramatic progress in the research and development of cation exchange membranes (CEM). NafionRTM (perfluorosulfonic acid membranes) is one example of a state-of-the-art CEM and has been successfully demonstrated in various electrochemical energy devices. Unlike CEMs, anion exchange membranes (AEMs) have been of limited utility to date due to their drawbacks, including poor chemical/mechanical stability and low ionic conductivity. However, alkaline environments result in better activity for electrochemical reactions and afford the possibility of using non-platinum group metal (PGM) electrocatalysts. AEMs, therefore, are still being studied in order to resolve existing challenges in terms of conductivity and stability in alkaline media and in strongly oxidizing solutions. In this work, AEMs derived from different types of polymer backbones were prepared, and their chemical stability and electrochemical property were investigated. Polysulfone (PSF) AEMs were prepared by first chloromethylating polysulfone, then by functionalizing chloromethylated polysulfone (CMPSF) with different base reagents. PSF-trimethylamine (TMA) AEMs showed a 40-fold reduction in vanadium (IV) ion (VO2+) permeability when compared to a NafionRTM membrane and exceptional oxidative stability after exposure to a 1.5 M vanadium (V) ion (VO2+) solution for 90 days. PSF-TMA AEMs were successfully demonstrated in the all-vanadium redox flow battery. Excellent energy efficiencies (>75 %) were attained and sustained over 75 charge-discharge cycles for a vanadium redox flow battery prepared using the PSF-TMA separator. Crosslinking of poly(2,6-dimethyl-1,4-phenylene oxide) (PPO) AEMs using diamine was tried with intentions to improve the mechanical stability and electrochemical property of PPO AEM. Crosslinked PPO AEMs (30 +/- 4 % at 25 °C) showed less liquid water uptake than non-crosslinked PPO AEMs (46 +/- 5% at 25 °C) while maintaining comparable ionic conductivities (hydroxide ion conductivity of 45 mS/cm at 60 °C). Crosslinked PPO AEMs maintained mechanical integrity and still showed some mechanical stability (ultimate tensile strength of 3˜4 MPa and elongation at break of 13˜17 %) after exposure to 1 M KOH at 60 °C for 14 days, while non-crosslinked PPO AEMs completely lost their mechanical durability. Finally, this dissertation presents research related to perfluorinated AEMs prepared using a Grignard reagent. These membranes exhibited 0.7 mmol/g of Cl- ion exchange capacity (IEC), 20 mS/cm of hydroxide ion conductivity at 20 °C, and 10 % of water uptake at room temperature. The membranes also maintained 90 % of their initial conductivity after an exposure to 1.5 M VO2+ in 3 M H2SO4 solution for seven days.

Preparation and wettability examinations of transparent SiO2 binder-added MgF2 nanoparticle coatings covered with fluoro-alkyl silane self-assembled monolayer.

PubMed

Murata, Tsuyoshi; Hieda, Junko; Saito, Nagahiro; Takai, Osamu

2012-05-01

SiO2-added MgF2 nanoparticle coatings with various surface roughness properties were formed on fused silica-glass substrates from autoclaved sols prepared at 100-180 °C. To give it hydrophobicity, we treated the samples with fluoro-alkyl silane (FAS) vapor to form self-assembled monolayers on the nanoparticle coating and we examined the wettability of the samples. The samples preserved good transparency even after the FAS treatment. The wettability examination revealed that higher autoclave temperatures produced a larger average MgF2 nanoparticle particle size, a larger surface roughness, and a higher contact angle and the roll-off angle.

The effect of grain size on aluminum anodes for Al-air batteries in alkaline electrolytes

NASA Astrophysics Data System (ADS)

Fan, Liang; Lu, Huimin

2015-06-01

Aluminum is an ideal material for metallic fuel cells. In this research, different grain sizes of aluminum anodes are prepared by equal channel angular pressing (ECAP) at room temperature. Microstructure of the anodes is examined by electron backscatter diffraction (EBSD) in scanning electron microscope (SEM). Hydrogen corrosion rates of the Al anodes in 4 mol L-1 NaOH are determined by hydrogen collection method. The electrochemical properties of the aluminum anodes are investigated in the same electrolyte using electrochemical impedance spectroscopy (EIS) and polarization curves. Battery performance is also tested by constant current discharge at different current densities. Results confirm that the electrochemical properties of the aluminum anodes are related to grain size. Finer grain size anode restrains hydrogen evolution, improves electrochemical activity and increases anodic utilization rate. The proposed method is shown to effectively improve the performance of Al-air batteries.

Fabrication and Performance Study on Individual Zno Nanowires Based Bioelectrode

NASA Astrophysics Data System (ADS)

Zhao, Yanguang; Yan, Xiaoqin; Kang, Zhuo; Lin, Pei

2012-08-01

One-dimensional zinc oxide nanowires (ZnO NWs) have unique advantages for use in biosensors as follows: oxide stable surface, excellent biosafety, high specific surface area, high isoelectric point (IEP = 9.5). In this work, we have prepared a kind of electrochemical bioelectrode based on individual ZnO NWs. Here, ZnO NWs with high quality were successfully synthesized by CVD method, which were characterized by scanning electron microscopy, X-ray diffraction and photoluminescence. Then the Raman spectra and electrical characterization demonstrated the adsorption of uricase on ZnO wires. At last, a series of electrochemical measurements were carried out by using an electrochemical workstation with a conventional three-electrode system to obtain the cyclic voltammetry characteristics of the bioelectrodes. The excellent performance of the fabricated bioelectrode implies the potential application for single ZnO nanowire to construct electrochemical biosensor for the detection of uric acid.

Investigating Li 2NiO 2–Li 2CuO 2 Solid Solutions as High-Capacity Cathode Materials for Li-Ion Batteries

DOE PAGES

Xu, Jing; Renfrew, Sara; Marcus, Matthew A.; ...

2017-05-11

Li 2Ni 1–xCu xO 2 solid solutions were prepared by a solid-state method to study the correlation between composition and electrochemical performance. Cu incorporation improved the phase purity of Li 2Ni 1–xCu xO 2 with orthorhombic Immm structure, resulting in enhanced capacity. However, the electrochemical profiles suggested Cu incorporation did not prevent irreversible phase transformation during the electrochemical process, instead, it likely influenced the phase transformation upon lithium removal. By combining ex situ X-ray diffraction (XRD), X-ray absorption spectroscopy (XAS), and differential electrochemical mass spectrometry (DEMS) measurements, this study elucidates the relevant phase transformation (e.g., crystal structure, local environment, andmore » charge compensation) and participation of electrons from lattice oxygen during the first cycle in these complex oxides.« less

Preparation of capacitor's electrode from sunflower seed shell.

PubMed

Li, Xiao; Xing, Wei; Zhuo, Shuping; Zhou, Jin; Li, Feng; Qiao, Shi-Zhang; Lu, Gao-Qing

2011-01-01

Series of nanoporous carbons are prepared from sunflower seed shell (SSS) by two different strategies and used as electrode material for electrochemical double-layer capacitor (EDLC). The surface area and pore-structure of the nanoporous carbons are characterized intensively using N2 adsorption technique. The results show that the pore-structure of the carbons is closely related to activation temperature and dosage of KOH. Electrochemical measurements show that the carbons made by impregnation-activation process have better capacitive behavior and higher capacitance retention ratio at high drain current than the carbons made by carbonization-activation process, which is due to that there are abundant macroscopic pores and less interior micropore surface in the texture of the former. More importantly, the capacitive performances of these carbons are much better than ordered mesoporous carbons and commercial wood-based active carbon, thus highlighting the success of preparing high performance electrode material for EDLC from SSS. Copyright © 2010 Elsevier Ltd. All rights reserved.

Lead paste recycling based on conversion into battery grade oxides. Electrochemical tests and industrial production of new batteries

NASA Astrophysics Data System (ADS)

Fusillo, G.; Rosestolato, D.; Scura, F.; Cattarin, S.; Mattarozzi, L.; Guerriero, P.; Gambirasi, A.; Brianese, N.; Staiti, P.; Guerriero, R.; La Sala, G.

2018-03-01

We present the preparation and characterization of pure lead monoxide obtained through recycling of the lead paste recovered from exhausted lead acid batteries. The recycling is based on a hydrometallurgical procedure reported in a STC Patent, that includes simple chemical operations (desulphurisation, leaching, precipitation, filtration) and a final thermal conversion. Materials obtained by treatment at 600 °C consist predominantly of β-PbO. The electrochemical behaviour of Positive Active Mass (PAM) prepared from different materials (or mixtures) is then investigated and compared. An optimized oxide material, obtained by prolonged (8 h) thermal treatment at 600 °C, consists of pure β-PbO and appears suitable for preparation of battery elements, alone or in mixture with a small fraction (10%-30%) of traditional industrial leady oxide. The resulting battery performances are similar to those obtained from pure leady oxide. In comparison with traditional recycling processes, the proposed method guarantees lower energy consumption, limited environmental impact and reduced operating risk for industry workers.

Preparation of glucose sensors using gold nanoparticles modified diamond electrode

NASA Astrophysics Data System (ADS)

Fachrurrazie; Ivandini, T. A.; Wibowo, W.

2017-04-01

A glucose sensor was successfully developed by immobilizing glucose oxidase (GOx) at boron-doped diamond (BDD) electrodes. Prior to GOx immobilization, the BDD was modified with gold nanoparticles (AuNPs). To immobilize AuNPs, the gold surface was modified to nitrogen termination. The characterization of the electrode surface was performed using an X-ray photoelectron spectroscopy and a scanning electron microscope, while the electrochemical properties of the enzyme electrode were characterized using cyclic voltammetry. Cyclic voltammograms of the prepared electrode for D-glucose in phosphate buffer solution pH 7 showed a new reduction peak at +0.16 V. The currents of the peak were linear in the concentration range of 0.1 M to 0.9 M, indicated that the GOx-AuNP-BDD can be applied for electrochemical glucose detection.

Investigation of novel zinc molybdate-graphene nanocomposite for supercapacitor applications

NASA Astrophysics Data System (ADS)

Reddy, B. Joji; Vickraman, P.; Justin, A. Simon

2018-06-01

Novel zinc molybdate-graphene nanocomposite is prepared for the first time in a fast, facile and eco-friendly microwave synthesis route as an electrode material for electrochemical supercapacitors. The as-prepared sample is investigated by X-ray diffraction, FTIR, Raman, scanning electron microscope and transmission electron microscope techniques. The studies have confirmed the formation of ZnMoO4 and its composite with graphene. The synthesized materials are subjected to electrochemical characterization studies in 2M KOH electrolyte solution which prove that ZnMoO4-graphene as an effective electrode material for supercapacitor applications. ZnMoO4 in its composite behavior has exhibited a specific capacitance of 272.93 F g- 1 at 0.5 A g- 1 with good cyclic stability for 1000 cycles.

Facile and Eco-Friendly Synthesis of Finger-Like Co3O4 Nanorods for Electrochemical Energy Storage

PubMed Central

Sun, Shijiao; Zhao, Xiangyu; Yang, Meng; Ma, Liqun; Shen, Xiaodong

2015-01-01

Co3O4 nanorods were prepared by a facile hydrothermal method. Eco-friendly deionized water rather than organic solvent was used as the hydrothermal media. The as-prepared Co3O4 nanorods are composed of many nanoparticles of 30–50 nm in diameter, forming a finger-like morphology. The Co3O4 electrode shows a specific capacitance of 265 F g−1 at 2 mV s−1 in a supercapacitor and delivers an initial specific discharge capacity as high as 1171 mAh g−1 at a current density of 50 mA g−1 in a lithium ion battery. Excellent cycling stability and electrochemical reversibility of the Co3O4 electrode were also obtained. PMID:28347124

Preparation and electrochemical capacitance performances of super-hydrophilic conducting polyaniline

NASA Astrophysics Data System (ADS)

Li, Xingwei; Li, Xiaohan; Dai, Na; Wang, Gengchao; Wang, Zhun

Super-hydrophilic conducting polyaniline was prepared by surface modification of polyaniline using tetraethyl orthosilicate in water/ethanol solution, whereas its conductivity was 4.16 S cm -1 at 25 °C. And its electrochemical capacitance performances as an electrode material were evaluated by the cyclic voltammetry and galvanostatic charge/discharge test in 0.1 M H 2SO 4 aqueous solution. Its initial specific capacitance was 500 F g -1 at a constant current density of 1.5 A g -1, and the capacitance still reached about 400 F g -1 after 5000 consecutive cycles. Moreover, its capacitance retention ratio was circa 70% with the growth of current densities from 1.5 to 20 A g -1, indicating excellent rate capability. It would be a promising electrode material for aqueous redox supercapacitors.

One step preparation and electrochemical analysis of IQS, a cell-cell communication signal in the nosocomial pathogen Pseudomonas aeruginosa.

PubMed

Shang, Fengjun; Muimhneacháin, Eoin Ó; Jerry Reen, F; Buzid, Alyah; O'Gara, Fergal; Luong, John H T; Glennon, Jeremy D; McGlacken, Gerard P

2014-10-01

Pseudomonas aeruginosa uses a hierarchical cell-cell communication system consisting of a number of regulatory elements to coordinate the expression of bacterial virulence genes. Sensitive detection of quorum sensing (QS) molecules has the potential for early identification of P. aeruginosa facilitating early medical intervention. A recently isolated cell-cell communication molecule, a thiazole termed IQS, can bypass the las QS system of P. aeruginosa under times of stress, activating a subset of QS-controlled genes. This compound offers a new target for pathogen detection and has been prepared in a one step protocol. A simple electrochemical strategy was employed for its sensitive detection using boron-doped diamond and glassy carbon electrodes by cyclic voltammetry and amperometry. Copyright © 2014 Elsevier Ltd. All rights reserved.

Flexible nanopillar-based electrochemical sensors for genetic detection of foodborne pathogens

NASA Astrophysics Data System (ADS)

Park, Yoo Min; Lim, Sun Young; Jeong, Soon Woo; Song, Younseong; Bae, Nam Ho; Hong, Seok Bok; Choi, Bong Gill; Lee, Seok Jae; Lee, Kyoung G.

2018-06-01

Flexible and highly ordered nanopillar arrayed electrodes have brought great interest for many electrochemical applications, especially to the biosensors, because of its unique mechanical and topological properties. Herein, we report an advanced method to fabricate highly ordered nanopillar electrodes produced by soft-/photo-lithography and metal evaporation. The highly ordered nanopillar array exhibited the superior electrochemical and mechanical properties in regard with the wide space to response with electrolytes, enabling the sensitive analysis. As-prepared gold and silver electrodes on nanopillar arrays exhibit great and stable electrochemical performance to detect the amplified gene from foodborne pathogen of Escherichia coli O157:H7. Additionally, lightweight, flexible, and USB-connectable nanopillar-based electrochemical sensor platform improves the connectivity, portability, and sensitivity. Moreover, we successfully confirm the performance of genetic analysis using real food, specially designed intercalator, and amplified gene from foodborne pathogens with high reproducibility (6% standard deviation) and sensitivity (10 × 1.01 CFU) within 25 s based on the square wave voltammetry principle. This study confirmed excellent mechanical and chemical characteristics of nanopillar electrodes have a great and considerable electrochemical activity to apply as genetic biosensor platform in the fields of point-of-care testing (POCT).

Nitrogen-Doped Three Dimensional Graphene for Electrochemical Sensing.

PubMed

Yan, Jing; Chen, Ruwen; Liang, Qionglin; Li, Jinghong

2015-07-01

The rational assembly and doping of graphene play an crucial role in the improvement of electrochemical performance for analytical applications. Covalent assembly of graphene into ordered hierarchical structure provides an interconnected three dimensional conductive network and large specific area beneficial to electrolyte transfer on the electrode surface. Chemical doping with heteroatom is a powerful tool to intrinsically modify the electronic properties of graphene due to the increased free charge-carrier densities. By incorporating covalent assembly and nitrogen doping strategy, a novel nitrogen doped three dimensional reduced graphene oxide nanostructure (3D-N-RGO) was developed with synergetic enhancement in electrochemical behaviors. The as prepared 3D-N-RGO was further applied for catechol detection by differential pulse voltammetry. It exhibits much higher electrocatalytic activity towards catechol with increased peak current and decreased potential difference between the oxidation and reduction peaks. Owing to the improved electro-chemical properties, the response of the electrochemical sensor varies linearly with the catechol concentrations ranging from 5 µM to 100 µM with a detection limit of 2 µM (S/N = 3). This work is promising to open new possibilities in the study of novel graphene nanostructure and promote its potential electrochemical applications.

Differences observed in the surface morphology and microstructure of Ni-Fe-Cu ternary thin films electrochemically deposited at low and high applied current densities

NASA Astrophysics Data System (ADS)

Sarac, U.; Kaya, M.; Baykul, M. C.

2016-10-01

In this research, nanocrystalline Ni-Fe-Cu ternary thin films using electrochemical deposition technique were produced at low and high applied current densities onto Indium Tin Oxide (ITO) coated conducting glass substrates. Change of surface morphology and microstructural properties of the films were investigated. Energy dispersive X-ray spectroscopy (EDX) measurements showed that the Ni-Fe-Cu ternary thin films exhibit anomalous codeposition behaviour during the electrochemical deposition process. From the X-ray diffraction (XRD) analyses, it was revealed that there are two segregated phases such as Cu- rich and Ni-rich within the films. The crystallographic structure of the films was face-centered cubic (FCC). It was also observed that the film has lower lattice micro-strain and higher texture degree at high applied current density. Scanning electron microscopy (SEM) studies revealed that the films have rounded shape particles on the base part and cauliflower-like structures on the upper part. The film electrodeposited at high current density had considerably smaller rounded shape particles and cauliflower-like structures. From the atomic force microscopy (AFM) analyses, it was shown that the film deposited at high current density has smaller particle size and surface roughness than the film grown at low current density.

Rational geometrical engineering of palladium sulfide multi-arm nanostructures as a superior bi-functional electrocatalyst.

PubMed

Nandan, R; Nanda, K K

2017-08-31

Geometrical tunability offers sharp edges and an open-armed structure accompanied with a high electrochemical active surface area to ensure the efficient and effective utilization of materials by exposing the electrochemical active sites for facile accessibility of reactant species. Herein, we report a one-step, single-pot, surfactant-free, electroless, and economic route to synthesize palladium sulfide nanostructures with different geometries at mild temperatures and their catalytic properties towards the oxygen reduction reaction (ORR) and methanol electro-oxidation (MOR). For ORR, the positive on-set, half wave potentials, smaller Tafel slope, high electrochemical active surface area, large roughness factor, and better cyclic stability of the proposed nanostructures as compared to those of the commercial state-of-the-art Pt-C/PdS catalysts suggest their superiority in an alkaline medium. In addition, high mass activity (J f ∼ 715 mA mg -1 ), in comparison with that of the commercial state-of-the-art Pt-C/PdS catalysts (J f ∼ 138/41 mA mg -1 , respectively), and high J f /J b (1.52) along with the superior operational stability of the multi-arm palladium sulfide nanostructures towards MOR advocates the bi-functional behavior of the catalyst and its potential as a promising Pt-free anode/cathode electrocatalyst in fuel cells.

An Ab Initio and Kinetic Monte Carlo Simulation Study of Lithium Ion Diffusion on Graphene

PubMed Central

Zhong, Kehua; Yang, Yanmin; Xu, Guigui; Zhang, Jian-Min; Huang, Zhigao

2017-01-01

The Li+ diffusion coefficients in Li+-adsorbed graphene systems were determined by combining first-principle calculations based on density functional theory with Kinetic Monte Carlo simulations. The calculated results indicate that the interactions between Li ions have a very important influence on lithium diffusion. Based on energy barriers directly obtained from first-principle calculations for single-Li+ and two-Li+ adsorbed systems, a new equation predicting energy barriers with more than two Li ions was deduced. Furthermore, it is found that the temperature dependence of Li+ diffusion coefficients fits well to the Arrhenius equation, rather than meeting the equation from electrochemical impedance spectroscopy applied to estimate experimental diffusion coefficients. Moreover, the calculated results also reveal that Li+ concentration dependence of diffusion coefficients roughly fits to the equation from electrochemical impedance spectroscopy in a low concentration region; however, it seriously deviates from the equation in a high concentration region. So, the equation from electrochemical impedance spectroscopy technique could not be simply used to estimate the Li+ diffusion coefficient for all Li+-adsorbed graphene systems with various Li+ concentrations. Our work suggests that interactions between Li ions, and among Li ion and host atoms will influence the Li+ diffusion, which determines that the Li+ intercalation dependence of Li+ diffusion coefficient should be changed and complex. PMID:28773122

Fabrication of flower-like Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} and their electrochemical properties evaluation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kong, Ling-Bin, E-mail: konglb@lut.cn; School of Materials Science and Engineering, Lanzhou University of Technology, Lanzhou 730050; Deng, Li

Graphical abstract: Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} nano-flakes materials, which have a flower-like structure, were successfully synthesized by a facile solvothermal method without adding any surfactant. The as-prepared Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} possesses a maximum specific capacitance of 2212.5 F g{sup −1} at the current density of 5 mA, suggesting its potential application in electrode material for secondary batteries and electrochemical capacitors. Highlights: ► Flower-like Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} materials were fabricated in a simple method. ► High specific capacitance of 2212.5 F g{sup −1} has been achieved. ► For the first time the effects of concentration andmore » temperature on its specific capacitance has been studied. -- Abstract: Flower-like Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} was successfully synthesized by a facile solvothermal method. The microstructure and surface morphology of prepared Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} were physically characterized by X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM) and transmission electron microscope (TEM). The electrochemical properties studies were carried out using cyclic voltammetry (CV), chronopotentiometry technology and AC impedance spectroscopy, respectively. The results indicate that the flower-like structure has a profound impact on electrode performance at high discharge capacitance. A maximum specific capacitance of 2212.5 F g{sup −1} at the current density of 5 mA could be achieved, suggesting its potential application in electrode material for secondary batteries and electrochemical capacitors. Furthermore, the effects of Ni(NO{sub 3}){sub 2}·6H{sub 2}O concentration and temperature on the microstructure and specific capacitance of prepared Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} have also been systematically studied. The results show that flower-like structure can be formed when the concentration is appropriate, while the temperature has just little effect on its electrochemical properties.« less

Enhanced photo-response of porous silicon photo-detectors by embeddingTitanium-dioxide nano-particles

NASA Astrophysics Data System (ADS)

Ali, Hiba M.; Makki, Sameer A.; Abd, Ahmed N.

2018-05-01

Porous silicon (n-PS) films can be prepared by photoelectochemical etching (PECE) Silicon chips n - types with 15 (mA / cm2), in 15 minutes etching time on the fabrication nano-sized pore arrangement. By using X-ray diffraction measurement and atomic power microscopy characteristics (AFM), PS was investigated. It was also evaluated the crystallites size from (XRD) for the PS nanoscale. The atomic force microscopy confirmed the nano-metric size chemical fictionalization through the electrochemical etching that was shown on the PS surface chemical composition. The atomic power microscopy checks showed the roughness of the silicon surface. It is also notified (TiO2) preparation nano-particles that were prepared by pulse laser eradication in ethanol (PLAL) technique through irradiation with a Nd:YAG laser pulses TiO2 target that is sunk in methanol using 400 mJ of laser energy. It has been studied the structural, optical and morphological of TiO2NPs. It has been detected that through XRD measurement, (TiO2) NPs have been Tetragonal crystal structure. While with AFM measurements, it has been realized that the synthesized TiO2 particles are spherical with an average particle size in the (82 nm) range. It has been determined that the energy band gap of TiO2 NPs from optical properties and set to be in (5eV) range.The transmittance and reflectance spectra have determined the TiO2 NPs optical constants. It was reported the effectiveness of TiO2 NPs expansion on the PS Photodetector properties which exposes the benefits in (Al/PS/Si/Al). The built-in tension values depend on the etching time current density and laser flounce. Al/TiO2/PS/Si/Al photo-detector heterojunction have two response peaks that are situated at 350 nm and (700 -800nm) with max sensitivity ≈ 0.7 A/W. The maximum given detectivity is 9.38at ≈ 780 nm wavelength.

Nonenzymatic free-cholesterol detection via a modified highly sensitive macroporous gold electrode with platinum nanoparticles.

PubMed

Lee, Yi-Jae; Park, Jae-Yeong

2010-12-15

A sensitive macroporous Au electrode with a highly rough surface obtained through the use of with Pt nanoparticles (macroporous Au-/nPts) is reported. It has been designed for nonenzymatic free-cholesterol biosensor applications. A macroporous Au-/nPts electrode was fabricated by electroplating Pt nanoparticles onto a coral-like shaped macroporous Au electrode structure. The macroporous Au-/nPts electrode was physically characterized by field emission scanning electron microscopy (FESEM). It was confirmed that the Pt nanoparticles were well deposited on the surface of the macroporous Au electrode. The porosity and window pore size of the macroporous Au electrode were 50% and 100-300 nm, respectively. The electroplated Pt nanoparticle size was approximately 10-20 nm. Electrochemical experiments showed that the macroporous Au-/nPts exhibited a much larger surface activation area (roughness factor (RF)=2024.7) than the macroporous Au electrode (RF=46.07). The macroporous Au-/nPts also presented a much stronger electrocatalytic activity towards cholesterol oxidation than does the macroporous Au electrode. At 0.2 V, the electrode responded linearly up to a 5 mM cholesterol concentration in a neutral media, with a detection limit of 0.015 mM and detection sensitivity of 226.2 μA mM(-1) cm(-2). Meanwhile, interfering species such as ascorbic acid (AA), acetaminophen (AP), and uric acid (UA), were effectively avoided. This novel nonenzymatic detection electrode has strong applications as an electrochemically based cholesterol biosensor. Copyright © 2010 Elsevier B.V. All rights reserved.

Sequential electrochemical treatment of dairy wastewater using aluminum and DSA-type anodes.

PubMed

Borbón, Brenda; Oropeza-Guzman, Mercedes Teresita; Brillas, Enric; Sirés, Ignasi

2014-01-01

Dairy wastewater is characterized by a high content of hardly biodegradable dissolved, colloidal, and suspended organic matter. This work firstly investigates the performance of two individual electrochemical treatments, namely electrocoagulation (EC) and electro-oxidation (EO), in order to finally assess the mineralization ability of a sequential EC/EO process. EC with an Al anode was employed as a primary pretreatment for the conditioning of 800 mL of wastewater. A complete reduction of turbidity, as well as 90 and 81% of chemical oxygen demand (COD) and total organic carbon (TOC) removal, respectively, were achieved after 120 min of EC at 9.09 mA cm(-2). For EO, two kinds of dimensionally stable anodes (DSA) electrodes (Ti/IrO₂-Ta₂O₅ and Ti/IrO₂-SnO₂-Sb₂O₅) were prepared by the Pechini method, obtaining homogeneous coatings with uniform composition and high roughness. The (·)OH formed at the DSA surface from H₂O oxidation were not detected by electron spin resonance. However, their indirect determination by means of H₂O₂ measurements revealed that Ti/IrO₂-SnO₂-Sb₂O₅ is able to produce partially physisorbed radicals. Since the characterization of the wastewater revealed the presence of indole derivatives, preliminary bulk electrolyses were done in ultrapure water containing 1 mM indole in sulfate and/or chloride media. The performance of EO with the Ti/IrO₂-Ta₂O₅ anode was evaluated from the TOC removal and the UV/Vis absorbance decay. The mineralization was very poor in 0.05 M Na₂SO₄, whereas it increased considerably at a greater Cl(-) content, meaning that the oxidation mediated by electrogenerated species such as Cl₂, HClO, and/or ClO(-) competes and even predominates over the (·)OH-mediated oxidation. The EO treatment of EC-pretreated dairy wastewater allowed obtaining a global 98 % TOC removal, decreasing from 1,062 to <30 mg L(-1).

One-step electrochemical deposition of Schiff base cobalt complex as effective water oxidation catalyst

NASA Astrophysics Data System (ADS)

Huang, Binbin; Wang, Yan; Zhan, Shuzhong; Ye, Jianshan

2017-02-01

Schiff base metal complexes have been applied in many fields, especially, a potential homogeneous catalyst for water splitting. However, the high overpotential, time consumed synthesis process and complicated working condition largely limit their application. In the present work, a one-step approach to fabricate Schiff base cobalt complex modified electrode is developed. Microrod clusters (MRC) and rough spherical particles (RSP) can be obtained on the ITO electrode through different electrochemical deposition condition. Both of the MRC and RSP present favorable activity for oxygen evolution reaction (OER) compared to the commercial Co3O4, taking an overpotential of 650 mV and 450 mV to drive appreciable catalytic current respectively. The highly active and stable RSP shows a Tafel plot of 84 mV dec-1 and negligible decrease of the current density for 12 h bulk electrolysis. The synthesis strategy of effective and stable catalyst in this work provide a simple method to fabricate heterogeneous OER catalyst with Schiff base metal complex.

Highly selective plasma-activated copper catalysts for carbon dioxide reduction to ethylene

DOE PAGES

Mistry, Hemma; Varela, Ana Sofia; Bonifacio, Cecile S.; ...

2016-06-30

There is an urgent need to develop technologies that use renewable energy to convert waste products such as carbon dioxide into hydrocarbon fuels. Carbon dioxide can be electrochemically reduced to hydrocarbons over copper catalysts, although higher efficiency is required. We have developed oxidized copper catalysts displaying lower overpotentials for carbon dioxide electroreduction and record selectivity towards ethylene (60%) through facile and tunable plasma treatments. Herein we provide insight into the improved performance of these catalysts by combining electrochemical measurements with microscopic and spectroscopic characterization techniques. Operando X-ray absorption spectroscopy and cross-sectional scanning transmission electron microscopy show that copper oxides aremore » surprisingly resistant to reduction and copper + species remain on the surface during the reaction. Furthermore, our results demonstrate that the roughness of oxide-derived copper catalysts plays only a partial role in determining the catalytic performance, while the presence of copper + is key for lowering the onset potential and enhancing ethylene selectivity.« less

High-performance aqueous asymmetric supercapacitor based on K0.3WO3 nanorods and nitrogen-doped porous carbon

NASA Astrophysics Data System (ADS)

Ma, Guofu; Zhang, Zhiguo; Sun, Kanjun; Feng, Enke; Peng, Hui; Zhou, Xiaozhong; Lei, Ziqiang

2016-10-01

A novel asymmetric supercapacitor device for energy storage is fabricated using K0.3WO3 nanorods as negative electrode and nitrogen-doped porous carbon (CBC-1) based on agricultural wastes corn bract as positive electrode. The K0.3WO3 nanorods are composed of some thinner needle-shaped nanorods which are parallel to each other, and the CBC-1 reveals rough surface of coral-like frameworks with abundant nanopores. The structures can provide high surface area, low diffusion paths and intercalation/de-intercalation of electrolyte ions between the electrode/electrolyte interfaces. Thus, the asymmetric supercapacitor exhibits high energy density about 26.3 Wh kg-1 at power density of 404.2 W kg-1 in the wide voltage region of 0-1.6 V, as well as a good electrochemical stability (80% capacitance retention after 1000 cycles). Such outstanding electrochemical behaviors imply the CBC-1//K0.3WO3 asymmetric supercapacitor is a promising practical energy-storage system.

A novel approach of chemical mechanical polishing for cadmium zinc telluride wafers.

PubMed

Zhang, Zhenyu; Wang, Bo; Zhou, Ping; Kang, Renke; Zhang, Bi; Guo, Dongming

2016-05-26

A novel approach of chemical mechanical polishing (CMP) is developed for cadmium zinc telluride (CdZnTe or CZT) wafers. The approach uses environment-friendly slurry that consists of mainly silica, hydrogen peroxide, and citric acid. This is different from the previously reported slurries that are usually composed of strong acid, alkali, and bromine methanol, and are detrimental to the environment and operators. Surface roughness 0.5 nm and 4.7 nm are achieved for Ra and peak-to-valley (PV) values respectively in a measurement area of 70 × 50 μm(2), using the developed novel approach. Fundamental polishing mechanisms are also investigated in terms of X-ray photoelectron spectroscopy (XPS) and electrochemical measurements. Hydrogen peroxide dominates the passivating process during the CMP of CZT wafers, indicating by the lowest passivation current density among silica, citric acid and hydrogen peroxide solution. Chemical reaction equations are proposed during CMP according to the XPS and electrochemical measurements.

A novel approach of chemical mechanical polishing for cadmium zinc telluride wafers

PubMed Central

Zhang, Zhenyu; Wang, Bo; Zhou, Ping; Kang, Renke; Zhang, Bi; Guo, Dongming

2016-01-01

A novel approach of chemical mechanical polishing (CMP) is developed for cadmium zinc telluride (CdZnTe or CZT) wafers. The approach uses environment-friendly slurry that consists of mainly silica, hydrogen peroxide, and citric acid. This is different from the previously reported slurries that are usually composed of strong acid, alkali, and bromine methanol, and are detrimental to the environment and operators. Surface roughness 0.5 nm and 4.7 nm are achieved for Ra and peak-to-valley (PV) values respectively in a measurement area of 70 × 50 μm2, using the developed novel approach. Fundamental polishing mechanisms are also investigated in terms of X-ray photoelectron spectroscopy (XPS) and electrochemical measurements. Hydrogen peroxide dominates the passivating process during the CMP of CZT wafers, indicating by the lowest passivation current density among silica, citric acid and hydrogen peroxide solution. Chemical reaction equations are proposed during CMP according to the XPS and electrochemical measurements. PMID:27225310

Study of reticulated vitreous carbon surface treated by plasma immersion ion implantation for electrodes production

NASA Astrophysics Data System (ADS)

Silva, L. L. G.; Conceição, D. A. S.; Oishi, S. S.; Toth, A.; Ueda, M.

2012-03-01

RVC samples were treated by nitrogen plasma immersion ion implantation (N-PIII) for electrodes production. High-voltage pulses with amplitudes of -3.0 kV or -10.0 kV were applied to the RVC samples while the treatment time was 10, 20 and 30 min. The samples were characterized by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and electrochemical measurements. The SEM images present an apparent enhancement of the surface roughness after the treatment probably due to the surface sputtering during the PIII process. This observation is in agreement with the specific electrochemical surface area (SESA) of RVC electrodes. An increase was observed of the SESA values for the PIII-treated samples compared to the untreated specimen. Some oxygen and nitrogen containing groups were introduced on the RVC surface after the PIII treatment. Both plasma-induced process: the surface roughening and the introduction of the polar species on the RVC surface are beneficial for the RVC electrodes application.

Electrochemical synthesis of porous cobalt nanowall arrays

NASA Astrophysics Data System (ADS)

He, Wei; Gao, Peng; Chu, Lei; Yin, Ligen; Li, Zhen; Xie, Yi

2006-07-01

Porous cobalt nanowall arrays have been prepared by electrochemical deposition of mono-precursor [Co(NH3)5Cl]Cl2 on copper substrates. Brunauer-Emmett-Teller (BET) and Barret-Joyner-Halenda (BJH) investigations of the surface properties indicate that the resulting porous nanomaterials possess high surface area and uniform pore size distribution, which implies potential applications in some fields, such as catalysis, energy, and magnetic data storage devices. The magnetism measurements of the porous cobalt nanowall arrays take on a good ferromagnetic behaviour with enhanced coercivity (Hc).

Facile Synthesis of Novel Networked Ultralong Cobalt Sulfide Nanotubes and Its Application in Supercapacitors.

PubMed

Liu, Sangui; Mao, Cuiping; Niu, Yubin; Yi, Fenglian; Hou, Junke; Lu, Shiyu; Jiang, Jian; Xu, Maowen; Li, Changming

2015-11-25

Ultralong cobalt sulfide (CoS(1.097)) nanotube networks are synthesized by a simple one-step solvothermal method without any surfactant or template. A possible formation mechanism for the growth processes is proposed. Owing to the hollow structure and large specific area, the novel CoS(1.097) materials present outstanding electrochemical properties. Electrochemical measurements for supercapacitors show that the as-prepared ultralong CoS(1.097) nanotube networks exhibit high specific capacity, good capacity retention, and excellent Coulombic efficiency.

Flexible capacitive behavior of hybrid carbon materials prepared from graphene sheets

NASA Astrophysics Data System (ADS)

Ding, Y.-H.; Xie, W.; Zhang, P.; Jiang, Y.

2016-06-01

High frequency ultrasonication was employed to reduce the aggregation of graphene by constructing hybrid carbon materials (HCMs), which are endowed with a large electrochemical reaction area and high energy density. HCMs exhibited a specific capacitance of 168.5 F · g-1 with ˜100% capacitance retention over 500 cycles. Flexible supercapacitors fabricated from HCMs also showed an excellent capacitive behavior even under tough conditions. These outstanding electrochemical properties were ascribed to the increased specific surface area and open structure of HCMs.

Method of preparing a powdered, electrically insulative separator for use in an electrochemical cell

DOEpatents

Cooper, Tom O.; Miller, William E.

1978-01-01

A secondary electrochemical cell includes electrodes separated by a layer of electrically insulative powder. The powder includes refractory materials selected from the oxides and nitrides of metals and metaloids. The powdered refractory material, blended with electrolyte particles, is compacted as layers onto an electrode to form an integral electrode structure and assembled into the cell. The assembled cell is heated to its operating temperature leaving porous layers of electrically insulative, refractory particles, containing molten electrolyte between the electrodes.

Point-of-need simultaneous electrochemical detection of lead and cadmium using low-cost stencil-printed transparency electrodes.

PubMed

Martín-Yerga, Daniel; Álvarez-Martos, Isabel; Blanco-López, M Carmen; Henry, Charles S; Fernández-Abedul, M Teresa

2017-08-15

In this work, we report a simple and yet efficient stencil-printed electrochemical platform that can be integrated into the caps of sample containers and thus, allows in-field quantification of Cd(II) and Pb(II) in river water samples. The device exploits the low-cost features of carbon (as electrode material) and paper/polyester transparency sheets (as substrate). Electrochemical analysis of the working electrodes prepared on different substrates (polyester transparency sheets, chromatographic, tracing and office papers) with hexaammineruthenium(III) showed that their electroactive area and electron transfer kinetics are highly affected by the porosity of the material. Electrodes prepared on transparency substrates showed the best electroanalytical performance for the simultaneous determination of Cd(II) and Pb(II) by square-wave anodic stripping voltammetry. Interestingly, the temperature and time at which the carbon ink was cured had significant effect on the electrochemical response, especially the capacitive current. The amount of Cd and Pb on the electrode surface can be increased about 20% by in situ electrodeposition of bismuth. The electrochemical platform showed a linear range comprised between 1 and 200 μg/L for both metals, sensitivity of analysis of 0.22 and 0.087 μA/ppb and limits of detection of 0.2 and 0.3 μg/L for Cd(II) and Pb(II), respectively. The analysis of river water samples was done directly in the container where the sample was collected, which simplifies the procedure and approaches field analysis. The developed point-of-need detection system allowed simultaneous determination of Cd(II) and Pb(II) in those samples using the standard addition method with precise and accurate results. Copyright © 2017 Elsevier B.V. All rights reserved.

The physics of water droplets on surfaces: exploring the effects of roughness and surface chemistry

NASA Astrophysics Data System (ADS)

Eid, K. F.; Panth, M.; Sommers, A. D.

2018-03-01

This paper explores the fluid property commonly called surface tension, its effect on droplet shape and contact angle, and the major influences of contact angle behaviour (i.e. surface roughness and surface chemistry). Images of water droplets placed on treated copper surfaces are used to measure the contact angles between the droplets and the surface. The surface wettability is manipulated either by growing a self-assembled monolayer on the surface to make it hydrophobic or by changing the surface roughness. The main activities in this experiment, then, are (1) preparing and studying surfaces with different surface wettability and roughness; (2) determining the shape and contact angles of water droplets on these surfaces; and (3) demonstrating the spontaneous motion of water droplets using surface tension gradients.

Preparation of Binary and Ternary Oxides by Molten Salt Method and its Electrochemical Properties

NASA Astrophysics Data System (ADS)

Reddy, M. V.; Theng, L. Pei; Soh, Hulbert; Beichen, Z.; Jiahuan, F.; Yu, C.; Ling, A. Yen; Andreea, L. Y.; Ng, C. H. Justin; Liang, T. J. L. Galen; Ian, M. F.; An, H. V. T.; Ramanathan, K.; Kevin, C. W. J.; Daryl, T. Y. W.; Hao, T. Yi; Loh, K. P.; Chowdari, B. V. R.

2013-07-01

We report simple binary oxides namely SnO2, TiO2, CuO, MnO2, Fe2O3, Co3O4 and ternary oxides like MnCo2O4 by molten salt method at a temperature range of 280°C to 950°C in air and discuss the effect of morphology, crystal structure and electrochemical properties of binary and ternary oxides. Materials were characterized by X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and Brunauer-Emmett-Teller (BET) surface area methods. XRD patterns showed all MSM prepared materials exhibited characteristic lattice parameter values. BET surface area varies depending on the nature of the material, molten salt and preparation temperature and the obtained values are in the range, 1 to 160 m2/g. Electrochemical properties were studied using cyclic voltammetry (CV) and electrochemical performance studies were carried in the voltage range, 0.005-1.0V for SnO2, 1.0-2.8V for TiO2 and Fe2O3, MCo2O4 (M = Co, Mn), MnO2 and CuO were cycled in the range, 0.005-3.0V. At a current rates of 30-100 mA/g and a scan rate of 0.058 mV/sec was used for galvanostatic cycling and cyclic voltammetry. SnO2 showed that an alloying-de-alloying reaction occurs at ˜0.2 and ˜0.5 V vs. Li. TiO2 main intercalation and de-interaction reactions at ˜1.7 and ˜1.8 V vs. Li. Co3O4, MnCo2O4, and MnO2 main discharge potentials at ˜1.2, 0.9V and 0.4V, resp. and charge potentials peak ˜2.0V and 1.5V vs. Li. CuO prepared at 750°C exhibited main anodic peak at ˜2.45V and cathodic peaks at ˜0.85V and ˜1.25V. We discussed the possible reaction mechanisms and Li-storage performance values in detail.

A new electrocatalyst and its application method for vanadium redox flow battery

NASA Astrophysics Data System (ADS)

Wei, Guanjie; Jing, Minghua; Fan, Xinzhuang; Liu, Jianguo; Yan, Chuanwei

2015-08-01

The edge plane in carbon structure has good electrocatalytic activity toward vanadium redox reaction. To apply it in vanadium redox flow battery (VRFB) practically, the graphite nanopowders (GNPs) containing amounts of edge planes are used as electrocatalyst and embedded in the electrospun carbon nanofibers (ECNFs) by different mass ratios to make composite electrodes. The morphology and electrochemical activity of the GNPs and the composite electrodes containing them are characterized. Compared with the pristine ECNFs, the composite electrodes show much higher electrochemical activity. With the increase of GNPs content in composite electrodes, the electrochemical reversibility of the vanadium redox couples also increases. It proves the addition of GNPs can surely improve the electrochemical activity of ECNFs. Among the composite electrodes, the ECNFs containing 30 nm GNP by mass ratio of 1:50 show the best electrochemical activity, largest active surface area and excellent stability. Due to the high performance of GNP/ECNFs composite electrode and its relatively low cost preparation process, the GNPs are expected to be used as electrocatalyst in VRFB on a large scale to improve the cell performance.

Construction of self-supported porous TiO2/NiO core/shell nanorod arrays for electrochemical capacitor application

NASA Astrophysics Data System (ADS)

Wu, J. B.; Guo, R. Q.; Huang, X. H.; Lin, Y.

2013-12-01

High-quality metal oxides hetero-structured nanoarrays have been receiving great attention in electrochemical energy storage application. Self-supported TiO2/NiO core/shell nanorod arrays are prepared on carbon cloth via the combination of hydrothermal synthesis and electro-deposition methods. The obtained core/shell nanorods consist of nanorod core and interconnected nanoflake shell, as well as hierarchical porosity. As cathode materials for pseudo-capacitors, the TiO2/NiO core/shell nanorod arrays display impressive electrochemical performances with both high capacitance of 611 F g-1 at 2 A g-1, and pretty good cycling stability with a retention of 89% after 5000 cycles. Besides, as compared to the single NiO nanoflake arrays on carbon cloth, the TiO2/NiO core/shell nanorod arrays exhibit much better electrochemical properties with higher capacitance, better electrochemical activity and cycling life. This enhanced performance is mainly due to the core/shell nanorods architecture offering fast ion/electron transfer and sufficient contact between active materials and electrolyte.

Regulation of the discharge reservoir of negative electrodes in Ni-MH batteries by using Ni(OH) x (x = 2.10) and γ-CoOOH

NASA Astrophysics Data System (ADS)

Shangguan, Enbo; Chang, Zhaorong; Tang, Hongwei; Yuan, Xiao-Zi; Wang, Haijiang

In this paper, a novel strategy to regulate the discharge reservoir of negative electrodes in Ni-MH batteries is introduced by using Ni(OH) x (x = 2.10) and γ-CoOOH. The electrochemical measurements of these batteries demonstrate that the use of Ni(OH) x (x = 2.10) and γ-CoOOH can not only successfully regulate the discharge reservoir of negative electrodes in Ni-MH batteries to an adequate quantity, but also effectively improve the electrochemical performance of the batteries. Compared with normal batteries, the in-house prepared batteries with a lower discharge reservoir exhibit an enhanced discharge capacity, improved high-rate discharge ability, higher discharge potential plateau and superior cycle stability. The effect of Ni(OH) x (x = 2.10) and γ-CoOOH on the electrochemical performance of nickel electrode is also investigated by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The results suggest that the new method is simple and effective for cost reduction of Ni-MH batteries with improved electrochemical performance.

Preparation and characterization of AuNPs/CNTs-ErGO electrochemical sensors for highly sensitive detection of hydrazine.

PubMed

Zhao, Zhenting; Sun, Yongjiao; Li, Pengwei; Zhang, Wendong; Lian, Kun; Hu, Jie; Chen, Yong

2016-09-01

A highly sensitive electrochemical sensor of hydrazine has been fabricated by Au nanoparticles (AuNPs) coating of carbon nanotubes-electrochemical reduced graphene oxide composite film (CNTs-ErGO) on glassy carbon electrode (GCE). Cyclic voltammetry and potential amperometry have been used to investigate the electrochemical properties of the fabricated sensors for hydrazine detection. The performances of the sensors were optimized by varying the CNTs to ErGO ratio and the quantity of Au nanoparticles. The results show that under optimal conditions, a sensitivity of 9.73μAμM(-1)cm(-2), a short response time of 3s, and a low detection limit of 0.065μM could be achieved with a linear concentration response range from 0.3μM to 319μM. The enhanced electrochemical performances could be attributed to the synergistic effect between AuNPs and CNTs-ErGO film and the outstanding catalytic effect of the Au nanoparticles. Finally, the sensor was successfully used to analyse the tap water, showing high potential for practical applications. Copyright © 2016 Elsevier B.V. All rights reserved.

A facile approach to prepare crumpled CoTMPyP/electrochemically reduced graphene oxide nanohybrid as an efficient electrocatalyst for hydrogen evolution reaction

NASA Astrophysics Data System (ADS)

Ma, Juanjuan; Liu, Lin; Chen, Qian; Yang, Min; Wang, Danping; Tong, Zhiwei; Chen, Zhong

2017-03-01

Elaborate design and synthesis of efficient and stable non-Pt electrocatalysts for some renewable energy related conversion/storage processes are one of the major goals of sustainable chemistry. Herein, we report a facile method to fabricate Co porphyrin functionalized electrochemically reduced graphene oxide (CoTMPyP/ERGO) thin film by direct assembly of oppositely charged tetrakis(N-methylpyridyl) porphyrinato cobalt (CoTMPyP) and GO nanosheets under mild conditions followed by an electrochemical reduction procedure. STEM analysis confirms that CoTMPyP nanoaggregates are homogeneously distributed over the graphene surface. The electrochemical properties of CoTMPyP/ERGO were investigated by cyclic voltammetry, linear sweep voltammetry and electrochemical impedance spectroscopy. The results demonstrate that CoTMPyP/ERGO nanohybrid film can serve as excellent electrocatalyst for hydrogen evolution in alkaline solution with high activity and stability. The intimate contact and efficient electron transfer between CoTMPyP and ERGO, as well as the crumpled structure, contribute to the improvement of the electrocatalytic performance.

Ion sensors based on novel fiber organic electrochemical transistors for lead ion detection.

PubMed

Wang, Yuedan; Zhou, Zhou; Qing, Xing; Zhong, Weibing; Liu, Qiongzhen; Wang, Wenwen; Li, Mufang; Liu, Ke; Wang, Dong

2016-08-01

Fiber organic electrochemical transistors (FECTs) based on polypyrrole and nanofibers have been prepared for the first time. FECTs exhibited excellent electrical performances, on/off ratios up to 10(4) and low applied voltages below 2 V. The ion sensitivity behavior of the fiber organic electrochemical transistors was investigated. It exhibited that the transfer curve of FECTs shifted to lower gate voltage with increasing cations concentration, the sensitivity reached to 446 μA/dec in the 10(-5)-10(-2) M Pb(2+) concentration range. The ion selective properties of the FECTs have also been systematically studied for the detection of potassium, calcium, aluminum, and lead ions. The devices with different cations showed great difference in response curves. It was suitable for selectively monitoring Pb(2+) with respect to other cations. The results indicated FECTs were very effective for electrochemical sensing of lead ion, which opened a promising perspective for wearable electronics in healthcare and biological application. Graphical Abstract The schematic diagram of fiber organic electrochemical transistors based on polypyrrole and nanofibers for ion sensing.

Nanocrystalline diamond thin films on titanium-6 aluminum-4 vanadium alloy temporomandibular joint prosthesis simulants by microwave plasma chemical vapor deposition

NASA Astrophysics Data System (ADS)

Fries, Marc Douglas

A course of research has been performed to assess the suitability of nanocrystal-line diamond (NCD) films on Ti-6Al-4V alloy as wear-resistant coatings in biomedical implant use. A series of temporomandibular (TMJ) joint condyle simulants were polished and acid-passivated as per ASTM F86 standard for surface preparation of implants. A 3-mum-thick coating of NCD film was deposited by microwave plasma chemical vapor deposition (MPCVD) over the hemispherical articulation surfaces of the simulants. Plasma chemistry conditions were measured and monitored by optical emission spectroscopy (OES), using hydrogen as a relative standard. The films consist of diamond grains around 20 nm in diameter embedded in an amorphous carbon matrix, free of any detectable film stress gradient. Hardness averages 65 GPa and modulus measures 600 GPa at a depth of 250 nm into the film surface. A diffuse film/substrate boundary produces a minimal film adhesion toughness (GammaC) of 158 J/m2. The mean RMS roughness is 14.6 +/- 4.2 nm, with an average peak roughness of 82.6 +/- 65.9 nm. Examination of the surface morphology reveals a porous, dendritic surface. Wear testing resulted in two failed condylar coatings out of three tests. No macroscopic delamination was found on any sample, but micron-scale film pieces broke away, exposing the substrate. Electrochemical corrosion testing shows a seven-fold reduction in corrosion rate with the application of an NCD coating as opposed to polished, passivated Ti-6Al-4V, producing a corrosion rate comparable to wrought Co-Cr-Mo. In vivo biocompatibility testing indicates that implanted NCD films did not elicit an immune response in the rabbit model, and osteointegration was apparent for both compact and trabecular bone on both NCD film and bare Ti-6Al-4V. Overall, NCD thin film material is reasonably smooth, biocompatible, and very well adhered. Wear testing indicates that this material is unacceptable for use in demanding TMJ applications without improvements to wear resistance behavior. Identified problems include high surface roughness due to an inadequate seeding procedure and a porous film surface. It is believed that these problems can be solved by future research, in which case NCD thin films should prove to-be well-suited as wear resistant coatings in biomedical applications.

Evaluation of Carbon Anodes for Rechargeable Lithium Cells

NASA Technical Reports Server (NTRS)

Huang, C-K.; Surampudi, S.; Attia, A.; Halpert, G.

1993-01-01

Both liquid phase intercalation technique and electrochemical intercalation technique were examined for the Li-carbon material preparation. The electrochemical techniques include a intermittent discharge method and a two step method. These two electrochemical techniques can ensure to achieve the maximum reversible Li capacity for common commercially available carbon materials. The carbon materials evaluated by the intercalacation method includes: pitch coke, petroleum cole, PAN fiber and graphite materials. Their reversible Li capacity were determined and compared. In this paper, we also demonstrate the importance of EPDM binder composition in the carbon electrode. Our results indicated that it can impact the Li intercalation and de-intercalation capacity in carbon materials. Finally, two possibilities that may help explain the capacity degradation during practical cell cycling were proposed.

Investigation on electrochemical behavior and its catalytic effect on oxygen reduction reaction of 3-Ferrocenyl dihydropyrazole derivative as electron relay

NASA Astrophysics Data System (ADS)

Zeng, Han; Huo, Wen-Shan; Zhao, Shu-Xian; Zhang, Yu-He

2017-11-01

Amino group surface tailored multi-wall carbon nano-tubes were covalently tethered to the gold disk electrode and Laccase molecules were covalently coupled to nano-tubes to prepare Lac-based electrode. Derivative of 3-ferrocenyl dihydropyrazole (FDPFFP) was proposed to be electron mediator for mediated oxygen reduction reaction. Investigation in electro-chemical behavior and catalytic performance to enzymatic reaction of FDPFFP indicated that it displayed quasi-reversible characteristics of electro-chemical reaction with rapid dynamics of electron shuttle and had apparent catalytic effect in oxygen reduction (onset potential for catalysis at 450 mV vs NHE). This enzymatic catalysis was restrained by the step in diffusion of substrate.

Investigation of the Magnetic Properties of Na0.7CoO2 Prepared by Electrochemical Reaction

NASA Astrophysics Data System (ADS)

Sassa, Y.; Umegaki, I.; Nozaki, H.; Forslund, O. K.; Delmas, C.; Orain, J.-C.; Amato, A.; Andreica, D.; Månsson, M.; Sugiyama, J.

We report a muon spin rotation and relaxation (μ+SR) study on Na0.7CoO2 powder samples, where the sodium (Na) has been intercalated via an electrochemical reaction inside a Na-ion battery. The zero field μ+SR measurement at T = 2 K shows a paramagnetic state for the as-grown sample whereas an antiferromagnetic (AF) ordered state is seen for the electrochemically cycled one. Furthermore, the temperature dependence of the muon-spin precession frequencies reveals a Néel transition temperature of TN = 22 K. The results demonstrate the importance of having high-quality homogenous samples, and put the existing NaxCoO2 magnetic phase diagram under debate.

Structural Dynamics and Evolution of Bismuth Electrodes during Electrochemical Reduction of CO 2 in Imidazolium-Based Ionic Liquid Solutions

DOE PAGES

Medina-Ramos, Jonnathan; Lee, Sang Soo; Fister, Timothy T.; ...

2017-09-12

Real-time changes in the composition and structure of bismuth electrodes used for catalytic conversion of CO 2 into CO were examined via X-ray absorption spectroscopy (including XANES and EXAFS), electrochemical quartz crystal microbalance (EQCM) and in situ X-ray reflectivity (XR). Measurements were performed with bismuth electrodes immersed in acetonitrile (MeCN) solutions containing a 1-butyl-3-methylimidazolium ([BMIM] +) ionic liquid promoter or electrochemically inactive tetrabutylammonium supporting electrolytes (TBAPF 6 or TBAOTf). Altogether, these measurements show that bismuth electrodes are originally a mixture of bismuth oxides (including Bi 2O 3) and metallic bismuth (Bi 0), and that the reduction of oxidized bismuth speciesmore » to Bi 0 is fully achieved under potentials at which CO 2 activation takes place. Furthermore, EQCM measurements conducted during cyclic voltammetry revealed that a bismuth-coated quartz crystal exhibits significant shifts in resistance (ΔR) prior to the onset of CO 2 reduction near -1.75 V vs. Ag/AgCl and pronounced hysteresis in frequency (Δf) and ΔR, which suggests significant changes in roughness or viscosity at the Bi/[BMIM] + solution interface. In situ XR performed on rhombohedral Bi (001) oriented films indicates extensive restructuring of the bismuth film cathodes takes place upon polarization to potentials more negative than -1.6 V vs. Ag/AgCl, which is characterized by a decrease of the Bi (001) Bragg peak intensity of ≥50% in [BMIM]OTf solutions in the presence and absence of CO 2. Over 90% of the reflectivity is recovered during the anodic half-scan, suggesting that the structural changes are mostly reversible. By contrast, such a phenomenon is not observed for thin Bi (001) oriented films in solutions of tetrabutylammonium salts that do not promote CO 2 reduction. In conclusion, these results highlight that Bi electrodes undergo significant potential-dependent chemical and structural transformations in the presence of [BMIM] + based electrolytes, including the reduction of bismuth oxide to bismuth metal, changes in roughness and near-surface viscosity.« less

Electron-beam patterned self-assembled monolayers as templates for Cu electrodeposition and lift-off

PubMed Central

She, Zhe; DiFalco, Andrea; Hähner, Georg

2012-01-01

Summary Self-assembled monolayers (SAMs) of 4'-methylbiphenyl-4-thiol (MBP0) adsorbed on polycrystalline gold substrates served as templates to control electrochemical deposition of Cu structures from acidic solution, and enabled the subsequent lift-off of the metal structures by attachment to epoxy glue. By exploiting the negative-resist behaviour of MBP0, the SAM was patterned by means of electron-beam lithography. For high deposition contrast a two-step procedure was employed involving a nucleation phase around −0.7 V versus Cu2+/Cu and a growth phase at around −0.35 V versus Cu2+/Cu. Structures with features down to 100 nm were deposited and transferred with high fidelity. By using substrates with different surface morphologies, AFM measurements revealed that the roughness of the substrate is a crucial factor but not the only one determining the roughness of the copper surface that is exposed after lift-off. PMID:22428101

Electropolishing effect on roughness metrics of ground stainless steel: a length scale study

NASA Astrophysics Data System (ADS)

Nakar, Doron; Harel, David; Hirsch, Baruch

2018-03-01

Electropolishing is a widely-used electrochemical surface finishing process for metals. The electropolishing of stainless steel has vast commercial application, such as improving corrosion resistance, improving cleanness, and brightening. The surface topography characterization is performed using several techniques with different lateral resolutions and length scales, from atomic force microscopy in the nano-scale (<0.1 µm) to stylus and optical profilometry in the micro- and mesoscales (0.1 µm-1 mm). This paper presents an experimental length scale study of the surface texture of ground stainless steel followed by an electropolishing process in the micro and meso lateral scales. Both stylus and optical profilometers are used, and multiple cut-off lengths of the standard Gaussian filter are adopted. While the commonly used roughness amplitude parameters (Ra, Rq and Rz) fail to characterize electropolished textures, the root mean square slope (RΔq) is found to better describe the electropolished surfaces and to be insensitive to scale.

One-pot hydrothermal synthesis, characterization, and electrochemical properties of rGO/MnFe2O4 nanocomposites

NASA Astrophysics Data System (ADS)

Kotutha, Isara; Swatsitang, Ekaphan; Meewassana, Worawat; Maensiri, Santi

2015-06-01

In this work, a simple facile route for preparing an rGO/MnFe2O4 nanocomposite through a one-pot hydrothermal approach was demonstrated. Graphite oxide (GO) was prepared from graphite powder by a modified Hummers method. Fe(NO3)2 • 9H2O and Mn(NO3)2 • H2O were used as the precursors for the preparation of the rGO/MnFe2O4 nanocomposite. The formation of the rGO/MnFe2O4 nanocomposite was confirmed by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), and Rama spectroscopy (Raman). The specific surface area of the prepared composite obtained by Brunauer-Emmett-Teller (BET) analysis was lower than that of pure rGO but higher than that of pure MnFe2O4. Consequently, the electrochemical performance was investigated by using a three-electrode cell system in 6.0 M KOH. The results show that the specific capacitance was determined to be 190.3, 276.9, and 144.5 F/g at a scan rate of 10 mV/s, and 194.9, 274.6, and 134.4 F/g at a current density of 5.0 A/g for rGO, rGO/(5 mmol) MnFe2O4, and rGO/(10 mmol) MnFe2O4, respectively. These results suggest that the composite of MnFe2O4 nanoparticles on an rGO nanosheet can improve the capacitive behavior of the fabricated electrode, but the electrochemical properties are reduced when the MnFe2O4 concentration ratio is high.

Nickel hydroxide nanoparticles-reduced graphene oxide nanosheets film: layer-by-layer electrochemical preparation, characterization and rifampicin sensory application.

PubMed

Rastgar, Shokoufeh; Shahrokhian, Saeed

2014-02-01

Electrochemical deposition, as a well-controlled synthesis procedure, has been used for subsequently layer-by-layer preparation of nickel hydroxide nanoparticle-reduced graphene oxide nanosheets (Ni(OH)2-RGO) on a graphene oxide (GO) film pre-cast on a glassy carbon electrode surface. The surface morphology and nature of the nano-hybrid film (Ni(OH)2-RGO) was thoroughly characterized by scanning electron and atomic force microscopy, spectroscopy and electrochemical techniques. The modified electrode appeared as an effective electro-catalytic model for analysis of rifampicin (RIF) by using linear sweep voltammetry (LSV). The prepared modified electrode exhibited a distinctly higher activity for electro-oxidation of RIF than either GO, RGO nanosheets or Ni(OH)2 nanoparticles. Enhancement of peak currents is ascribed to the fast heterogeneous electron transfer kinetics that arise from the synergistic coupling between the excellent properties of RGO nanosheets (such as high density of edge plane sites, subtle electronic characteristics and attractive π-π interaction) and unique properties of metal nanoparticles. Under the optimized analysis conditions, the modified electrode showed two oxidation processes for rifampicin at potentials about 0.08 V (peak I) and 0.69 V (peak II) in buffer solution of pH 7.0 with a wide linear dynamic range of 0.006-10.0 µmol L(-1) and 0.04-10 µmol L(-1) with a detection limit of 4.16 nmol L(-1) and 2.34 nmol L(-1) considering peaks I and II as an analytical signal, respectively. The results proved the efficacy of the fabricated modified electrode for simple, low cost and highly sensitive medicine sensor well suited for the accurate determinations of trace amounts of rifampicin in the pharmaceutical and clinical preparations. © 2013 Elsevier B.V. All rights reserved.

A simple preparation of graphite/gelatin composite for electrochemical detection of dopamine.

PubMed

Rajkumar, Chellakannu; Thirumalraj, Balamurugan; Chen, Shen-Ming; Chen, His-An

2017-02-01

In this study, we demonstrate a simple preparation of graphite (GR) sheets assisted with gelatin (GLN) polypeptide composite was developed for sensitive detection of dopamine (DA) sensor. The GR/GLN composite was prepared by GR powder in GLN solution (5mg/mL) via sonication process. The prepared GR/GLN composite displays well dispersion ability in biopolymer matrix and characterized via scanning electron microscope (SEM), Fourier transform infrared (FTIR) spectroscopy and electrochemical impedance spectroscopy (EIS) studies. The GR/GLN modified electrode showed an excellent electrocatalytic activity toward the oxidation of DA, suggesting that the successful formation of GR sheets crosslinked with the functional groups of GLN polypeptide. In addition, the GR/GLN modified electrode achieved a wide linear response ranging from 0.05 to 79.5μM with a detection limit of 0.0045μM. The calculated analytical sensitivity of the sensor was 1.36±0.02μAμM -1 cm -2 . Conversely, the modified electrode demonstrates a good storage stability, reproducibility and repeatability. In addition, the sensor manifests the determination of DA in human serum and urine samples for practical applications. Copyright © 2016 Elsevier Inc. All rights reserved.

Mass and charge transport in IPMC actuators with fractal interfaces

NASA Astrophysics Data System (ADS)

Chang, Longfei; Wu, Yucheng; Zhu, Zicai; Li, Heng

2016-04-01

Ionic Polymer-Metal Composite (IPMC) actuators have been attracting a growing interest in extensive applications, which consequently raises the demands on the accuracy of its theoretical modeling. For the last few years, rough landscape of the interface between the electrode and the ionic membrane of IPMC has been well-documented as one of the key elements to ensure a satisfied performance. However, in most of the available work, the interface morphology of IPMC was simplified with structural idealization, which lead to perplexity in the physical interpretation on its interface mechanism. In this paper, the quasi-random rough interface of IPMC was described with fractal dimension and scaling parameters. And the electro-chemical field was modeled by Poisson equation and a properly simplified Nernst-Planck equation set. Then, by simulation with Finite Element Method, a comprehensive analysis on he inner mass and charge transportation in IPMC actuators with different fractal interfaces was provided, which may be further adopted to instruct the performance-oriented interface design for ionic electro-active actuators. The results also verified that rough interface can impact the electrical and mechanical response of IPMC, not only from the respect of the real surface increase, but also from mass distribution difference caused by the complexity of the micro profile.

Real-time electrochemical detection of hydrogen peroxide secretion in live cells by Pt nanoparticles decorated graphene-carbon nanotube hybrid paper electrode.

PubMed

Sun, Yimin; He, Kui; Zhang, Zefen; Zhou, Aijun; Duan, Hongwei

2015-06-15

In this work, we develop a new type of flexible and lightweight electrode based on highly dense Pt nanoparticles decorated free-standing graphene-carbon nanotube (CNT) hybrid paper (Pt/graphene-CNT paper), and explore its practical application as flexible electrochemical biosensor for the real-time tracking hydrogen peroxide (H2O2) secretion by live cells. For the fabrication of flexible nanohybrid electrode, the incorporation of CNT in graphene paper not only improves the electrical conductivity and the mechanical strength of graphene paper, but also increases its surface roughness and provides more nucleation sites for metal nanoparticles. Ultrafine Pt nanoparticles are further decorated on graphene-CNT paper by well controlled sputter deposition method, which offers several advantages such as defined particle size and dispersion, high loading density and strong adhesion between the nanoparticles and the substrate. Consequently, the resultant flexible Pt/graphene-CNT paper electrode demonstrates a variety of desirable electrochemical properties including large electrochemical active surface area, excellent electrocatalytic activity, high stability and exceptional flexibility. When used for nonenzymatic detection of H2O2, Pt/graphene-CNT paper exhibits outstanding sensing performance such as high sensitivity, selectivity, stability and reproducibility. The sensitivity is 1.41 µA µM(-1) cm(-2) with a linear range up to 25 µM and a low detection limit of 10 nM (S/N=3), which enables the resultant biosensor for the real-time tracking H2O2 secretion by live cells macrophages. Copyright © 2015. Published by Elsevier B.V.

Development of binary and ternary titanium alloys for dental implants.

PubMed

Cordeiro, Jairo M; Beline, Thamara; Ribeiro, Ana Lúcia R; Rangel, Elidiane C; da Cruz, Nilson C; Landers, Richard; Faverani, Leonardo P; Vaz, Luís Geraldo; Fais, Laiza M G; Vicente, Fabio B; Grandini, Carlos R; Mathew, Mathew T; Sukotjo, Cortino; Barão, Valentim A R

2017-11-01

The aim of this study was to develop binary and ternary titanium (Ti) alloys containing zirconium (Zr) and niobium (Nb) and to characterize them in terms of microstructural, mechanical, chemical, electrochemical, and biological properties. The experimental alloys - (in wt%) Ti-5Zr, Ti-10Zr, Ti-35Nb-5Zr, and Ti-35Nb-10Zr - were fabricated from pure metals. Commercially pure titanium (cpTi) and Ti-6Al-4V were used as controls. Microstructural analysis was performed by means of X-ray diffraction and scanning electron microscopy. Vickers microhardness, elastic modulus, dispersive energy spectroscopy, X-ray excited photoelectron spectroscopy, atomic force microscopy, surface roughness, and surface free energy were evaluated. The electrochemical behavior analysis was conducted in a body fluid solution (pH 7.4). The albumin adsorption was measured by the bicinchoninic acid method. Data were evaluated through one-way ANOVA and the Tukey test (α=0.05). The alloying elements proved to modify the alloy microstructure and to enhance the mechanical properties, improving the hardness and decreasing the elastic modulus of the binary and ternary alloys, respectively. Ti-Zr alloys displayed greater electrochemical stability relative to that of controls, presenting higher polarization resistance and lower capacitance. The experimental alloys were not detrimental to albumin adsorption. The experimental alloys are suitable options for dental implant manufacturing, particularly the binary system, which showed a better combination of mechanical and electrochemical properties without the presence of toxic elements. Copyright © 2017 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Cellular Behavior of Human Adipose-Derived Stem Cells on Wettable Gradient Polyethylene Surfaces

PubMed Central

Ahn, Hyun Hee; Lee, Il Woo; Lee, Hai Bang; Kim, Moon Suk

2014-01-01

Appropriate surface wettability and roughness of biomaterials is an important factor in cell attachment and proliferation. In this study, we investigated the correlation between surface wettability and roughness, and biological response in human adipose-derived stem cells (hADSCs). We prepared wettable and rough gradient polyethylene (PE) surfaces by increasing the power of a radio frequency corona discharge apparatus with knife-type electrodes over a moving sample bed. The PE changed gradually from hydrophobic and smooth surfaces to hydrophilic (water contact angle, 90º to ~50º) and rough (80 to ~120 nm) surfaces as the power increased. We found that hADSCs adhered better to highly hydrophilic and rough surfaces and showed broadly stretched morphology compared with that on hydrophobic and smooth surfaces. The proliferation of hADSCs on hydrophilic and rough surfaces was also higher than that on hydrophobic and smooth surfaces. Furthermore, integrin beta 1 gene expression, an indicator of attachment, and heat shock protein 70 gene expression were high on hydrophobic and smooth surfaces. These results indicate that the cellular behavior of hADSCs on gradient surface depends on surface properties, wettability and roughness. PMID:24477265

Synthesis and characterization of MoS2/Ti composite coatings on Ti6Al4V prepared by laser cladding

NASA Astrophysics Data System (ADS)

Yang, Rongjuan; Liu, Zongde; Wang, Yongtian; Yang, Guang; Li, Hongchuan

2013-02-01

The MoS2/Ti composite coating with sub-micron grade structure has been prepared on Ti6Al4V by laser method under argon protection. The morphology, microstructure, microhardness and friction coefficient of the coating were examined. The results indicated that the molybdenum disulfide was decomposed during melting and resolidification. The phase organization of composite coating mainly consisted of ternary element sulfides, molybdenum sulfides and titanium sulfides. The friction coefficient of and the surface roughness the MoS2/Ti coating were lower than those of Ti6Al4V. The composite coating exhibits excellent adhesion to the substrates, less surface roughness, good wear resistance and harder surface.

Novel electrochemical redox-active species: one-step synthesis of polyaniline derivative-Au/Pd and its application for multiplexed immunoassay

NASA Astrophysics Data System (ADS)

Wang, Liyuan; Feng, Feng; Ma, Zhanfang

2015-11-01

Electrochemical redox-active species play crucial role in electrochemically multiplexed immunoassays. A one-pot method for synthesizing four kinds of new electrochemical redox-active species was reported using HAuCl4 and Na2PdCl4 as dual oxidating agents and aniline derivatives as monomers. The synthesized polyaniline derivative-Au/Pd composites, namely poly(N-methyl-o-benzenediamine)-Au/Pd, poly(N-phenyl-o-phenylenediamine)-Au/Pd, poly(N-phenyl-p-phenylenediamine)-Au/Pd and poly(3,3’,5,5’-tetramethylbenzidine)-Au/Pd, exhibited electrochemical redox activity at -0.65 V, -0.3 V, 0.12 V, and 0.5 V, respectively. Meanwhile, these composites showed high H2O2 electrocatalytic activity because of the presence of Au/Pd. The as-prepared composites were used as electrochemical immunoprobes in simultaneous detection of four tumor biomarkers (carcinoembryonic antigen (CEA), carbohydrate antigen 19-9 (CA199), carbohydrate antigen 72-4 (CA724), and alpha fetoprotein (AFP)). This immunoassay shed light on potential applications in simultaneous gastric cancer (related biomarkers: CEA, CA199, CA724) and liver cancer diagnosis (related biomarkers: CEA, CA199, AFP). The present strategy to the synthesize redox species could be easily extended to other polymers such as polypyrrole derivatives and polythiophene derivatives. This would be of great significance in the electrochemical detection of more analytes.

Freestanding NiFe Oxyfluoride Holey Film with Ultrahigh Volumetric Capacitance for Flexible Asymmetric Supercapacitors.

PubMed

Liang, Kun; Marcus, Kyle; Yang, Zhenzhong; Zhou, Le; Pan, Hao; Bai, Yuanli; Du, Yingge; Engelhard, Mark H; Yang, Yang

2018-01-01

In this work, a freestanding NiFe oxyfluoride (NiFeOF) holey film is prepared by electrochemical deposition and anodic treatments. With the combination of good electrical conductivity and holey structure, the NiFeOF holey film offers superior electrochemical performance with maximum specific capacitance of 670 F cm -3 (134 mF cm -2 ), due to the following reasons: (i) The residual metal alloy framework can be used as the current collector to improve electrode conductivity. Moreover, the as-prepared freestanding NiFeOF holey film can be used as a supercapacitor electrode without reliance on binders and other additives. The residual metal alloy framework and binder-free electrode effectively reduce electrode resistance, thus improving electron transport. (ii) The highly interconnected holey structure and hierarchical pore distribution provide a high specific surface area to improve electron transport, enhancing rapid ion transport, and mitigating diffusion limitations throughout the holey film. (iii) The excellent mechanical characteristics facilitate flexibility and cyclability related performance. Additionally, the NiFeOF holey film presents exceptional electrochemical performance, showing that it is a promising alternative for small/microsize electronic devices. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparation, characterization, and application of Ti/TiO2-NTs/Sb-SnO2 electrode in photo-electrochemical treatment of industrial effluents under mild conditions.

PubMed

Subba Rao, Anantha N; Venkatarangaiah, Venkatesha T

2018-04-01

Ti/TiO 2 -NTs/Sb-SnO 2 electrode was prepared by gradient pulsed electrodeposition, and its electrochemical properties were evaluated. The catalytic activity and reusability of the electrode were tested by electrochemical oxidation (EO) and photoelectrochemical oxidation (PEO) of organics present in textile industry wastewater (TWW) and coffee bean processing industry wastewater (CWW). COD removal of ~ 41% was achieved after 5-h electrolysis under a constant applied current density of 30 mA cm -2 for TWW and 50 mA cm -2 for CWW. Nearly 14 and 18% increment in COD removal was observed under PEO for TWW and CWW, respectively. The turbidity of TWW reduced from 15 to ~ 3 NTU and the turbidity of CWW reduced from 27 to ~ 3 NTU by both EO and PEO. The % COD removal observed after 5-h electrolysis remained consistent for 7 repeated cycles; however, the catalytic activity of the electrode reduced gradually. These results suggested that the Ti/TiO 2 -NTs/Sb-SnO 2 can be a potential electrode for the treatment of industrial wastewater.

Electrochemical preparation of nickel and copper oxides-decorated graphene composite for simultaneous determination of dopamine, acetaminophen and tryptophan.

PubMed

Liu, Bingdi; Ouyang, Xiaoqian; Ding, Yaping; Luo, Liqing; Xu, Duo; Ning, Yanqun

2016-01-01

In the present work, transition metal oxides decorated graphene (GR) have been fabricated for simultaneous determination of dopamine (DA), acetaminophen (AC) and tryptophan (Trp) using square wave voltammetry. Electro-deposition is a facile preparation strategy for the synthesis of nickel oxide (NiO) and copper oxide (CuO) nanoparticles. GR can be modified by using citric acid to produce more functional groups, which is conducive to the deposition of dispersed metal particles. The morphologies and interface properties of the obtained NiO-CuO/GR nanocomposite were examined by scanning electron microscopy, energy dispersive X-ray spectroscopy and Raman spectroscopy. Moreover, the electrochemical performances of the composite film were investigated by cyclic voltammetry and electrochemical impedance spectroscopy. The modified electrode exhibited that the linear response ranges for detecting DA, AC and Trp were 0.5-20 μM, 4-400 μM and 0.3-40 μM, respectively, and the detection limits were 0.17 μM, 1.33 μM and 0.1 μM (S/N=3). Under optimal conditions, the sensor displayed high sensitivity, excellent stability and satisfactory results in real samples analysis. Copyright © 2015 Elsevier B.V. All rights reserved.

Li+ /Mg2+ Hybrid-Ion Batteries with Long Cycle Life and High Rate Capability Employing MoS2 Nano Flowers as the Cathode Material.

PubMed

Ju, Yanming; Meng, Yuan; Wei, Yingjin; Bian, Xiaofei; Pang, Qiang; Gao, Yu; Du, Fei; Liu, Bingbing; Chen, Gang

2016-12-12

The demand for large-scale and safe energy storage is increasing rapidly due to the strong push for smartphones and electric vehicles. As a result, Li + /Mg 2+ hybrid-ion batteries (LMIBs) combining a dendrite-free deposition of Mg anode and Li + intercalation cathode have attracted considerable attention. Here, a LMIB with hydrothermal-prepared MoS 2 nano flowers as cathode material was prepared. The battery showed remarkable electrochemical properties with a large discharge capacity (243 mAh g -1 at the 0.1 C rate), excellent rate capability (108 mAh g -1 at the 5 C rate), and long cycle life (87.2 % capacity retention after 2300 cycles). Electrochemical analysis showed that the reactions occurring in the battery cell involved Mg stripping/plating at the anode side and Li + intercalation at the cathode side with a small contribution from Mg 2+ adsorption. The excellent electrochemical performance and extremely safe cell system show promise for its use in practical applications. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

An alternative to hydrogenation processes. Electrocatalytic hydrogenation of benzophenone.

PubMed

Mozo Mulero, Cristina; Sáez, Alfonso; Iniesta, Jesús; Montiel, Vicente

2018-01-01

The electrocatalytic hydrogenation of benzophenone was performed at room temperature and atmospheric pressure using a polymer electrolyte membrane electrochemical reactor (PEMER). Palladium (Pd) nanoparticles were synthesised and supported on a carbonaceous matrix (Pd/C) with a 28 wt % of Pd with respect to carbon material. Pd/C was characterised by transmission electron microscopy (TEM), and thermogravimetric analysis (TGA). Cathodes were prepared using Pd electrocatalytic loadings (L Pd ) of 0.2 and 0.02 mg cm -2 . The anode consisted of hydrogen gas diffusion for the electrooxidation of hydrogen gas, and a 117 Nafion exchange membrane acted as a cationic polymer electrolyte membrane. Benzophenone solution was electrochemically hydrogenated in EtOH/water (90/10 v/v) plus 0.1 M H 2 SO 4 . Current densities of 10, 15 and 20 mA cm -2 were analysed for the preparative electrochemical hydrogenation of benzophenone and such results led to the highest fractional conversion (X R ) of around 30% and a selectivity over 90% for the synthesis of diphenylmethanol upon the lowest current density. With regards to an increase by ten times the Pd electrocatalytic loading the electrocatalytic hydrogenation led neither to an increase in fractional conversion nor to a change in selectivity.

An alternative to hydrogenation processes. Electrocatalytic hydrogenation of benzophenone

PubMed Central

Mozo Mulero, Cristina; Iniesta, Jesús; Montiel, Vicente

2018-01-01

The electrocatalytic hydrogenation of benzophenone was performed at room temperature and atmospheric pressure using a polymer electrolyte membrane electrochemical reactor (PEMER). Palladium (Pd) nanoparticles were synthesised and supported on a carbonaceous matrix (Pd/C) with a 28 wt % of Pd with respect to carbon material. Pd/C was characterised by transmission electron microscopy (TEM), and thermogravimetric analysis (TGA). Cathodes were prepared using Pd electrocatalytic loadings (LPd) of 0.2 and 0.02 mg cm−2. The anode consisted of hydrogen gas diffusion for the electrooxidation of hydrogen gas, and a 117 Nafion exchange membrane acted as a cationic polymer electrolyte membrane. Benzophenone solution was electrochemically hydrogenated in EtOH/water (90/10 v/v) plus 0.1 M H2SO4. Current densities of 10, 15 and 20 mA cm−2 were analysed for the preparative electrochemical hydrogenation of benzophenone and such results led to the highest fractional conversion (XR) of around 30% and a selectivity over 90% for the synthesis of diphenylmethanol upon the lowest current density. With regards to an increase by ten times the Pd electrocatalytic loading the electrocatalytic hydrogenation led neither to an increase in fractional conversion nor to a change in selectivity. PMID:29623115

Synthesis of netlike gold nanoparticles using ampicillin as a stabilizing reagent and its application

DOE Office of Scientific and Technical Information (OSTI.GOV)

Song, Y.Z., E-mail: singyuanzhi@sina.com; Zhou, J.F.; Song, Y., E-mail: songyang@mail.buct.edu.cn

Graphical abstract: Electrochemical deposition of netlike gold nanoparticles (GNPs) on the surface of glassy carbon electrode and preparation of netlike GNPs in aqueous solution using ampicillin as a stabilizing reagent were proposed. The catalytic properties of netlike gold nanoparticles on the glassy carbon electrode for dopamine were demonstrated. The results indicate that the netlike gold nanoparticle modified electrode has an excellent repeatability and reproducibility. Display Omitted Highlights: ► Synthesis of netlike gold nanoparticles using ampicillin as a stabilizing reagent. ► Excellent repeatability and reproducibility of netlike gold nanoparticle modified glassy carbon electrode. ► The catalytic properties of netlike gold nanoparticlemore » for dopamine. -- Abstract: Electrochemical deposition of netlike gold nanoparticles on the surface of glassy carbon electrode and preparation of netlike GNPs in aqueous solution using ampicillin as a stabilizing reagent were proposed. The netlike gold nanoparticles were characterized by scanning electron microscope, transmission electron microscope, infrared spectrometer, UV spectrophotometer, powder X-ray diffractometer and electrochemical analyzer. The catalysis of the netlike gold nanoparticles on the glassy carbon electrode for dopamine was demonstrated. The results indicate that the gold nanoparticle modified electrode has an excellent repeatability and reproducibility.« less

Preparation of NiCoP Hollow Quasi-Polyhedra and Their Electrocatalytic Properties for Hydrogen Evolution in Alkaline Solution.

PubMed

Li, Yapeng; Liu, Jindou; Chen, Chen; Zhang, Xiaohua; Chen, Jinhua

2017-02-22

Double metal phosphide (NiCoP) with hollow quasi-polyhedron structure was prepared by acidic etching and precipitation of ZIF-67 polyhedra and further phosphorization treatment with NaH 2 PO 2 . The morphology and microstructure of NiCoP quasi-polyhedron and its precursors were investigated by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and a micropore and chemisorption analyzer. Electrocatalytic properties were examined by typical electrochemical methods, such as linear sweep voltammetry, cyclic voltammetry, chronoamperometry, and electrochemical impedance spectroscopy in 1.0 M KOH aqueous solution. Results reveal that, compared with CoP hollow polyhedra, NiCoP hollow quasi-polyhedra exhibit better electrochemical properties for hydrogen evolution with a low onset overpotential of 74 mV and a small Tafel slope of 42 mV dec -1 . When the current density is 10 mA cm -2 , the corresponding overpotential is merely 124 mV, and 93% of its electrocatalytic activity can be maintained for 12 h. This indicates that NiCoP with hollow quasi-polyhedron structure, bimetallic merit, and low cost may be a good candidate as electrocatalyst in the practical application of hydrogen evolution.

Time resolved impedance spectroscopy analysis of lithium phosphorous oxynitride - LiPON layers under mechanical stress

NASA Astrophysics Data System (ADS)

Glenneberg, Jens; Bardenhagen, Ingo; Langer, Frederieke; Busse, Matthias; Kun, Robert

2017-08-01

In this paper we present investigations on the morphological and electrochemical changes of lithium phosphorous oxynitride (LiPON) under mechanically bent conditions. Therefore, two types of electrochemical cells with LiPON thin films were prepared by physical vapor deposition. First, symmetrical cells with two blocking electrodes (Cu/LiPON/Cu) were fabricated. Second, to simulate a more application-related scenario cells with one blocking and one non-blocking electrode (Cu/LiPON/Li/Cu) were analyzed. In order to investigate mechanical distortion induced transport property changes in LiPON layers the cells were deposited on a flexible polyimide substrate. Morphology of the as-prepared samples and deviations from the initial state after applying external stress by bending the cells over different radii were investigated by Focused Ion Beam- Scanning Electron Microscopy (FIB-SEM) cross-section and surface images. Mechanical stress induced changes in the impedance were evaluated by time-resolved electrochemical impedance spectroscopy (EIS). Due to the formation of a stable, ion-conducting solid electrolyte interphase (SEI), cells with lithium show decreased impedance values. Furthermore, applying mechanical stress to the cells results in a further reduction of the electrolyte resistance. These results are supported by finite element analysis (FEA) simulations.

Electrochemical preparation of nanostructured lanthanum using lanthanum chloride as a precursor in 1-butyl-3-methylimidazolium dicyanamide ionic liquid.

PubMed

Zhang, Q B; Yang, C; Hua, Y X; Li, Y; Dong, P

2015-02-14

Nanostructured lanthanum was electrochemically prepared on a platinum (Pt) substrate in the room temperature ionic liquid 1-butyl-3-methylimidazolium dicyanamide (BMI-DCA) containing anhydrous LaCl3 at 333 K. The electrochemical reduction behavior of La(iii) was investigated using cyclic voltammetry and chronoamperometry techniques. Cyclic voltammogram revealed that the reduction of La(iii) in BMI-DCA involved an irreversible process controlled by diffusion. Chronoamperometric transient analysis confirmed the diffusion controlled electrodeposition process with the diffusion coefficient of La(iii) species in the range of 10(-10) cm(2) s(-1). The strong complexing capability of DCA(-) anions facilitated the displacement of chloride ligands and induced the solubility of LaCl3. The subsequent coordination of La(iii) and DCA(-) anions forming [La(DCA)4](-) complex anions was monitored by designing amperometric titration experiments. Potentiostatically deposited La-deposits with different nanostructures were characterized by SEM, XRD and XPS analyses. The electrodeposition potential was found to play an important role in controlling the nucleation and growth kinetics of the nanocrystal during the electrodeposition process. Depending on the deposition potential, metallic lanthanum with either nanoparticles or nanoporous structures was obtained.

High performance supercapacitor from activated carbon derived from waste orange skin

NASA Astrophysics Data System (ADS)

Ahmed, Sultan; Hussain, S.; Ahmed, Ahsan; Rafat, M.

2018-05-01

Activated carbon due to its inherent properties such as large surface area and low cost is most frequently used electrode material for supercapacitor. Activated carbon has been previously derived from various biomass such as coconut shell, coffee bean etc. Herein, we report the synthesis of activated carbon from waste orange skin. The material was synthesized employing chemical activation method and the success of synthesis was confirmed by its physical and electrochemical properties. The physical properties of the as-prepared sample were studied using the techniques of XRD, SEM, Raman spectroscopy and N2 adsorption/desorption analysis while its electrochemical properties were studied in two-electrode assembly using liquid electrolyte (consisting of 1 M solution of LiTFSI dispersed in ionic liquid EMITFSI) and employing the techniques of cyclic voltammetry, electrochemical impedance spectroscopy and galvanostatic charge- discharge. The synthesized sample of activated carbon exhibits high specific capacitance of 115 F g-1 at 10 mV s-1. Also, the activated carbon electrode shows the retention of ˜75% in initial capacitance value for more than 2000 initial cycles, indicating the as-prepared activated carbon can be profitably used as electrode material for energy storage devices.

"Sign-on/off" sensing interface design and fabrication for propyl gallate recognition and sensitive detection.

PubMed

Dai, Yunlong; Li, Xueyan; Fan, Limei; Lu, Xiaojing; Kan, Xianwen

2016-12-15

A new strategy based on sign-on and sign-off was proposed for propyl gallate (PG) determination by an electrochemical sensor. The successively modified poly(thionine) (PTH) and molecular imprinted polymer (MIP) showed an obvious electrocatalysis and a good recognition toward PG, respectively. Furthermore, the rebound PG molecules in imprinted cavities not only were oxidized but also blocked the electron transmission channels for PTH redox. Thus, a sign-on from PG current and a sign-off from PTH current were combined as a dual-sign for PG detection. Meanwhile, the modified MIP endowed the sensor with recognition capacity. The electrochemical experimental results demonstrated that the prepared sensor possessed good selectivity and high sensitivity. A linear ranging from 5.0×10(-8) to 1.0×10(-4)mol/L for PG detection was obtained with a limit of detection of 2.4×10(-8)mol/L. And the sensor has been applied to analyze PG in real samples with satisfactory results. The simple, low cost, and effective strategy reported here can be further used to prepare electrochemical sensors for other compounds selective recognition and sensitive detection. Copyright © 2016 Elsevier B.V. All rights reserved.

Effect of solvents on the electrochemical properties of binder-free sulfur cathode films in lithium–sulfur batteries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ryu, Ho-Suk; Kim, Byeong-Wook; Park, Jin-Woo

Highlights: • The binder-free sulfur electrode with high sulfur contents of 75 wt.% was fabricated. • The binder-free sulfur electrode using NMP solvents showed 784 mAh g{sup −1} after 40 cycles. • The solvent affect the electrochemical properties of binder-free sulfur electrode films. - Abstract: The effects of solvents on the preparation of sulfur cathodes were investigated by fabricating binder-free sulfur electrode films using three different solvents: 1-methyl-2-pyrrolidinone (NMP), acetonitrile, and deionized water. These solvents are commonly employed to dissolve binders used to prepare sulfur cathodes for lithium–sulfur batteries. The sulfur electrode fabricated with NMP had a higher discharge capacitymore » and longer cycle life than the ones fabricated with acetonitrile and deionized water. Better adhesion between the current collector and the sulfur electrode accounted for the improved capacity and cycle life of the battery. In addition, the stability of the electrode in the electrolyte was a result of the solubility of sulfur in the solvent. We thus concluded that the solvents used in the fabrication of sulfur electrodes had a positive influence on the electrochemical properties of Li–S batteries.« less

Hierarchical Mesoporous Lithium-Rich Li[Li0.2Ni0.2Mn0.6]O2 Cathode Material Synthesized via Ice Templating for Lithium-Ion Battery.

PubMed

Li, Yu; Wu, Chuan; Bai, Ying; Liu, Lu; Wang, Hui; Wu, Feng; Zhang, Na; Zou, Yufeng

2016-07-27

Tuning hierarchical micro/nanostructure of electrode materials is a sought-after means to reinforce their electrochemical performance in the energy storage field. Herein, we introduce a type of hierarchical mesoporous Li[Li0.2Ni0.2Mn0.6]O2 microsphere composed of nanoparticles synthesized via an ice templating combined coprecipitation strategy. It is a low-cost, eco-friendly, and easily operated method using ice as a template to control material with homogeneous morphology and rich porous channels. The as-prepared material exhibits remarkably enhanced electrochemical performances with higher capacity, more excellent cycling stability and more superior rate property, compared with the sample prepared by conventional coprecipitation method. It has satisfactory initial discharge capacities of 280.1 mAh g(-1) at 0.1 C, 207.1 mAh g(-1) at 2 C, and 152.4 mAh g(-1) at 5 C, as well as good cycle performance. The enhanced electrochemical performance can be ascribed to the stable hierarchical microsized structure and the improved lithium-ion diffusion kinetics from the highly porous structure.

Fast Preparation of Porous MnO/C Microspheres as Anode Materials for Lithium-Ion Batteries

PubMed Central

Su, Jing; Liang, Hao; Gong, Xian-Nian; Lv, Xiao-Yan; Long, Yun-Fei; Wen, Yan-Xuan

2017-01-01

Porous MnO/C microspheres have been successfully fabricated by a fast co-precipitation method in a T-shaped microchannel reactor. The structures, compositions, and electrochemical performances of the obtained MnO/C microspheres are characterized by X-ray diffraction, field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (HRTEM), Brunauer–Emmett–Teller analysis, charge-discharge testing, cyclic voltammograms, and electrochemical impedance spectra. Experimental results reveal that the as-prepared MnO/C, with a specific surface area of 96.66 m2·g−1 and average pore size of 24.37 nm, exhibits excellent electrochemical performance, with a discharge capacity of 655.4 mAh·g−1 after cycling 50 times at 1 C and capacities of 808.3, 743.7, 642.6, 450.1, and 803.1 mAh·g−1 at 0.2, 0.5, 1, 2, and 0.2 C, respectively. Moreover, the controlled method of using a microchannel reactor, which can produce larger specific surface area porous MnO/C with improved cycling performance by shortening lithium-ion diffusion distances, can be easily applied in real production on a large scale. PMID:28587120

Semi-conducting single-walled carbon nanotubes are detrimental when compared to metallic single-walled carbon nanotubes for electrochemical applications.

PubMed

Dong, Qi; Nasir, Muhammad Zafir Mohamad; Pumera, Martin

2017-10-18

As-synthetized single walled carbon nanotubes (SWCNTs) contain both metallic and semiconducting nanotubes. For the electronics, it is desirable to separate semiconducting SWCNTs (s-SWCNTs) from the metallic ones as s-SWCNTs provide desirable electronic properties. Here we test whether ultrapure semi-conducting single-walled carbon nanotubes (s-SWCNTs) provide advantageous electrochemical properties over the as prepared SWCNTs which contain a mixture of semiconducting and metallic CNTs. We test them as a transducer platform which enhanced the detection of target analytes (ascorbic acid, dopamine, uric acid) when compared to a bare glassy carbon (GC) electrode. Despite that, the two materials exhibit significantly different electrochemical properties and performances. A mixture of m-SWCNTs and s-SWCNTs demonstrated superior performance over ultrapure s-SWCNTs with greater peak currents and pronounced shift in peak potentials to lower values in cyclic and differential pulse voltammetry for the detection of target analytes. The mixture of m- and s-SWCNTs displayed about a 4 times improved heterogeneous electron transfer rate as compared to bare GC and a 2 times greater heterogeneous electron transfer rate than s-SWCNTs, demonstrating that ultrapure SWCNTs do not provide any major enhancement over the as prepared SWCNTs.

A Facile Electrochemical Preparation of Reduced Graphene Oxide@Polydopamine Composite: A Novel Electrochemical Sensing Platform for Amperometric Detection of Chlorpromazine

PubMed Central

Palanisamy, Selvakumar; Thirumalraj, Balamurugan; Chen, Shen-Ming; Wang, Yi-Ting; Velusamy, Vijayalakshmi; Ramaraj, Sayee Kannan

2016-01-01

We report a novel and sensitive amperometric sensor for chlorpromazine (CPZ) based on reduced graphene oxide (RGO) and polydopamine (PDA) composite modified glassy carbon electrode. The RGO@PDA composite was prepared by electrochemical reduction of graphene oxide (GO) with PDA. The RGO@PDA composite modified electrode shows an excellent electro-oxidation behavior to CPZ when compared with other modified electrodes such as GO, RGO and GO@PDA. Amperometric i-t method was used for the determination of CPZ. Amperometry result shows that the RGO@PDA composite detects CPZ in a linear range from 0.03 to 967.6 μM. The sensor exhibits a low detection limit of 0.0018 μM with the analytical sensitivity of 3.63 ± 0.3 μAμM–1 cm–2. The RGO@PDA composite shows its high selectivity towards CPZ in the presence of potentially interfering drugs such as metronidazole, phenobarbital, chlorpheniramine maleate, pyridoxine and riboflavin. In addition, the fabricated RGO@PDA modified electrode showed an appropriate recovery towards CPZ in the pharmaceutical tablets. PMID:27650697

[Silicate coating of cemented titanium-based shafts in hip prosthetics reduces high aseptic loosening].

PubMed

Marx, R; Faramarzi, R; Jungwirth, F; Kleffner, B V; Mumme, T; Weber, M; Wirtz, D C

2009-01-01

For cemented hip prostheses, all requirements can be fulfilled by using forged Co/Cr/Mo stems. Co/Cr/Mo alloys, however, are contraindicated for allergy sufferers. For these patients, a cemented prosthesis made of titanium (alloy) would be indicated. Cemented stems from titanium (alloy), depending on the geometry of the prosthesis and its specific surface texture, however, may have loosening rates which are clinically not tolerable. In comparison to Co/Cr/Mo alloys, the greater roughness in conjunction with lesser abrasion resistance of titanium-based alloys leads to high loosening rates caused by abrasion. On the other hand, the greater surface roughness permits good mechanical retention of bone cement to the surface. Good mechanical retention enhances migration behaviour and reduces micromotions. However, there is no stable hydrolytic bond between bone cement and metallic surface; intermediate-term debonding between metal and bone cement is predictable. This debonding results in relative movements, consequently in wear particles which have their origin both from the rough metallic surface and from the PMMA cement. The roughness of the metallic surface operates as emery and with that, a rubbing wear from the PMMA. For the above reasons, a low or moderate roughness is essential for easily abradable implants such as shafts made of titanium (alloy) because low roughness provides a fail-safe running function in case of debonding. Thus, one must allow for inappropriate migration behaviour accompanied by greater micromotions due to insufficient mechanical retention in the case of low roughness. This can be accomplished by a silicate layer coating applied to the metal shaft surface via electrochemical "ECD" or physical vapour deposition "PVD". For analysis, specimens (screws for pull-out, cones for push-out tests) were sand-blasted, so that roughnesses between Ra = 0.8 microm (Rz = 4 microm) and Ra = 2.0 microm (Rz = 9 microm) were generated. The bond strengths observed in tensile tests for roughnesses of Ra = 1.7 mm were always well above 25 MPa for all periods of hydrolytic load. Therefore, the investigation shows that surfaces of moderate roughness (Ra = 1.7 microm), however coated, provide a steady retention. Cave-in and micromotions should widely be prevented. The abrasion, which is a consequence of and reason for debonding and loosening at the same time, should be avoidable if the bonding of cement on the metallic shaft is stabilised with the help of a suitable chemical bond system.

Poly(arylene)-based anion exchange polymer electrolytes

DOEpatents

Kim, Yu Seung; Bae, Chulsung

2015-06-09

Poly(arylene) electrolytes including copolymers lacking ether groups in the polymer may be used as membranes and binders for electrocatalysts in preparation of anodes for electrochemical cells such as solid alkaline fuel cells.

Voltammetric Determination of Ferulic Acid Using Polypyrrole-Multiwalled Carbon Nanotubes Modified Electrode with Sample Application

PubMed Central

Abdel-Hamid, Refat; Newair, Emad F.

2015-01-01

A polypyrrole-multiwalled carbon nanotubes modified glassy carbon electrode-based sensor was devised for determination of ferulic acid (FA). The fabricated sensor was prepared electrochemically using cyclic voltammetry (CV) and characterized using CV and scanning electron microscope (SEM). The electrode shows an excellent electrochemical catalytic activity towards FA oxidation. Under optimal conditions, the anodic peak current correlates linearly to the FA concentration throughout the range of 3.32 × 10−6 to 2.59 × 10−5 M with a detection limit of 1.17 × 10−6 M (S/N = 3). The prepared sensor is highly selective towards ferulic acid without the interference of ascorbic acid. The sensor applicability was tested for total content determination of FA in a commercial popcorn sample and showed a robust functionality. PMID:28347090

Nanosheet-assembled NiO microstructures for high-performance supercapacitors.

PubMed

Purushothaman, Kamatchi Kamaraj; Babu, Inbamani Manohara; Sethuraman, Balasubramanian; Muralidharan, Gopalan

2013-11-13

Nanosheet-assembled NiO microstructures have been synthesized via a hydrothermal method. The presence of anionic surfactant in the fabrication process initiates the formation of lamellar micelles and a self-assembling process. This leads to the formation of NiO nanosheets and organizes it into microstructures. The effect of preparation temperature on the morphological, structural, and electrochemical properties and stability upon continuous charge/discharge cycles has been examined for supercapacitor applications. Electrochemical analysis demonstrated that NiO nanosheets prepared at 160 °C are capable of delivering a specific capacitance of 989 F g(-1) at a scan rate of 3 mV s(-1) for the potential window of 0-0.6 V. The nanosheets exhibit excellent capacity retention, 97% retention after 1000 continuous charge/discharge cycles, and an energy density of 49.45 W h kg(-1).

Vertically aligned single-walled carbon nanotubes by chemical assembly--methodology, properties, and applications.

PubMed

Diao, Peng; Liu, Zhongfan

2010-04-06

Single-walled carbon nanotubes (SWNTs), as one of the most promising one-dimension nanomaterials due to its unique structure, peculiar chemical, mechanical, thermal, and electronic properties, have long been considered as an important building block to construct ordered alignments. Vertically aligned SWNTs (v-SWNTs) have been successfully prepared by using direct growth and chemical assembly strategies. In this review, we focus explicitly on the v-SWNTs fabricated via chemical assembly strategy. We provide the readers with a full and systematic summary covering the advances in all aspects of this area, including various approaches for the preparation of v-SWNTs using chemical assembly techniques, characterization, assembly kinetics, and electrochemical properties of v-SWNTs. We also review the applications of v-SWNTs in electrochemical and bioelectrochemical sensors, photoelectric conversion, and scanning probe microscopy.

Structural and optical properties of nanostructured CdSe thin films prepared by electrochemical deposition

NASA Astrophysics Data System (ADS)

Bai, Rekha; Chaudhary, Sujeet; Pandya, Dinesh K.

2018-05-01

Cadmium selenide (CdSe) nanostructured thin films have been grown on fluorine doped tin oxide (FTO) coated glass substrates by potentiostatic electrochemical deposition (ECD) technique for use in solar energy conversion devices. The effect of bath temperature on the structural, morphological and optical properties of prepared CdSe films has been explored. X-ray diffraction (XRD) and Raman spectroscopy clearly show that the CdSe films are polycrystalline and exhibit phase transformation from wurtzite to zincblende structure with increase in bath temperature. Optical spectra reveal that the nanostructured CdSe films have high absorbance in visible region and the films show a red shift in direct optical energy band gap from 1.90 to 1.65 eV with increase in bath temperature due to change in phase and bandgap tuning related to quantum confinement effect.

Potassium chloride templated carbon preparation for supercapacitor

NASA Astrophysics Data System (ADS)

Cao, Yuhe; Wang, Xiaomin; Gu, Zhengrong; Fan, Qihua; Gibbons, William; Gadhamshetty, Venkataramana; Ai, Ning; Zeng, Ganning

2018-04-01

This is the first report of KCl templated carbon preparation from walnut shell. Activated carbon (AC) with high specific surface area (1958 m2 g-1) was obtained by CO2 activation of KCl templated biochar at 900 °C. The electrochemical properties were evaluated by cyclic voltammetry, galvanostatic charge/discharge and electrochemical impedance spectroscopy. WS-90 had relatively low inner resistance of 1.7 Ω. The specific capacitance was 245.0 F g-1 in 6 mol L-1 KOH electrolyte at a current density of 0.1 A g-1, and it can maintain very good cyclic stability with capacitance retention ratio of 95.4% (from 245.0 to 233.7 F g-1 at current density of 0.1 A g-1 after 4000 cycles (0.1, 0.5, 1.0 and 5.0 A g-1 for 1000 cycles, respectively)).

Highly Active PdNi/RGO/Polyoxometalate Nanocomposite Electrocatalyst for Alcohol Oxidation.

PubMed

Hu, Jing; Wu, Xiaofeng; Zhang, Qingfan; Gao, Mingyan; Qiu, Haifang; Huang, Keke; Feng, Shouhua; Wang, Tingting; Yang, Ying; Liu, Zhelin; Zhao, Bo

2018-02-27

A PdNi/RGO/polyoxometalate nanocomposite has been successfully synthesized by a simple wet-chemical method. Characterizations such as transmission electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction analysis, and X-ray photoelectron spectroscopy are employed to verify the morphology, structure, and elemental composition of the as-prepared nanocomposite. Inspired by the fast-developing fuel cells, the electrochemical catalytic performance of the nanocomposite toward methanol and ethanol oxidation in alkaline media is further tested. Notably, the nanocomposite exhibits excellent catalytic activity and long-term stability toward alcohol electrooxidation compared with the PdNi/RGO and commercial Pd/C catalyst. Furthermore, the electrochemical results reveal that the prepared nanocomposite is attractive as a promising electrocatalyst for direct alcohol fuel cells, in which the phosphotungstic acid plays a crucial role in enhancing the electrocatalytic activities of the catalyst.

Molecularly imprinted polymer nanoparticles-based electrochemical sensor for determination of diazinon pesticide in well water and apple fruit samples.

PubMed

Motaharian, Ali; Motaharian, Fatemeh; Abnous, Khalil; Hosseini, Mohammad Reza Milani; Hassanzadeh-Khayyat, Mohammad

2016-09-01

In this research, an electrochemical sensor based on molecularly imprinted polymer (MIP) nanoparticles for selective and sensitive determination of diazinon (DZN) pesticides was developed. The nanoparticles of diazinon imprinted polymer were synthesized by suspension polymerization and then used for modification of carbon paste electrode (CPE) composition in order to prepare the sensor. Cyclic voltammetry (CV) and square wave voltammetry (SWV) methods were applied for electrochemical measurements. The obtained results showed that the carbon paste electrode modified by MIP nanoparticles (nano-MIP-CP) has much higher adsorption ability for diazinon than the CPE based non-imprinted polymer nanoparticles (nano-NIP-CP). Under optimized extraction and analysis conditions, the proposed sensor exhibited excellent sensitivity (95.08 μA L μmol(-1)) for diazinon with two linear ranges of 2.5 × 10(-9) to 1.0 × 10(-7) mol L(-1) (R (2) = 0.9971) and 1.0 × 10(-7) to 2.0 × 10(-6) mol L(-1) (R (2) = 0.9832) and also a detection limit of 7.9 × 10(-10) mol.L(-1). The sensor was successfully applied for determination of diaznon in well water and apple fruit samples with recovery values in the range of 92.53-100.86 %. Graphical abstract Procedure for preparation of electrochemical sensor based on MIP nanoparticles for determination of diazinon.

Scalable Preparation of Ternary Hierarchical Silicon Oxide-Nickel-Graphite Composites for Lithium-Ion Batteries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang , Jing; Bao, Wurigumula; Ma, Lu

2015-11-09

Silicon monoxide is a promising anode candidate because of its high theoretical capacity and good cycle performance. To solve the problems associated with this material, including large volume changes during charge-discharge processes, we report a ternary hierarchical silicon oxide–nickel–graphite composite prepared by a facile two-step ball-milling method. The composite consists of nano-Si dispersed silicon oxides embedded in nano-Ni/graphite matrices (Si@SiOx/Ni/graphite). In the composite, crystalline nano-Si particles are generated by the mechanochemical reduction of SiO by ball milling with Ni. These nano-Si dispersed oxides have abundant electrochemical activity and can provide high Li-ion storage capacity. Furthermore, the milled nano-Ni/graphite matrices stickmore » well to active materials and interconnect to form a crosslinked framework, which functions as an electrical highway and a mechanical backbone so that all silicon oxide particles become electrochemically active. Owing to these advanced structural and electrochemical characteristics, the composite enhances the utilization efficiency of SiO, accommodates its large volume expansion upon cycling, and has good ionic and electronic conductivity. The composite electrodes thus exhibit substantial improvements in electrochemical performance. This ternary hierarchical Si@SiOx/Ni/graphite composite is a promising candidate anode material for high-energy lithium-ion batteries. Additionally, the mechanochemical ball-milling method is low cost and easy to reproduce, indicating potential for the commercial production of the composite materials.« less

Label-Free 3D Ag Nanoflower-Based Electrochemical Immunosensor for the Detection of Escherichia coli O157:H7 Pathogens

NASA Astrophysics Data System (ADS)

Huang, He; Liu, Minghuan; Wang, Xiangsheng; Zhang, Wenjie; Yang, Da-Peng; Cui, Lianhua; Wang, Xiansong

2016-11-01

It is highly desirable to develop a rapid and simple method to detect pathogens. Combining nanomaterials with electrochemical techniques is an efficient way for pathogen detection. Herein, a novel 3D Ag nanoflower was prepared via a biomineralization method by using bovine serum albumin (BSA) as a template. It was adopted as a sensing interface to construct an electrochemical bacteria immunosensor for the rapid detection of foodborne pathogens Escherichia coli ( E. coli) O157:H7. Bacterial antibody was immobilized onto the surface of Ag nanoflowers through covalent conjugation. Electrochemical impedance spectroscopy (EIS) was used to detect and validate the resistance changes, where [Fe(CN)6]3-/4- acted as the redox probe. A linear relation between R et and E. coli concentration was obtained in the E. coli concentration range of 3.0 × 102-3.0 × 108 cfu mL-1. The as-prepared biosensor gave rise to an obvious response to E. coli but had no distinct response to Cronobacter sakazakii, methicillin-resistant Staphylococcus aureus (MRSA), Staphylococcus albus, Lactobacillus easei, and Shigella flexneri, revealing a high selectivity for the detection of the pathogens down to 100 cfu mL-1 in a short time. We believe that this BSA-conjugated 3D Ag nanoflowers could be used as a powerful interface material with good conductivity and biocompatibility for improving pathogen detection and treatment in the field of medicine, environment, and food safety.

Insight into the isoelectronic character of azomethines and vinylenes using representative models: a spectroscopic and electrochemical study.

PubMed

Bolduc, Andréanne; Al Ouahabi, Abelaziz; Mallet, Charlotte; Skene, W G

2013-09-20

A series of azomethine and vinylene dyad and triad analogues were prepared. Their absorbance, fluorescence, and redox properties were examined experimentally and theoretically using density functional theory (DFT) calculations. These measurements were done to determine the effect of the heteroatom of the azomethine relative to its all-carbon counterpart and to assess the isoelectronic character of the two bonds. The orientation of the azomethine was found to have little effect on the absorbance, fluorescence, and electrochemical properties. In contrast, the spectral and electrochemical properties were highly contingent on the electronic groups and degree of conjugation. The spectral properties could be tuned 200 nm across the visible region. More importantly, the heteroatom in the conjugated bond was found to give rise to only a 20 nm bathochromic shift in the absorbance and fluorescence spectra. The fluorescence quantum yield (ΦFl) of the vinylene derivatives varied between 5% and 20% with fluorescence quenching occurring by photoisomerization from the E to Z isomers. In contrast, the fluorescence of the analogous azomethine derivatives was completely quenched. The collective spectroscopic and electrochemical ab initio DFT data additionally confirmed that the azomethine and its analogous vinylene are isoelectronic. It was also found that a conjugated thiophene vinylene dyad with primary amines in the α,α'-positions could be prepared and isolated. The compound was stable under aerobic conditions providing electron withdrawing (either ester or nitrile) groups were located in the adjacent positions.

Electrochemical Determination of Chlorpyrifos on a Nano-TiO₂Cellulose Acetate Composite Modified Glassy Carbon Electrode.

PubMed

Kumaravel, Ammasai; Chandrasekaran, Maruthai

2015-07-15

A rapid and simple method of determination of chlorpyrifos is important in environmental monitoring and quality control. Electrochemical methods for the determination of pesticides are fast, sensitive, reproducible, and cost-effective. The key factor in electrochemical methods is the choice of suitable electrode materials. The electrode materials should have good stability, reproducibility, more sensitivity, and easy method of preparation. Mercury-based electrodes have been widely used for the determination of chlorpyrifos. From an environmental point of view mercury cannot be used. In this study a biocompatible nano-TiO2/cellulose acetate modified glassy carbon electrode was prepared by a simple method and used for the electrochemical sensing of chlorpyrifos in aqueous methanolic solution. Electroanalytical techniques such as cyclic voltammetry, differential pulse voltammetry, and amperometry were used in this work. This electrode showed very good stability, reproducibility, and sensitivity. A well-defined peak was obtained for the reduction of chlorpyrifos in cyclic voltammetry and differential pulse voltammetry. A smooth noise-free current response was obtained in amperometric analysis. The peak current obtained was proportional to the concentration of chlorpyrifos and was used to determine the unknown concentration of chlorpyrifos in the samples. Analytical parameters such as LOD, LOQ, and linear range were estimated. Analysis of real samples was also carried out. The results were validated through HPLC. This composite electrode can be used as an alternative to mercury electrodes reported in the literature.

Insulated InP (100) semiconductor by nano nucleus generation in pure water

NASA Astrophysics Data System (ADS)

Ghorab, Farzaneh; Es'haghi, Zarrin

2018-01-01

Preparation of specified designs on optoelectronic devices such as Light-Emitting Diodes (LEDs) and Laser Diodes (LDs) by using insulated thin films is very important. InP as one of those semiconductors which is used as optoelectronic devices, have two different kinds of charge carriers as n-InP and p-InP in the microelectronic industry. The surface preparation of this kind of semiconductor can be accomplished with individually chemical, mechanical, chemo - mechanical and electrochemical methods. But electrochemical method can be suitably replaced instead of the other methods, like CMP (Chemical Mechanical Polishing), because of the simplicity. In this way, electrochemically formation of insulated thin films by nano nucleus generation on semiconductor (using constant current density of 0.07 mA /cm2) studied in this research. Insulated nano nucleus generation and their growth up to thin film formation on semiconductor single crystal (100), n-InP, inpure water (0.08 µs/cm,25°c) characterized by Atomic Force Microscopy (AFM), Scanning Electron Microscopy (SEM), Four-point probe and Styloprofilometer techniques. The SEM images show active and passive regions on the n-InP surface and not uniform area on p-InP surface by passing through the passive condition. So the passive regions were nonuniform, and only the active regions were uniform and clean. The various semiconducting behavior in electrochemical condition, studied and compared with structural specification of InP type group (III-V).

Molecularly imprinted electrochemical biosensor based on Fe@Au nanoparticles involved in 2-aminoethanethiol functionalized multi-walled carbon nanotubes for sensitive determination of cefexime in human plasma.

PubMed

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

2014-10-15

The molecular imprinting technique depends on the molecular recognition. It is a polymerization method around the target molecule. Hence, this technique creates specific cavities in the cross-linked polymeric matrices. In present study, a sensitive imprinted electrochemical biosensor based on Fe@Au nanoparticles (Fe@AuNPs) involved in 2-aminoethanethiol (2-AET) functionalized multi-walled carbon nanotubes (f-MWCNs) modified glassy carbon (GC) electrode was developed for determination of cefexime (CEF). The results of X-ray photoelectron spectroscopy (XPS) and reflection-absorption infrared spectroscopy (RAIRS) confirmed the formation of the developed surfaces. CEF imprinted film was constructed by cyclic voltammetry (CV) for 9 cycles in the presence of 80 mM pyrrole in phosphate buffer solution (pH 6.0) containing 20mM CEF. The developed electrochemical biosensor was validated according to the International Conference on Harmonisation (ICH) guideline and found to be linear, sensitive, selective, precise and accurate. The linearity range and the detection limit were obtained as 1.0 × 10(-10)-1.0 × 10(-8)M and 2.2 × 10(-11)M, respectively. The developed CEF imprinted sensor was successfully applied to real samples such as human plasma. In addition, the stability and reproducibility of the prepared molecular imprinted electrode were investigated. The excellent long-term stability and reproducibility of the prepared CEF imprinted electrodes make them attractive in electrochemical sensors. Copyright © 2014 Elsevier B.V. All rights reserved.

Scalable Preparation of Ternary Hierarchical Silicon Oxide-Nickel-Graphite Composites for Lithium-Ion Batteries.

PubMed

Wang, Jing; Bao, Wurigumula; Ma, Lu; Tan, Guoqiang; Su, Yuefeng; Chen, Shi; Wu, Feng; Lu, Jun; Amine, Khalil

2015-12-07

Silicon monoxide is a promising anode candidate because of its high theoretical capacity and good cycle performance. To solve the problems associated with this material, including large volume changes during charge-discharge processes, we report a ternary hierarchical silicon oxide-nickel-graphite composite prepared by a facile two-step ball-milling method. The composite consists of nano-Si dispersed silicon oxides embedded in nano-Ni/graphite matrices (Si@SiOx /Ni/graphite). In the composite, crystalline nano-Si particles are generated by the mechanochemical reduction of SiO by ball milling with Ni. These nano-Si dispersed oxides have abundant electrochemical activity and can provide high Li-ion storage capacity. Furthermore, the milled nano-Ni/graphite matrices stick well to active materials and interconnect to form a crosslinked framework, which functions as an electrical highway and a mechanical backbone so that all silicon oxide particles become electrochemically active. Owing to these advanced structural and electrochemical characteristics, the composite enhances the utilization efficiency of SiO, accommodates its large volume expansion upon cycling, and has good ionic and electronic conductivity. The composite electrodes thus exhibit substantial improvements in electrochemical performance. This ternary hierarchical Si@SiOx /Ni/graphite composite is a promising candidate anode material for high-energy lithium-ion batteries. Additionally, the mechanochemical ball-milling method is low cost and easy to reproduce, indicating potential for the commercial production of the composite materials. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effect of various de-anodizing techniques on the surface stability of non-colored and colored nanoporous AAO films in acidic solution

NASA Astrophysics Data System (ADS)

Awad, Ahmed M.; Shehata, Omnia S.; Heakal, Fakiha El-Taib

2015-12-01

Anodic aluminum oxide (AAO) is well known as an important nanostructured material, and a useful template in the fabrication of nanostructures. Nanoporous anodic alumina (PAA) with high open porosity was prepared by adopting three de-anodizing regimes following the first anodizing step and preceding the second one. The de-anodizing methods include electrolytic etching (EE) and chemical etching using either phosphoric acid (PE) or sodium hydroxide (HE) solutions. Three of the obtained AAO samples were black colored by electrodeposition of copper nanoparticles in their pores. Electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization techniques were used to characterize the electrochemical performance of the two sets of the prepared samples. In general, the data obtained in aggressive aerated 0.5 M HCl solution demonstrated dissimilar behavior for the three prepared samples despite that the second anodizing step was the same for all of them. The data indicated that the resistance and thickness of the inner barrier part of nano-PAA film, are the main controlling factors determining its stability. On the other hand, coloring the film decreased its stability due to the galvanic effect. The difference in the electrochemical behavior of the three colored samples was discussed based on the difference in both the pore size and thickness of the outer porous part of PAA film as supported by SEM, TEM and cross-sectional micrographs. These results can thus contribute for better engineering applications of nanoporous AAO.

Solid-Solution Sulfides Derived from Tunable Layered Double Hydroxide Precursors/Graphene Aerogel for Pseudocapacitors and Sodium-Ion Batteries.

PubMed

Song, Yajie; Li, Hui; Yang, Lan; Bai, Daxun; Zhang, Fazhi; Xu, Sailong

2017-12-13

Transition-metal sulfides (TMSs) are suggested as promising electrode materials for electrochemical pseudocapacitors and lithium- and sodium-ion batteries; however, they typically involve mixed composites or conventionally stoichiometric TMSs (such as NiCo 2 S 4 and Ni 2 CoS 4 ). Herein we demonstrate a preparation of solid-solution sulfide (Ni 0.7 Co 0.3 )S 2 supported on three-dimensional graphene aerogel (3DGA) via a sulfuration of NiCo-layered double hydroxide (NiCo-LDH) precursor/3DGA. The electrochemical tests show that the (Ni 0.7 Co 0.3 )S 2 /3DGA electrode exhibits a capacitance of 2165 F g -1 at 1 A g -1 , 2055 F g -1 at 2 A g -1 , and 1478 F g -1 at 10 A g -1 ; preserves 78.5% capacitance retention upon 1000 cycles for pseudocapacitors; and in particular, possesses a relatively high charge capacity of 388.7 mA h g -1 after 50 cycles at 100 mA g -1 as anode nanomaterials for sodium-ion batteries. Furthermore, the electrochemical performances are readily tuned by varying the cationic type of the tunable LDH precursors to prepare different solid-solution sulfides, such as (Ni 0.7 Fe 0.3 )S 2 /3DGA and (Co 0.7 Fe 0.3 )S 2 /3DGA. Our results show that engineering LDH precursors can offer an alternative for preparing diverse transition-metal sulfides for energy storage.

Preparation of Al-Si Master Alloy by Electrochemical Reduction of Volcanic Rock in Cryolite Molten Salt

NASA Astrophysics Data System (ADS)

Liu, Aimin; Shi, Zhongning; Xu, Junli; Hu, Xianwei; Gao, Bingliang; Wang, Zhaowen

2016-06-01

Volcanic rock found in the Longgang Volcano Group in Jilin Province of China has properties essentially similar to Apollo lunar soils and previously prepared lunar soil simulants, such as Johnson Space Center Lunar simulant and Minnesota Lunar simulant. In this study, an electrochemical method of preparation of Al-Si master alloy was investigated in 52.7 wt.%NaF-47.3 wt.%AlF3 melt adding 5 wt.% volcanic rock at 1233 K. The cathodic electrochemical process was studied by cyclic voltammetry, and the results showed that the cathodic reduction of Si(IV) is a two-step reversible diffusion-controlled reaction. Si(IV) is reduced to Si(II) by two electron transfers at -1.05 V versus platinum quasi-reference electrode in 52.7 wt.%NaF-47.3 wt.%AlF3 molten salt adding 5 wt.% volcanic rock, while the reduction peak at -1.18 V was the co-deposition of aluminum and silicon. In addition, the cathodic product obtained by galvanostatic electrolysis for 4 h was analyzed by means of x-ray diffraction, x-ray fluorescence, scanning electron microscopy and energy dispersive spectrometry. The results showed that the phase compositions of the products are Al, Si, Al5FeSi, and Al3.21Si0.47, while the components are 90.5 wt.% aluminum, 4.4 wt.% silicon, 1.9 wt.% iron, and 0.2 wt.% titanium.

Controlled crystallization and granulation of nano-scale β-Ni(OH) 2 cathode materials for high power Ni-MH batteries

NASA Astrophysics Data System (ADS)

He, Xiangming; Li, Jianjun; Cheng, Hongwei; Jiang, Changyin; Wan, Chunrong

A novel synthesis of controlled crystallization and granulation was attempted to prepare nano-scale β-Ni(OH) 2 cathode materials for high power Ni-MH batteries. Nano-scale β-Ni(OH) 2 and Co(OH) 2 with a diameter of 20 nm were prepared by controlled crystallization, mixed by ball milling, and granulated to form about 5 μm spherical grains by spray drying granulation. Both the addition of nano-scale Co(OH) 2 and granulation significantly enhanced electrochemical performance of nano-scale Ni(OH) 2. The XRD and TEM analysis shown that there were a large amount of defects among the crystal lattice of as-prepared nano-scale Ni(OH) 2, and the DTA-TG analysis shown that it had both lower decomposition temperature and higher decomposition reaction rate, indicating less thermal stability, as compared with conventional micro-scale Ni(OH) 2, and indicating that it had higher electrochemical performance. The granulated grains of nano-scale Ni(OH) 2 mixed with nano-scale Co(OH) 2 at Co/Ni = 1/20 presented the highest specific capacity reaching its theoretical value of 289 mAh g -1 at 1 C, and also exhibited much improved electrochemical performance at high discharge capacity rate up to 10 C. The granulated grains of nano-scale β-Ni(OH) 2 mixed with nano-scale Co(OH) 2 is a promising cathode active material for high power Ni-MH batteries.

V-doped TiO2 supported Pt as a promising oxygen reduction reaction catalyst: Synthesis, characterization and in-situ evaluation in proton exchange membrane fuel cell

NASA Astrophysics Data System (ADS)

Bharti, Abha; Cheruvally, Gouri

2017-09-01

This study deals with the synthesis and characterization of V-doped, TiO2 supported Pt catalyst (Pt/V-TiO2) for oxygen reduction reaction (ORR) and its in-situ performance investigation in proton exchange membrane (PEM) fuel cell. Pt/V-TiO2 nanocomposite catalyst is prepared via a facile sol-gel and microwave assisted, modified chemical reduction route and its performance is compared with the undoped TiO2 supported catalyst, Pt/TiO2 prepared in an identical way. The prepared Pt/V-TiO2 and Pt/TiO2 catalysts are employed as cathode catalyst in PEM fuel cell and compared with standard Pt/C catalyst. Their comparative studies are conducted with physical and electrochemical techniques. In-situ electrochemical characterization studies show improved ORR catalytic activity of Pt/V-TiO2 compared to Pt/TiO2. Furthermore, both Pt/TiO2 and Pt/V-TiO2 are more stable than Pt/C when subjected to 6000 voltammetric cycles in the range of 0.2-1.2 V vs. standard hydrogen electrode in operating fuel cell conditions, losing only <20% of its electrochemical surface area as compared to 50% loss exhibited by Pt/C. This study thus demonstrates Pt/V-TiO2 nanocomposite material as a potential cathode catalyst for PEM fuel cell with immense scope for further investigation.

In-situ preparation of poly(ethylene oxide)/Li3PS4 hybrid polymer electrolyte with good nanofiller distribution for rechargeable solid-state lithium batteries

NASA Astrophysics Data System (ADS)

Chen, Shaojie; Wang, Junye; Zhang, Zhihua; Wu, Linbin; Yao, Lili; Wei, Zhenyao; Deng, Yonghong; Xie, Dongjiu; Yao, Xiayin; Xu, Xiaoxiong

2018-05-01

Nano-sized fillers in a polymer matrix with good distribution can play a positive role in improving polymer electrolytes in the aspects of ionic conductivity, mechanical property and electrochemical performance of Li-ion cells. Herein, polyethylene oxide (PEO)/Li3PS4 hybrid polymer electrolyte is prepared via a new in-situ approach. The ionic conductivities of the novel hybrid electrolytes with variable proportions are measured, and the optimal electrolyte of PEO-2%vol Li3PS4 presents a considerable ionic conductivity of 8.01 × 10-4 S cm-1 at 60 °C and an electrochemical window up to 5.1 V. The tests of DSC and EDXS reveal that the Li3PS4 nanoparticles with better distribution, as active fillers scattering in the PEO, exhibit a positive effect on the transference of lithium ion and electrochemical interfacial stabilities. Finally, the assembled solid-state LiFePO4/Li battery presents a decent cycling performance (80.9% retention rate after 325 cycles at 60 °C) and excellent rate capacities with 153, 143, 139 and 127 mAh g-1 at the discharging rate of 0.1 C, 0.2 C, 0.5 C and 1 C at 60 °C. It is fully proved that it is an advanced strategy to preparing the new organic/inorganic hybrid electrolytes for lithium-ion batteries applications.

Prepared multifunctional aerogel for high performance supercapacitors and effective adsorbents

NASA Astrophysics Data System (ADS)

Zhang, Yimei; Wang, Fei; Ou, Ping; Zhu, Hao; Zhao, Yalong; Wang, Liquan; Chen, Zhuang; Li, Shuai

2018-05-01

Energy and environment as the current research hots pot, how to effectively combine the two is very important and full of challenge. In this research, we design a new type multifunctional aerogel material, which not only can applied for supuercapacitors, but also acted as adsorbents for adsorb organic pollutant. This multifunctional aerogel was prepared by one-pot hydrothermal and freeze-drying method based on elongated TiO2 nanotubes (eTNTs) and graphene. During the hydrothermal process, the graphene nanosheets and eTNTs self-assembled into three-dimensional (3D) interconnected networks, in which the eTNTs with uniform size are intercalate the pore interconnected framework. The results show that the as-prepared eTNTs/graphene aerogel (TGA) exhibits a high specific surface area of 343.2 m2 g‑1. The highly porous and interconnected 3D nanostructure provided efficient migration of electrolyte ions and electrons, and thus the TGA exhibited excellent electrochemical performance for supercapacitors. The binder free TGA electrode possessed high performance electrochemical properties with an excellent specific capacitance (476.8 F g‑1 at scan rate of 5 mV s‑1), and outstanding cycle stability (92% capacitance retention after 5000 cycles). In addition, the TGA also showed admirable adsorption capacity for organic pollutant of bisphenol A, which reached 523.5 mg g‑1. The excellent electrochemical and adsorption capacities suggest the TGA to be the promising materials application in energy storage and environmental remediation.

Methods and electrolytes for electrodeposition of smooth films

DOEpatents

Zhang, Jiguang; Xu, Wu; Graff, Gordon L; Chen, Xilin; Ding, Fei; Shao, Yuyan

2015-03-17

Electrodeposition involving an electrolyte having a surface-smoothing additive can result in self-healing, instead of self-amplification, of initial protuberant tips that give rise to roughness and/or dendrite formation on the substrate and/or film surface. For electrodeposition of a first conductive material (C1) on a substrate from one or more reactants in an electrolyte solution, the electrolyte solution is characterized by a surface-smoothing additive containing cations of a second conductive material (C2), wherein cations of C2 have an effective electrochemical reduction potential in the solution lower than that of the reactants.

Surfactant-Templated Mesoporous Metal Oxide Nanowires

DOE PAGES

Luo, Hongmei; Lin, Qianglu; Baber, Stacy; ...

2010-01-01

We demore » monstrate two approaches to prepare mesoporous metal oxide nanowires by surfactant assembly and nanoconfinement via sol-gel or electrochemical deposition. For example, mesoporous Ta 2 O 5 and zeolite nanowires are prepared by block copolymer Pluronic 123-templated sol-gel method, and mesoporous ZnO nanowires are prepared by electrodeposition in presence of anionic surfactant sodium dodecyl sulfate (SDS) surfactant, in porous membranes. The morphologies of porous nanowires are studied by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analyses.« less

New generation "nanohybrid supercapacitor".

PubMed

Naoi, Katsuhiko; Naoi, Wako; Aoyagi, Shintaro; Miyamoto, Jun-Ichi; Kamino, Takeo

2013-05-21

To meet growing demands for electric automotive and regenerative energy storage applications, researchers all over the world have sought to increase the energy density of electrochemical capacitors. Hybridizing battery-capacitor electrodes can overcome the energy density limitation of the conventional electrochemical capacitors because they employ both the system of a battery-like (redox) and a capacitor-like (double-layer) electrode, producing a larger working voltage and capacitance. However, to balance such asymmetric systems, the rates for the redox portion must be substantially increased to the levels of double-layer process, which presents a significant challenge. An in situ material processing technology called "ultracentrifuging (UC) treatment" has been used to prepare a novel ultrafast Li4Ti5O12 (LTO) nanocrystal electrode for capacitive energy storage. This Account describes an extremely high-performance supercapacitor that utilizes highly optimized "nano-nano-LTO/carbon composites" prepared via the UC treatment. The UC-treated LTO nanocrystals are grown as either nanosheets or nanoparticles, and both have hyperlinks to two types of nanocarbons: carbon nanofibers and supergrowth (single-walled) carbon nanotubes. The spinel structured LTO has been prepared with two types of hyperdispersed carbons. The UC treatment at 75 000G stoichiometrically accelerates the in situ sol-gel reaction (hydrolysis followed by polycondensation) and further forms, anchors, and grafts the nanoscale LTO precursors onto the carbon matrices. The mechanochemical sol-gel reaction is followed by a short heat-treatment process in vacuo. This immediate treatment with heat is very important for achieving optimal crystallization, inhibiting oxidative decomposition of carbon matrices, and suppressing agglomeration. Such nanocrystal composites can store and deliver energy at the highest rate attained to this date. The charge-discharge profiles indicate a very high sustained capacity of 80 mAh g(-1) at an extremely high rate of 1200 C. Using this ultrafast material, we assembled a hybrid device called a "nanohybrid capacitor" that consists of a Faradaic Li-intercalating LTO electrode and a non-Faradaic AC electrode employing an anion (typically BF4(-)) adsorption-desorption process. The "nanohybrid capacitor" cell has demonstrated remarkable energy, power, and cycleability performance as an electrochemical capacitor electrode. It also exhibits the same ion adsorption-desorption process rates as those of standard activated carbon electrodes in electrochemical capacitors. The new-generation "nanohybrid capacitor" technology produced more than triple the energy density of a conventional electrochemical capacitor. Moreover, the synthetic simplicity of the high-performance nanostructures makes it possible to scale them up for large-volume material production and further applications in many other electrochemical energy storage devices.

Preparation and characterization of zinc oxide nanoparticles and their sensor applications for electrochemical monitoring of nucleic acid hybridization.

PubMed

Yumak, Tugrul; Kuralay, Filiz; Muti, Mihrican; Sinag, Ali; Erdem, Arzum; Abaci, Serdar

2011-09-01

In this study, ZnO nanoparticles (ZNP) of approximately 30 nm in size were synthesized by the hydrothermal method and characterized by X-ray diffraction (XRD), Braun-Emmet-Teller (BET) N2 adsorption analysis and transmission electron microscopy (TEM). ZnO nanoparticles enriched with poly(vinylferrocenium) (PVF+) modified single-use graphite electrodes were then developed for the electrochemical monitoring of nucleic acid hybridization related to the Hepatitis B Virus (HBV). Firstly, the surfaces of polymer modified and polymer-ZnO nanoparticle modified single-use pencil graphite electrodes (PGEs) were characterized using scanning electron microscopy (SEM). The electrochemical behavior of these electrodes was also investigated using differential pulse voltammetry (DPV) and electrochemical impedance spectroscopy (EIS). Subsequently, the polymer-ZnO nanoparticle modified PGEs were evaluated for the electrochemical detection of DNA based on the changes at the guanine oxidation signals. Various modifications in DNA oligonucleotides and probe concentrations were examined in order to optimize the electrochemical signals that were generated by means of nucleic acid hybridization. After the optimization studies, the sequence-selective DNA hybridization was investigated in the case of a complementary amino linked probe (target), or noncomplementary (NC) sequences, or target and mismatch (MM) mixture in the ratio of (1:1). Copyright © 2011 Elsevier B.V. All rights reserved.

Electrochemical performance of electrospun free-standing nitrogen-doped carbon nanofibers and their application for glucose biosensing.

PubMed

Liu, Dong; Zhang, Xueping; You, Tianyan

2014-05-14

In spite of excellent electrochemical properties, nitrogen-doped carbon nanofibers (NCNFs) have rarely been studied in the field of electroanalysis. In this work, we investigated the electrochemical properties and biosensing performance of NCNFs prepared by a newly proposed approach. The as-obtained NCNFs present a unique free-standing structure with high flexibility which could be convenient for electrode modification. Electrochemical measurements of typical redox species including [Ru(NH3)6]3+/2+, [Fe(CN)6]3-/4-, [Fe(H2O)6]3+/2+, and dopamine indicate that the NCNFs have a larger surface area and faster electron transfer rate compared with carbon nanofibers (CNFs). The presence of high content of pyrrolic-N and abundant defective sites in NCNFs leads to an obvious positive shift of peak potential for oxygen reduction at NCNFs relative to that obtained at CNFs. The unique structure and properties greatly enhance the electrochemical performance of NCNFs. The glucose biosensor based on glucose oxidase/NCNFs shows linear ranges of 0.2-1.2 mM at -0.42 V and 0.05-3 mM at 0.40 V both with high stability. These results suggest that the NCNFs could be a convenient and stable platform for electrochemical biosensors.

Exploiting differential electrochemical stripping behaviors of Fe3O4 nanocrystals toward heavy metal ions by crystal cutting.

PubMed

Yao, Xian-Zhi; Guo, Zheng; Yuan, Qing-Hong; Liu, Zhong-Gang; Liu, Jin-Huai; Huang, Xing-Jiu

2014-08-13

This study attempts to understand the intrinsic impact of different morphologies of nanocrystals on their electrochemical stripping behaviors toward heavy metal ions. Two differently shaped Fe3O4 nanocrystals, i.e., (100)-bound cubic and (111)-bound octahedral, have been synthesized for the experiments. Electrochemical results indicate that Fe3O4 nanocrystals with different shapes show different stripping behaviors toward heavy metal ions. Octahedral Fe3O4 nanocrystals show better electrochemical sensing performances toward the investigated heavy metal ions such as Zn(II), Cd(II), Pb(II), Cu(II), and Hg(II), in comparison with cubic ones. Specifically, Pb(II) is found to have the best stripping performance on both the (100) and (111) facets. To clarify these phenomena, adsorption abilities of as-prepared Fe3O4 nanocrystals have been investigated toward heavy metal ions. Most importantly, combined with theoretical calculations, their different electrochemical stripping behaviors in view of facet effects have been further studied and enclosed at the level of molecular/atom. Finally, as a trial to find a disposable platform completely free from noble metals, the potential application of the Fe3O4 nanocrystals for electrochemical detection of As(III) in drinking water is demonstrated.

Carbon decorative coatings by dip-, spin-, and spray-assisted layer-by-layer assembly deposition.

PubMed

Hong, Jinkee; Kang, Sang Wook

2011-09-01

We performed a comparative surface analysis of all-carbon nano-objects (multiwall carbon nanotubes (MWNT) or graphene oxide (GO) sheets) based multilayer coatings prepared using three widely used nanofilm fabrication methods: dip-, spin-, and spray-assisted layer-by-layer (LbL) deposition. The resultant films showed a marked difference in their growth mechanisms and surface morphologies. Various carbon decorative coatings were synthesized with different surface roughness values, despite identical preparation conditions. In particular, smooth to highly rough all-carbon surfaces, as determined by atomic force microscopy (AFM) and scanning electron microscopy (SEM), were readily obtained by manipulating the LbL deposition methods. As was confirmed by the AFM and SEM analyses, this finding indicated the fundamental morphological evolution of one-dimensional nano-objects (MWNT) and two-dimensional nano-objects (GO) by control of the surface roughness through the deposition method. Therefore, an analysis of the three LbL-assembly methods presented herein may offer useful information about the industrial use of carbon decorative coatings and provide an insight into ways to control the structures of multilayer coatings by tuning the morphologies of carbon nano-objects.

A honeycomb-like porous carbon derived from pomelo peel for use in high-performance supercapacitors

NASA Astrophysics Data System (ADS)

LiangThese Two Authors Are Equal Main Contributors., Qinghua; Ye, Ling; Huang, Zheng-Hong; Xu, Qiang; Bai, Yu; Kang, Feiyu; Yang, Quan-Hong

2014-10-01

A cost-effective approach to obtain electrode materials with excellent electrochemical performance is critical to the development of supercapacitors (SCs). Here we report the preparation of a three-dimensional (3D) honeycomb-like porous carbon (HLPC) by the simple carbonization of pomelo peel followed by KOH activation. Structural characterization indicates that the as-prepared HLPC with a high specific surface area (SSA) up to 2725 m2 g-1 is made up of interconnected microporous carbon walls. Chemical analysis shows that the HLPC is doped with nitrogen and also has oxygen-containing groups. Electrochemical measurements show that the HLPC not only exhibits a high specific capacitance of 342 F g-1 and 171 F cm-3 at 0.2 A g-1 but also shows considerable rate capability with a retention of 62% at 20 A g-1 as well as good cycling performance with 98% retention over 1000 cycles at 10 A g-1 in 6 M KOH. Furthermore, an as-fabricated HLPC-based symmetric SC device delivers a maximum energy density of ~9.4 Wh kg-1 in the KOH electrolyte. Moreover, the outstanding cycling stability (only 2% capacitance decay over 1000 cycles at 5 A g-1) of the SC device makes it promising for use in a high-performance electrochemical energy system.A cost-effective approach to obtain electrode materials with excellent electrochemical performance is critical to the development of supercapacitors (SCs). Here we report the preparation of a three-dimensional (3D) honeycomb-like porous carbon (HLPC) by the simple carbonization of pomelo peel followed by KOH activation. Structural characterization indicates that the as-prepared HLPC with a high specific surface area (SSA) up to 2725 m2 g-1 is made up of interconnected microporous carbon walls. Chemical analysis shows that the HLPC is doped with nitrogen and also has oxygen-containing groups. Electrochemical measurements show that the HLPC not only exhibits a high specific capacitance of 342 F g-1 and 171 F cm-3 at 0.2 A g-1 but also shows considerable rate capability with a retention of 62% at 20 A g-1 as well as good cycling performance with 98% retention over 1000 cycles at 10 A g-1 in 6 M KOH. Furthermore, an as-fabricated HLPC-based symmetric SC device delivers a maximum energy density of ~9.4 Wh kg-1 in the KOH electrolyte. Moreover, the outstanding cycling stability (only 2% capacitance decay over 1000 cycles at 5 A g-1) of the SC device makes it promising for use in a high-performance electrochemical energy system. Electronic supplementary information (ESI) available: Experimental section and additional table and figures (Fig. S1-S8). See DOI: 10.1039/c4nr04541f